Indian Patents. 255480:A METHOD OF MAKING CARBON BLACK PRODUCT

Title of Invention	A METHOD OF MAKING CARBON BLACK PRODUCT
Abstract	Methods of producing carbon black in a multi-stage reaction are described. Also described is carbon black formed from the processes.

Full Text	CARBON BLACK AND MULTI-STAGE PROCESS FOR MAKING SAME [0001] This application claims the benefit under 35 U.S.C §120 of prior U.S. Patent Application No. 10/838,530 filed May 4S 2004 which is incorporated in its entirety by reference herein. BACKGROUND OF THE INVENTION [0002] The present invention relates to carbon black and to processes for making ca&on blacL More particularly, the present invention relates to unique forms of carbon black and to several multi-stage carbon black forming processes. [0003] The present invention relates to the production of carbon black such as furnace bkcks having many important applications, such as fillers, pigments, and reinforcing agents, in rubbers and plastics. Generally, the furnace process for preparing these blacks entails Hie cracking and/or incomplete combustion of a hydrocarbon feedstock such as natural gas or catalytic cracker cycle stock in a closed conversion zone to produce carbon black. The carbon black entrained in fee gases emanating from the conversion zone is then quenched and collected by any suitable means conventionally used in the art It has, however, been extremely costly to produce carbon blacks having high surface area with increased structure. [0004] US, Patent No. 5,190,739 to MacKay et aL relates, in part, to a process for preparing carbon blacks having lower-than-normal structure at a given surface area and a lower-than-normal surface area at a given overall combustion level. The process can involve the use of a multi-stage furnace wherein a second source of hydrocarbons is added to the stream of hot first-stage gases. Certain embodiments of the 6739 patent also relate to the use of potassium to make low structure carbon blacks. However, foe amount of the auxiliary hydrocarbons used in the '739 patent are considerably lower amounts than in the first stage. Furthermore, the '739 patent can optionally use additional fuel and/or oxygen to achieve further combustion "Upon the introduction of the auxiliary hydrocarbons. la addition, there is no significant temperature zone difference between the zone where the first feedstock is mtroduced and the zone where the auxiliary feedstock is introduced in the '739 patent [0005] In U.S* Patent No. 4,383,973 to Cheng, this patent relates to a process which involves two carbon hlack reactors in sequence where one of the reactors is jfor a high-structure carbon black and the second is for a low-structure carbon "black. In the one figure of the '973 patent, the reactors are apparently connected together in sequence. However, in this process, additional air and fuel are introduced to the second feedstock and there is no significant temperature difference between the two feedstock introduction zones. Further, there is no partial quenching occurring prior to the complete quenching. The 6973 patent further states that there is no quenching occurring between the first and second carbon black forming zones and further 10 ppm or more potassium can be introduced in the high structure zone. Furthermore, with the high combustion occurring in each feedstock introduction zone, there would not be any significant temperature zone difference between the first carbon black of high structure is formed and the zone where the low structure carbon blackis formed. [0006] In U.S. Patent No. 4,976,945* a process for producing carbon black is described which uses various amounts of alkali metal, such as potassium, in a carbon black reactor to regulate structure. The '945 patent does state that an alkali metal compound and/or alkaline earth metal compound can be added in an amount of 500 to 50,000 ppm relative to the hydrocarbon starting material The 4945 patent does not relate to a multi-stage carbon black forming process and shows no partial quenching occurring prior to the complete quenching. The '945 patent further states that an alkali metal compound is particularly effective far the production of carbon black whe^e the DBP absorption is at most 90 cc/lOOg, r [0007] VS. Patent No. 4,822,588 to Gravely et aL relates to a carbon black reactor which has a first reaction zone and a second reaction zone that are serially connected In this process, in the second stage, additianal carbonaceous feedstock is introduced to form a second reaction mixture* hi this process, the goal was to not substantially form carbon black in the first reaction zone. Also, the process didn't use an alkaK metal or tffaflinfl earth metal [0008] Accordingly, there is a need to provide a novel and improved process for preparing carbon blacks which exhibit improved or increased structure with increased surface area, [0009] All of the patents and publications mentioned throughout are incorporated in fteir entirety by reference herein. BRIEF DESCRIPTION OF THE DRAWINGS [0010] Figure 1 is cross sectional view of a carbon black reactor that can be used in the present invention, SUMMARY OF THE PRESENT INVENTION [0011] It is therefore a feature of the present invention to provide a method of producing carbon black with high surface area and high structure. [0012] Aaother feature of the present invention is to provide a method of producing caibon black which is cost effective. [0013] Additional features and advantages of the present invention will be set forth in part in the description that follows, and in part will be apparent from the description, or may be learned by practice of the present invention. The objectives and other advantages of Hie present invention will be realized and attained by means of the elements and combinations particularly pointed out in the description and appended claims. [0014] To achieve these and other advantages and m accordance with fixe purposes of the present invention, as embodied and broadly described herein, the present invention relates to a method of making a carbon black product The method includes introducing a carbon black yielding feedstock in a first stage of a carbon black reactor and combining this feedstock with a stream of hot gases to form a precursor which essentially is a first carbon black and optionally byproducts. Then, a second carbon black yielding feedstock is subsequently introduced to the precursor to at least partially quench the reaction stream containing the first carbon black and then the process includes completely quenching to form fixe carbon black product I001S] The present invention farther relates to a process of making a carbon black product which includes iatroducing a caibon black yielding feedstock in a first stage of a caxbon black reactor and combining this feedstock with a stream of hot gases to form a precursor. The precursor contains a first carbon black. Then, in the process, a second carbon black yielding feedstock is introduced to the precursor, wherein the second carbon black yielding feedstock contains at least 15% by weight of the total amount by weight of the carbon black yielding feedstock utilized during the entire process, [0016J In addition, the present invention relates to a process of making a carbon black product which includes introducing a first carbon black yielding feedstock in a first stage of a carbon black reactor and combining this feedstock with a stream of hot gases to form a precursor which contains a first carbon black Then, in the process, a second carbon black yielding feedstock is introduced to the precursor, wherein no oxidizing sotnce and no fiiel source are introduced after formation of the precursor, [0017] Furthermore, the present invention relates to a process of making a carbon black product which includes forming a precursor which contains a first carbon black in a first temperature zone and then forming a carbon black product from this precursor in a second temperature zone before a quench zone. The first temperature zone and the second temperature zone have a temperature difference of 200°C or more. [0018] In each of these processes, the process can* include the introduction of at least one substance containing at least one Group IA or Group HA element at one or more locations of the process, [0019] Also, the present invention relates to a carbon black having a DBF range of from about 30 to about 150 cc/lOOg with a total Group LA or Group DA element content of from about 50 to about 5,000 ppm. The carbon black can have other physical or chemical attributes including, but not limited tos a leachable Group IA or Group HA content, a porosity amount, and desirable t-area such as a t-area of from about 10 to about 180 m2/g. Other characteristics are farther described herein. [0020] It is to be understood that both the foregoing general description and the following detailed description axe exemplary and explanatory only and are intended to provide a ftdher explanation of the present invention, as claimed DETAILED DESCRIPTION OF THE PRESENT INVEmiON [0021] The present invention relates to carbon black products as well as various methods of making carbon black products. In the preferred embodiments, the methods of making the carbon black product involves the use of a multi-stage carbon black reactor. More preferably, the multi-stage reactor has at least two stages (two, three, four, or more stages) where generally there are at least two feedstock (e.g., two, three, four, or more feedstocks) introductions occurring. The carbon black product is preferably a furnace black. [0022] In more detail, in one embodiment of the present invention, the present invention relates to a method of making a carbon black product which involves introducing a carbon blade yielding feedstock in a first stage of a carbon black reactor. The carbon black yielding feedstock is combined with a stream of hot gases to form a precursor. The precursor is or at least contains a first carbon black A second carbon black yielding feedstock is then subsequently introduced into the carbon black reactor downstream of the first stage and this second carbon black yielding feedstock k preferably introduced in the presence of the precursor formed in the first stage. Li this method, the second carbon black yielding feedstock at least partially quenches the reactions that are occurring. Afterwards, the complete quenching can occur downstream, wherein the carbon forming reactions are completely stopped or quenched and a carbon black product is formed, [0023] For purposes of this method as well as the other methods described herein* a multi-stage carbon black reactor can be used such as the ones described in U.S. Patent No, 4,383,973, UJ3. Patent No. 5,190,739, U.S. Patent No. 5,877,251, U.S. Patent No. 6,153,684, or U.S. Patent No. 6,403,695, all of which are incorporated in their entirety by reference herein. Thus, the present invention can use a multi-stage furnace process. [0024] The carbon black yielding feedstock can be any conventions] carbon black yielding feedstock which results in the formation of carbon black For instance, any hydrocarbon material can be used. A suitable feedstock can be any carbon black-yielding hydrocarbon feedstock which is readily volatilizable under the conditions of the reaction. ,For example, unsaturated hydrocarbons such as acetylene; olefins such as ediylene, propylene, butylene; aromatics such as benzene, toluene and xylene; certain saturated hydrocarbons; and other hydrocarbons such as kerosenes, naphthalenes, teipenes, ethylene tars, aromatic cycle stocks and the like may be used [0025] With respect to the stream of hot gases that is combined with the carbon black yielding feedstock, the stream of hot gases can also be consideied hot combustion gases that can be generated by contacting a solid, liquid, and/or gaseous fuel with a suitable oxidant stream such as, but not limited to, air, oxygen, mixtures of air and oxygen, or the like. Alternatively, a preheated oxidant stream may be passed through without adding a liquid or gaseous fuel. Examples of the fiiel suitable for use in contacting the oxidant stream to generate the hot gases include any of the readily combustible gas, vapor, or liquid streams, such as natural gas, hydrogen, carbon monoxide, methane, acetylene, alcohol, or kerosene. Generally, it is preferred to use fuels having a high content of carbon-containing components and in particular, hydrocarbons- The ratio of air to fiiel utilized to produce the carbon blacks of the present invention may be from about 1;1 (stiochiometric ratio) to infinity. As stated, to facilitate the generation of hot gases, the oxidant stream may be preheated. [0026] The general process of forming carbon black through the use of a multi-stage reactor and achieving appropriate hot gases to form carbon black are described in the above-identified referenced patents which are incorporated by reference herein and can be applied in the present invention with the changes described herein* in one embodiment of the present invention, surface area is maximized by maintaining high temperature preferably after introduction of the first carbon black yielding feedstock, such as by no water cooling, rapid mixing of the hot gases with the carbon black yielding feedstock, and/or short mixing lengths, and the like. {0027] The present invention can be practiced using any suitable carbon black producing reactor. Figure 1, for example, illustrates a cross-section of one example of such a reactor. Reactors of this type generally use a combustion gas which is mixed with an oxidant such as air. The gas mixture is generally introduced into a combustion chamber and ignited by any suitable method. Gas flow is left to right (direction A) in Figure 1. Once ignited, the hot gas mixture can be moved through the reactor, and "brought into contact with a hydrocarbon feedstock suitable for producing carbon black in Figure X, and simply as an example, fuel can be introduced at location 1 and oxidant can be introduced at location 2. Other locations are possible. The first location 3 (one or more) is an example of a point of intcoduction of the first carbon black yielding feedstock. The second and third location 3 axe examples of points of introduction of the second carbon black yielding feedstock. Location 4 is an example of a suitable location of a partial quenching agent, like water. Location 5 is an example of a suitable location for complete quenching. The double parallel lines signify that the reactor can be any length. The various D numbers represent various lengths of the reactor. Dl through D8 can be any suitable diameter and can be the same or different For instance, D2 can be less than Dl and D8, and Dl and D8 can be the same or different. Zone LI or zone L2 are examples of the first temperature zone, and zone L3 is an example of the second temperature zone. If a partial quench agent is used at for instance point 4, then the first temperature zone is typically LI. [0028] Generally, carbon black-yielding feedstock can be injected into a reactor by a plurality of streams 3 (in L-2)? shown in Figure 1, which penetrate into the interior regions of the hot combustion gas stream, to insure a high rate of mixing and shearing of the hot combustion gases and the carbon black-yielding feedstock. This insures that the feedstock rapidly and completely decomposes and converts into a first carbon black material. [0029] The precursor fonned in the methods described herein contains a first carbon black and can contain other components such as unused fuel or oxidants or combustion products and can also contain other components such as, but not limited toa inorganic substances, metals, salts, and metal oxides. Primarily, the precursor is a carbon black product For instance, 80 to 99% and, more preferably, 95% to 99% or greater (e,g,, 100%) by weight of the precursor is carbon black. [0030] With respect to the subsequent introduction of a second carbon black yielding feedstock to the precursor containing the first carbon black, this second carbon black yielding feedstock is added downstream of the first stage in an amount to at least partially quench the reactions that are still occurring from the first stage- For purposes of the present invention, the partial quenching of the reactions means that this introduction of the second carbon black yielding feedstock is not a complete quenching of the reactions but quenches a portion of the reactions. Preferably, the introduction of the second carbon black yielding feedstock does not completely quench the reactions. The second caibon black yielding feedstock can be the same type of feedstock or a different feedstock firom the carbon black yielding feedstock introduced in the first stage. [0031] The above-identified patents provide various carbon black forming conditions and starting amounts that can be used in the formation of the precursor. [0032] The carbon black yielding feedstock introduced in either stage can be introduced in any conventional way such as a single stream or plurality of streams and the introduction of the feedstocks can occur at any rate. With a plurality of streams, the rates for each stream can be the same or different. [0033] Preferably, the subsequent introduction of the carbon black yielding feedstock to the precursor is done by a plurality of streams. Any manner in which the second carbon black yielding feedstock can be introduced can be used. [0034] After the mixture of hot combustion gases and carbon black-yielding feedstock is quenched, the cooled gases pass downstream into any conventional cooling and separating means whereby the carbon black is recovered. The separation of the carbon black firom the gas stream is readily accomplished by conventional means such as a precipitator, cyclone separator or bag filter. With respect to completely quenching the reactions to form the final carbon black product any conventional means to quench the reaction downstream of the introduction of the second carbon black yielding feedstock can be used and is known to those skilled in the art. For instance, a quenching fluid can be injected which may be water or other suitable fluids to stop the chemical reaction. (0035] In an embodiment of the present invention, the method farther includes introducing at least one substance that is or that contains at least one Group IA or Group HA element (or ion thereof) of the Periodic Table, Preferably., the substance contains at least one alkali metal or alkaline earth metal. Examples include lithium, sodium, potassium, rubidium, cesium, francium, calcium, barium, strontium, or radium, or combinations thereof. Any mixtures of one or more of these components can be present in the substance. The substance can be a solid, solution* dispersion, gas, or any combinations thereof More than one substance having the same or different Group IA or Group HA metal can be used. If multiple substances are used, the substances can be added together separately, sequentially, or in different reaction locations. For purposes of the present invention, the substance can be the metal (or metal ion) itself, a compound containing one or more of these elements, including a salt containing one or more of these elements, and the like. Preferably, the substance is capable of introducing a metal or metal ion into the reaction that is ongoing to form the carbon black product Fox purposes of the present invention, preferably, tbe substance is introduced prior to the complete quenching as described above. For instance, the substance can be added at any point prior to the complete quenching, including prior to the introduction of the carbon black yielding feedstock in the first stage; during the introduction of the carbon black yielding feedstock in the first stage; after the introduction of the carbon black yielding feedstock in the first stage; prior to, during, or immediately after the introduction of the second carbon black yielding feedstock to the precursor; or any step after the introduction of the second carbon black yielding feedstock but prior to the complete quenching. More than one point of introduction of the substance can be used. Preferably, the introduction of the substance is prior to the introduction of the second carbon black yielding feedstock and/or during or right after the introduction of the carbon black yielding feedstock in the first stage. The amount of the Group IA or Group HA metal containing substance can be any amount as long as a carbon black product can be formed. For instance, the amount of the substance can be added in an amount such that 200 ppm or more of the Group IA or Group IIA element is present in the carbon black product ultimately formed. Other amounts include from about 200 ppm to about 5000 ppm or more and other ranges can be from about 300 ppm to about 1000 ppm, or from about 500 ppm to about 1000 ppm of the Group IA or Group HA element present in the carbon black product that is formed These levels can be with respect to the metal ion concentration. As stated, these amounts of the Group IA or Group HA element present in the carbon black product that is formed can be with respect to one element or more than one Group IA or Group HA element and would be therefore a combined amount of the Group IA or Group HA elements present in the carbon black product that is formed. The substance can be added in any fashion including any conventional means. In other words, the substance can be added in the same manner that a carbon black yielding feedstock is introduced. The substance can be added as a gas, liquid, or solid, or any combination thereof. The substance can be added at one point or several points and can be added as a single stream or a plurality of streams. The substance can be mixed in with the feedstock, fuel, and/or oxidant prior to or during their introduction. [0036] One method by which a substance containing at least one Group IA ox Group HA element such as, for example, potassium can be introduced into fee feedstock is by the incorporation of fee substance into the feedstock. Upon combustion, the metal ions can become uniformly incorporated into the carbon black. The charge of metal ions provides a repulsive force between individual carbon black particles. Has repulsive force can keep particles from aggregating, thus decreasing fee overall structure of the carbon black. [0037] The application of additional feedstock to the preexisting carbon black particles may be repeated any number of times until fee reaction of feedstock to carbon black ceases. Each time additional feedstock is added, fee temperature of fee entire reaction mixture generally goes down, and carbon black particle size increases. In this way fee feedstock can act as a quenching agent for fee cooling of fee carbon black. [00381 In another embodiment of fee present invention, fee present invention also relates to a method of making a carbon black product wherein a carbon black yielding feedstock is introduced in a first stage and combined wife a stream of hot gases to form a precursor. Furfeermoie, a second carbon black yielding feedstock is subsequently introduced downstream to fee precursor, Thus this method is, up to this point, fee same as fee above-described embodiment and therefore fee same conditions and examples would apply to this process. Furthermore, in this process* fee second carbon black yielding feedstock contains at least 15 % by weight of the total amount of fee carbon black yielding feedstock utilized during fee entire process. The second carbon black yielding feedstock can contain from about 15% by weight to about 80% by weight of fee total amount of fee carbon black yielding feedstock utilized during fee entire process. Other ranges include from about 25% to about 70% or from about 30% to about 60% by weight of fee total amount by weight of fee carbon black yielding feedstock utilized during fee eaitire process, The introduction of fee second carbon black yielding feedstock can be introduced in two ot more segments, or stages wherein the segments can be downstream from the first segment This is quite different from previous multi-stage processes where any subsequent introduction of a carbon black yielding feedstock would be a veiy low amount such as on the order of 10% by weight or lower. This large amount of the second carbon black yielding feedstock leads to beneficial carbon black products as to be described later. Also, this amount of carbon black can serve as a partial quenching of the reactions that are occurring. f0039] As in the first described process, a substance that is or contains a Group IA or Group HA element or ion thereof can be added in the same manner as described above. These above-described details apply equally here. [0040] In another embodiment of the present invention, the present invention relates to a process of making a carbon black product wherein a first carbon black yielding feedstock is introduced in a first stage and combined with a stream of hot gases to form a precursor as with respect to the first and second above-described processes. A second carbon black yielding feedstock is then introduced to the precursor and in this process, no oxidizing source and no fuel source are introduced after formation of the precursor. Urns, in this process, any oxidizing source and/or fuel source are only introduced prior to the introduction of the first carbon black yielding feedstock or during the introduction of the first carbon black yielding feedstock. Again, this is quite different from previous processes where typically, if a second carbon black yielding feedstock is introduced; sufficient fuel and an oxidizing source are added to promote sufficient pyrolysis of the second carbon black yielding feedstock, Again, as with the previous processes, at least one Group IA or Group DA metal containing substance can be introduced in the same manner as described above and these details apply equally here, [0041] In another embodiment of the present invention, the present invention relates to a process of making a carbon black product wherein a precursor containing a first carbon black is formed in a first temperature zone of a carbon black reactor and then a carbon black yielding feedstock can be introduced to the precursor* The method then involves farming a carbon black product in a second temperature zone which is located before a quench zone. In Ibis process, the first temperature zone and the second temperature zoue have a temperature difference of 200°C or more, and preferably a temperature difference of 300°C or more-Suitable ranges with respect to the temperature difference can be, for instance, from about 200°C to about 900°C or from about 400° to about 700°G Other temperature ranges with regard to the temperature difference can be used. Generally, with respect to this temperature difference, the first temperature zone has the higher temperature and the second temperature zone has the lower temperature thus creating the temperature difference though this is a preferred embodiment only, The difference in temperatures can be achieved any number of ways such as avoiding any further introduction of combustion gases or avoiding or minimizing formation of combustion gases in the second temperature zone. Other means to achieve ibis difference can be used. Again, as with the previous embodiments, a Group IA or Group HA metal containing substance can be used and introduced in the same manner as described above and the details as set forth above apply equally here. Preferably, the Group IA or Group HA metal containing substance is introduced in the first temperature zone or at least before the quench zone. As an option, the Group IA or Group DA metal containing substance can be introduced during or prior or both during and prior to the formation of the precursor. In addition, in this process, a carbon black yielding feedstock can be introduced to the precursor. [0042] With respect to the above processes, one or more features of the processes can be used in a single process. For instance, the second carbon black yielding feedstock can be used to partially quench and the first and second temperature zone difference can be 200°C or more. Any combination of process features as-described herein can be combined. {0043] In the embodiments which involve achieving a difference in temperature of 200° C or more with respect to the first temperature zone and the second temperature zone, and in any other of the embodiments described herein, any means to reduce the temperature between the temperature zones or sxmes where the first carbon black yielding feedstock is introduced compared to where the second carbon black yielding feedstock is introduced can be used For instance, a water jacket can be used around the reactor (or parts thereof) where the second carbon black yielding feedstock is introduced or thereafter. In the alternative, or in combination, steam can be introduced at this point In addition, or in the alternative, other quench agents, such as nitrogen, water, or other suitable quench agents, can be used to achieve a reduction in temperature at the point of where the second carbon black yielding feedstock is introduced or thereafter. Preferably, there is no water jacket or other quench devices or means in the first temperature zone in any of fee embodiments of the present invention and preferably any such quenching occurs just prior, during, or right after introduction of the second carbon black yielding feedstock [0044] Furthermore, with respect to the above processes, preferably, in the first stage where the first carbon black yielding feedstock is introduced, the goal is to maximize surface area. For instance, in the first stage, it is preferably operated to achieve a high surface area such as from about 100 to about 400 mVg based on BET, [0045] In one embodiment of the present invention, the first carbon black yielding feedstock which forms the precursor is eventually coated by the subsequent carbon black yielding feedstock which vaporizes and coats the precursor. [0046] Beneficial carbon black products can be formed, for instance, a carbon black having a DBP range of from about 120 to about 150 cc/lOOg with a total Group IA or Group DA metal content of from about 50 to about 150 ppna can be fonnei Other DBP ranges include from about 90 to about 120 cc/lOOg with a total Group IA or Group HA metal content of from about 100 to about 500 ppm; a DBP range of from about 60 to about 90 cc/lOOg with a Group IA or Group HA metal containing content of from about 200 to about 1,000 ppm; a DBP range of from about 30 to about 60 cc/lOOg, with a total Group IA or Group HA content of from about 500 ppm to about 5,000 ppm. The carbon black of the present invention can have a teachable amount of the Group IA or Group HA metaL For instance, the carbon black can have a teachable Group IA or Group HA metal content of about 20% or less by weight of the Group IA or HA element present, and more preferably 15 weight % or less, 10 weight % or less, 5 weight % or less, 1 weight % or less, or Vz weight % or less. Ranges include, but are not limited to, about 0 weight % to about 20 weight % or about 0.25 weight % to about 10 weight %, The teachable amount can be detooiued by soxbiet extraction of the carbon black followed by analysis of the aqueous extract for potassium* similar in concept to ASTM methods D4527, C871, or EPA methods SW8-1311 and SW84312, In addition, the caibon black can have any porosity amount The carbon black can have a BET surfece aiea (in mVg) to t-area (in ma/g) ratio of 1.5 or less, such as 0.9 to 1.5. In general, preferably, the carbon blacks of the present invention have low levels of microporosity; Also, the carbon black can have a t-area of from about 10 m2/g to about 180 m2/g. Other ranges include from about 30 m2/g to about 150 m^/g and from about 50 m2/g to about 120 m2/g. Generally, the carbon black of the present invention contains no appreciable amount of silicon. [0047] The carbon black of the present invention can be used in any product where conventional carbon black is used such as rubber products, tires, inks, ink jets, toners, gas diffusion electrodes, coatings, plastics, polymers, and the like, [0048] The present invention will be further clarified by the following examples, which are intended to be purely exemplary of the present invention- Examples [0049] In a pilot plant, one embodiment of the carbon black of the present invention was made. In this process, a carbon black reactor, illustrated in Figure 1 and having a design similar to that set forth in U.8. Patent No. 6,403,695, was used Examples 1-7 are outlined in Table 1, In each case, a primary combustion of 140% was used herein this amounts to 40% of an oxygen rich combustion reaction. The primaiy fuel for the combustion reaction was natural gas and introduced to the reactor in Stream 1. Hie natural gas fed to Hie carbon black forming process was about ambient temperature of approximately 77°F, The liquid feedstock utilized was a commercially available feedstock having the typical properties listed in U.S. patent No. 5,190,739. In this process, the first carbon black containing feedstock was introduced- at a first stage in the presence of a stream of hot gases formed by a primary combustion. The first carbon black yielding feedstock was introduced to the process in the varying amounts as shown in Table 1. Once the first carbon black yielding feedstock in the first stage was combined with a stream of hot gases to form a precursor which contained a first carbon black, a second carbon black yielding feedstock was then subsequently introduced downstream. This second carbon black yielding feedstock was introduced without any oxidizing source or fuel source present and was introduced before the quench zone. (0051] In Example 5, an amount of water was introduced between the two feedstock injections in the amount of 100 kg/hr. This water was introduced as a fine spray by means of an pressurized atomizer. [0052] In Example 6, the second carbon black yielding feedstock was split into two equal amounts. The fiist part was introduced at LI of Figure 1 as indicated in Table L The second part was introduced lm downstream. [0053] During the introduction of the first carbon black yielding feedstock, a varied amount of potassium in the form of a potassium acetate solution was introduced in order for the precursor to have a potassium content [0054] The carbon black formed in the reaction was then completely quenched with water downstream of the second carbon black yielding feedstock to form the carbon black product of the present invention. The carbon blacks formed had a t-area, BET areas and DBP absorption shown in Table 1. [0055J Applicants specifically incorporate the entire contents of all cited references in this disclosure. Further, when an amount, concentration, or other value or parameter is given as either a range, preferred range, or a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. Where a range of numerical values is recited herein, unless otherwise stated, the range is intended to include the endpoints thereof, and all integers * and fractions within the range. It is not intended that the scope of the invention be limited to the specific values recited when defining a range. r [0056] Other embodiments of the present invention will be apparent to those skilled in the art from consideration of the present specification and practice of the present invention disclosed herein. It is intended that the present specification and examples be considered as exemplary only with a txue scope and spirit of the invention being mdicated by the following claims and equivalents thereof. WHAT IS CLAIMED IS: 1. A method of making a carbon black product comprising introducing to a reactor a carbon black yielding feedstock in a first stage and combining with a stream of hot gases to form a precursor consists essentially a first carbon black in a reaction stream and them subsequently introducing a second carbon black yielding feedstock to said precursor to partially quench the reaction stream containing the first carbon black and then completely quenching to form said carbon black product 2. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA or Group HA element prior to introduction of said second carbon black yielding feedstock. 3. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA or Group DA element containing substance prior to said completely quenching. 4. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA element prior to introduction of said second carbon black yielding feedstock. 5. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA element prior to said completely quenching. 6. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA or Group HA element in an amount sufficient to have 200 ppm or more in the carbon black product prior to iatrodaction of said second caibon black yielding feedstock. 7. The method of claim 6, wherein said amount is 500 ppm or more, 8. The method of claim 5? wherein said Group IA element comprises potassium. 9. Hie method of claim 53 wherein said Group IA element is potassium. 10. A method of making a carbon black product comprising introducing a carbon black yielding feedstock in a first stage and combining with a stream of hot gases to fbim a precursor comprising a first carbon black and subsequently introducing a second carbon black yielding feedstock to said precursor* wherein said second carbon black yielding feedstock comprises at least 15% by weight of the total amount by weight of caibon black yielding feedstock utilized during said process and further comprising introducing at least one substance containing at least one Group IA or Group HA element prior to formation of said carbon black product 11- The method of claim 10, wherein said second carbon black yielding feedstock is added in two or more segments. 12. The method of claim 10, further comprising introducing at least one substance containing at least one Group IA element prior to formation of said carbon black product. 13. The method of claim 12, wherein said Group IA element comprises potassium. 14. The method of claim 12, wherein said Group IA element is potassium. 15. The method of claim 10, wherein said substance is introduced during or prior to introducing said second carbon black yielding feedstock. 16. The method of claim 10, wherein said substance is introduced prior to introducing said second carbon black yielding feedstock 17. A process of making a carbon black product comprising introducing a first carbon black yielding feedstock in a first stage and combining with a stream of hot gases to form a precursor comprising a first carbon black and subsequently introducing a second carbon black yielding feedstock to said precursor, wherein no oxidizing source and no fuel source is introduced after formation of said precursor, said process further comprising introducing a substance containing at least one Group IA or HA element 18. The method of claim 17, further comprising introducing at least one substance containing at least one Group IA element during or prior to introducing said second carbon black yielding feedstock. 19. The method of claim 17, forthfir comprising introducing at least one substance containing at least one Group IA element during or prior to formation of said precursor. 20. The method of claim 17, further comprising introducing at least one substance containing at least one Group IA or Group HA element during or prior to formation of said precursor. 21. The mefhod of claim 17, wherein said Group IA element comprises potassium. 22. The method of claim 17, wherein said Group IA element is potassium. 23. A method of making a carbon black product comprising forming a precursor consisting essentially of a first carbon black in a first temperature zone and then introducing a carbon black yielding feedstock to said precursor and forming said carbon black product in a second temperature zone before a quench zone, wherein said first temperature zone and second temperature zone have a temperature difference (A) of 200°C or rnore, 24. The method of claim 23, wherein said temperature difference is 300°C or more, 25. The method of claim 23 , wherein said temperature differences from 200°C to about 900°C. 26. The mefhod of claim 235 wherein said temperature differences from about 400°C to about 700°C 27. The method of claim 23, wherein said temperature difference is obtained at least in part by a cooling jacket, water spraying, and/or steam in between said first and second temperature zone. 28. The method of claim 23, wherein no quenching occurs between the forming of said precursor and introducing of said carbon black yielding feedstock 29. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA element before said quench zone. 30. The method of claim 23, farther comprising introducing at least one substance containing at least one Group IA or Group IIA element before said quench zone. 31. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA or Group HA element in said first temperature zone. 32. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA or Group HA element during formation of said precursor, 33. The method of claim 23, further comprising introducing at least one substance containing at least one Group JA or Group HA element prior to formation of said precursor. 34. The method of claim 239 further comprising introducing at least one substance containing at least one Group IA element in said first temperature zone. 35- The method of claim 23, further comprising introducing at least one substance containing at least one Group IA element during formation of said precursor. 36. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA element prior to formation of said precursor. 37. The method of claim 2, wherein said substance is a salt 38. The method of claim 2, wherein said substance is a solution. 39. The method of claim 2, wherein said substance is a compound containing at least one Group IA or Group HA element 40. A carbon black having a DBP range of firom about 120 to about 150 cc/lOOg with a total Group IA or Group IIA element content of from about 50 to about 150 ppm; or a DBP range of from about 90 to about 120 cc/lOOg with a total Group IA or Group HA content of from about 100 to about 500 ppm; or a DBP range of from about 60 to about 90 cc/lOOg with a total Group IA or Group DA content of from about 200 to about 1,000 ppm; or a DBP range of from about 30 to about 60 cc/lOOg with a total Group IA or Group HA content of from about 500 to about 5,000 ppm. 41. The carbon black of claim 40, wherein said carbon black has a leachable Group IA or Group IIA element content of 20% by weight or less. 42. The carbon black of claim 40, wherein said carbon black has a leachable Group IA or Group HA element content of 10 weight % or less. 43. The carbon black of claim 40, wherein said carbon black has a ratio of a BET surface area in m2/g to t-area in m2/g of 1,5 or less. 44. The carbon black of claim 40, wherein said carbon black has a leachable Group IA or Group IIA content of about 0.25 weight % to about 5 weight %, 45. The carbon black of claim 40, wherein said carbon black has a t-area of from about 10 ma/g to about 180 m2/g. 46. The method of claim 103 wherein said substance is a salt 47. The method of claim 103 wherein said substance is a solution. 48. The method of claim 10, wherein said substance is a compound containing at least one Group IA or Group HA element 49. The method of claim 17, wherein said substance is a salt 50. The method of claim 17, wherein said substance is a solution. 51* The method of claim 17, wherein said substance is a compound containing at least one Group IA or Group HA element. 52. The method of any of claims 1 -39 and 46-51, ftrther comprising conducting a partial intermediate quenching prior to introducing said second carbon "black yielding feedstock. 53, The process of claim 10, wherein said second carbon hlack yielding feedstock is from 30% to 60% by weight of the total amount by weight of carbon black yielding feedstock.

Full Text

CARBON BLACK AND MULTI-STAGE PROCESS FOR MAKING SAME
[0001] This application claims the benefit under 35 U.S.C §120 of prior U.S. Patent Application No. 10/838,530 filed May 4S 2004 which is incorporated in its entirety by reference herein.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to carbon black and to processes for making ca&on blacL More particularly, the present invention relates to unique forms of carbon black and to several multi-stage carbon black forming processes.
[0003] The present invention relates to the production of carbon black such as furnace bkcks having many important applications, such as fillers, pigments, and reinforcing agents, in rubbers and plastics. Generally, the furnace process for preparing these blacks entails Hie cracking and/or incomplete combustion of a hydrocarbon feedstock such as natural gas or catalytic cracker cycle stock in a closed conversion zone to produce carbon black. The carbon black entrained in fee gases emanating from the conversion zone is then quenched and collected by any suitable means conventionally used in the art It has, however, been extremely costly to produce carbon blacks having high surface area with increased structure. [0004] US, Patent No. 5,190,739 to MacKay et aL relates, in part, to a process for preparing carbon blacks having lower-than-normal structure at a given surface area and a lower-than-normal surface area at a given overall combustion level. The process can involve the use of a multi-stage furnace wherein a second source of hydrocarbons is added to the stream of hot first-stage gases. Certain embodiments of the 6739 patent also relate to the use of potassium to make low structure carbon blacks. However, foe amount of the auxiliary hydrocarbons used in the '739 patent are considerably lower amounts than in the first stage.

Furthermore, the '739 patent can optionally use additional fuel and/or oxygen to achieve further combustion "Upon the introduction of the auxiliary hydrocarbons. la addition, there is no significant temperature zone difference between the zone where the first feedstock is mtroduced and the zone where the auxiliary feedstock is introduced in the '739 patent [0005] In U.S* Patent No. 4,383,973 to Cheng, this patent relates to a process which involves two carbon hlack reactors in sequence where one of the reactors is jfor a high-structure carbon black and the second is for a low-structure carbon "black. In the one figure of the '973 patent, the reactors are apparently connected together in sequence. However, in this process, additional air and fuel are introduced to the second feedstock and there is no significant temperature difference between the two feedstock introduction zones. Further, there is no partial quenching occurring prior to the complete quenching. The 6973 patent further states that there is no quenching occurring between the first and second carbon black forming zones and further 10 ppm or more potassium can be introduced in the high structure zone. Furthermore, with the high combustion occurring in each feedstock introduction zone, there would not be any significant temperature zone difference between the first carbon black of high structure is formed and the zone where the low structure carbon blackis formed. [0006] In U.S. Patent No. 4,976,945* a process for producing carbon black is described which uses various amounts of alkali metal, such as potassium, in a carbon black reactor to regulate structure. The '945 patent does state that an alkali metal compound and/or alkaline earth metal compound can be added in an amount of 500 to 50,000 ppm relative to the hydrocarbon starting material The 4945 patent does not relate to a multi-stage carbon black forming process and shows no partial quenching occurring prior to the complete quenching. The '945 patent further states that an alkali metal compound is particularly effective far the production of carbon black whe^e the DBP absorption is at most 90 cc/lOOg,

r
[0007] VS. Patent No. 4,822,588 to Gravely et aL relates to a carbon black reactor which has a first reaction zone and a second reaction zone that are serially connected In this process, in the second stage, additianal carbonaceous feedstock is introduced to form a second reaction mixture* hi this process, the goal was to not substantially form carbon black in the first reaction zone. Also, the process didn't use an alkaK metal or tffaflinfl earth metal [0008] Accordingly, there is a need to provide a novel and improved process for preparing carbon blacks which exhibit improved or increased structure with increased surface area, [0009] All of the patents and publications mentioned throughout are incorporated in fteir entirety by reference herein.
BRIEF DESCRIPTION OF THE DRAWINGS [0010] Figure 1 is cross sectional view of a carbon black reactor that can be used in the present invention,
SUMMARY OF THE PRESENT INVENTION [0011] It is therefore a feature of the present invention to provide a method of producing carbon black with high surface area and high structure.
[0012] Aaother feature of the present invention is to provide a method of producing caibon black which is cost effective.
[0013] Additional features and advantages of the present invention will be set forth in part in the description that follows, and in part will be apparent from the description, or may be learned by practice of the present invention. The objectives and other advantages of Hie present invention will be realized and attained by means of the elements and combinations particularly pointed out in the description and appended claims.
[0014] To achieve these and other advantages and m accordance with fixe purposes of the present invention, as embodied and broadly described herein, the present invention relates to a

method of making a carbon black product The method includes introducing a carbon black yielding feedstock in a first stage of a carbon black reactor and combining this feedstock with a stream of hot gases to form a precursor which essentially is a first carbon black and optionally byproducts. Then, a second carbon black yielding feedstock is subsequently introduced to the precursor to at least partially quench the reaction stream containing the first carbon black and then the process includes completely quenching to form fixe carbon black product
I001S] The present invention farther relates to a process of making a carbon black product which includes iatroducing a caibon black yielding feedstock in a first stage of a caxbon black reactor and combining this feedstock with a stream of hot gases to form a precursor. The precursor contains a first carbon black. Then, in the process, a second carbon black yielding feedstock is introduced to the precursor, wherein the second carbon black yielding feedstock contains at least 15% by weight of the total amount by weight of the carbon black yielding feedstock utilized during the entire process,
[0016J In addition, the present invention relates to a process of making a carbon black product which includes introducing a first carbon black yielding feedstock in a first stage of a carbon black reactor and combining this feedstock with a stream of hot gases to form a precursor which contains a first carbon black Then, in the process, a second carbon black yielding feedstock is introduced to the precursor, wherein no oxidizing sotnce and no fiiel source are introduced after formation of the precursor,
[0017] Furthermore, the present invention relates to a process of making a carbon black product which includes forming a precursor which contains a first carbon black in a first temperature zone and then forming a carbon black product from this precursor in a second temperature zone before a quench zone. The first temperature zone and the second temperature

zone have a temperature difference of 200°C or more.
[0018] In each of these processes, the process can* include the introduction of at least one
substance containing at least one Group IA or Group HA element at one or more locations of
the process,
[0019] Also, the present invention relates to a carbon black having a DBF range of from
about 30 to about 150 cc/lOOg with a total Group LA or Group DA element content of from
about 50 to about 5,000 ppm. The carbon black can have other physical or chemical attributes
including, but not limited tos a leachable Group IA or Group HA content, a porosity amount,
and desirable t-area such as a t-area of from about 10 to about 180 m2/g. Other characteristics
are farther described herein.
[0020] It is to be understood that both the foregoing general description and the following
detailed description axe exemplary and explanatory only and are intended to provide a ftdher
explanation of the present invention, as claimed
DETAILED DESCRIPTION OF THE PRESENT INVEmiON [0021] The present invention relates to carbon black products as well as various methods of making carbon black products. In the preferred embodiments, the methods of making the carbon black product involves the use of a multi-stage carbon black reactor. More preferably, the multi-stage reactor has at least two stages (two, three, four, or more stages) where generally there are at least two feedstock (e.g., two, three, four, or more feedstocks) introductions occurring. The carbon black product is preferably a furnace black. [0022] In more detail, in one embodiment of the present invention, the present invention relates to a method of making a carbon black product which involves introducing a carbon blade yielding feedstock in a first stage of a carbon black reactor. The carbon black yielding

feedstock is combined with a stream of hot gases to form a precursor. The precursor is or at least contains a first carbon black A second carbon black yielding feedstock is then subsequently introduced into the carbon black reactor downstream of the first stage and this second carbon black yielding feedstock k preferably introduced in the presence of the precursor formed in the first stage. Li this method, the second carbon black yielding feedstock at least partially quenches the reactions that are occurring. Afterwards, the complete quenching can occur downstream, wherein the carbon forming reactions are completely stopped or quenched and a carbon black product is formed, [0023] For purposes of this method as well as the other methods described herein* a multi-stage carbon black reactor can be used such as the ones described in U.S. Patent No, 4,383,973, UJ3. Patent No. 5,190,739, U.S. Patent No. 5,877,251, U.S. Patent No. 6,153,684, or U.S. Patent No. 6,403,695, all of which are incorporated in their entirety by reference herein. Thus, the present invention can use a multi-stage furnace process. [0024] The carbon black yielding feedstock can be any conventions] carbon black yielding feedstock which results in the formation of carbon black For instance, any hydrocarbon material can be used. A suitable feedstock can be any carbon black-yielding hydrocarbon feedstock which is readily volatilizable under the conditions of the reaction. ,For example, unsaturated hydrocarbons such as acetylene; olefins such as ediylene, propylene, butylene; aromatics such as benzene, toluene and xylene; certain saturated hydrocarbons; and other hydrocarbons such as kerosenes, naphthalenes, teipenes, ethylene tars, aromatic cycle stocks and the like may be used
[0025] With respect to the stream of hot gases that is combined with the carbon black yielding feedstock, the stream of hot gases can also be consideied hot combustion gases that can be generated by contacting a solid, liquid, and/or gaseous fuel with a suitable oxidant

stream such as, but not limited to, air, oxygen, mixtures of air and oxygen, or the like. Alternatively, a preheated oxidant stream may be passed through without adding a liquid or gaseous fuel. Examples of the fiiel suitable for use in contacting the oxidant stream to generate the hot gases include any of the readily combustible gas, vapor, or liquid streams, such as natural gas, hydrogen, carbon monoxide, methane, acetylene, alcohol, or kerosene. Generally, it is preferred to use fuels having a high content of carbon-containing components and in particular, hydrocarbons- The ratio of air to fiiel utilized to produce the carbon blacks of the present invention may be from about 1;1 (stiochiometric ratio) to infinity. As stated, to facilitate the generation of hot gases, the oxidant stream may be preheated.
[0026] The general process of forming carbon black through the use of a multi-stage reactor and achieving appropriate hot gases to form carbon black are described in the above-identified referenced patents which are incorporated by reference herein and can be applied in the present invention with the changes described herein* in one embodiment of the present invention, surface area is maximized by maintaining high temperature preferably after introduction of the first carbon black yielding feedstock, such as by no water cooling, rapid mixing of the hot gases with the carbon black yielding feedstock, and/or short mixing lengths, and the like.
{0027] The present invention can be practiced using any suitable carbon black producing reactor. Figure 1, for example, illustrates a cross-section of one example of such a reactor. Reactors of this type generally use a combustion gas which is mixed with an oxidant such as air. The gas mixture is generally introduced into a combustion chamber and ignited by any suitable method. Gas flow is left to right (direction A) in Figure 1. Once ignited, the hot gas mixture can be moved through the reactor, and "brought into contact with a hydrocarbon

feedstock suitable for producing carbon black in Figure X, and simply as an example, fuel can be introduced at location 1 and oxidant can be introduced at location 2. Other locations are possible. The first location 3 (one or more) is an example of a point of intcoduction of the first carbon black yielding feedstock. The second and third location 3 axe examples of points of introduction of the second carbon black yielding feedstock. Location 4 is an example of a suitable location of a partial quenching agent, like water. Location 5 is an example of a suitable location for complete quenching. The double parallel lines signify that the reactor can be any length. The various D numbers represent various lengths of the reactor. Dl through D8 can be any suitable diameter and can be the same or different For instance, D2 can be less than Dl and D8, and Dl and D8 can be the same or different. Zone LI or zone L2 are examples of the first temperature zone, and zone L3 is an example of the second temperature zone. If a partial quench agent is used at for instance point 4, then the first temperature zone is typically LI.
[0028] Generally, carbon black-yielding feedstock can be injected into a reactor by a plurality of streams 3 (in L-2)? shown in Figure 1, which penetrate into the interior regions of the hot combustion gas stream, to insure a high rate of mixing and shearing of the hot combustion gases and the carbon black-yielding feedstock. This insures that the feedstock rapidly and completely decomposes and converts into a first carbon black material. [0029] The precursor fonned in the methods described herein contains a first carbon black and can contain other components such as unused fuel or oxidants or combustion products and can also contain other components such as, but not limited toa inorganic substances, metals, salts, and metal oxides. Primarily, the precursor is a carbon black product For instance, 80 to 99% and, more preferably, 95% to 99% or greater (e,g,, 100%) by weight of the precursor is carbon black.

[0030] With respect to the subsequent introduction of a second carbon black yielding feedstock to the precursor containing the first carbon black, this second carbon black yielding feedstock is added downstream of the first stage in an amount to at least partially quench the reactions that are still occurring from the first stage- For purposes of the present invention, the partial quenching of the reactions means that this introduction of the second carbon black yielding feedstock is not a complete quenching of the reactions but quenches a portion of the reactions. Preferably, the introduction of the second carbon black yielding feedstock does not completely quench the reactions. The second caibon black yielding feedstock can be the same type of feedstock or a different feedstock firom the carbon black yielding feedstock introduced in the first stage.
[0031] The above-identified patents provide various carbon black forming conditions and starting amounts that can be used in the formation of the precursor. [0032] The carbon black yielding feedstock introduced in either stage can be introduced in any conventional way such as a single stream or plurality of streams and the introduction of the feedstocks can occur at any rate. With a plurality of streams, the rates for each stream can be the same or different.
[0033] Preferably, the subsequent introduction of the carbon black yielding feedstock to the precursor is done by a plurality of streams. Any manner in which the second carbon black yielding feedstock can be introduced can be used.
[0034] After the mixture of hot combustion gases and carbon black-yielding feedstock is quenched, the cooled gases pass downstream into any conventional cooling and separating means whereby the carbon black is recovered. The separation of the carbon black firom the gas stream is readily accomplished by conventional means such as a precipitator, cyclone separator or bag filter. With respect to completely quenching the reactions to form

the final carbon black product any conventional means to quench the reaction downstream of the introduction of the second carbon black yielding feedstock can be used and is known to those skilled in the art. For instance, a quenching fluid can be injected which may be water or other suitable fluids to stop the chemical reaction.
(0035] In an embodiment of the present invention, the method farther includes introducing at least one substance that is or that contains at least one Group IA or Group HA element (or ion thereof) of the Periodic Table, Preferably., the substance contains at least one alkali metal or alkaline earth metal. Examples include lithium, sodium, potassium, rubidium, cesium, francium, calcium, barium, strontium, or radium, or combinations thereof. Any mixtures of one or more of these components can be present in the substance. The substance can be a solid, solution* dispersion, gas, or any combinations thereof More than one substance having the same or different Group IA or Group HA metal can be used. If multiple substances are used, the substances can be added together separately, sequentially, or in different reaction locations. For purposes of the present invention, the substance can be the metal (or metal ion) itself, a compound containing one or more of these elements, including a salt containing one or more of these elements, and the like. Preferably, the substance is capable of introducing a metal or metal ion into the reaction that is ongoing to form the carbon black product Fox purposes of the present invention, preferably, tbe substance is introduced prior to the complete quenching as described above. For instance, the substance can be added at any point prior to the complete quenching, including prior to the introduction of the carbon black yielding feedstock in the first stage; during the introduction of the carbon black yielding feedstock in the first stage; after the introduction of the carbon black yielding feedstock in the first stage; prior to, during, or immediately after the introduction of the second carbon black yielding feedstock to the precursor; or any

step after the introduction of the second carbon black yielding feedstock but prior to the complete quenching. More than one point of introduction of the substance can be used. Preferably, the introduction of the substance is prior to the introduction of the second carbon black yielding feedstock and/or during or right after the introduction of the carbon black yielding feedstock in the first stage. The amount of the Group IA or Group HA metal containing substance can be any amount as long as a carbon black product can be formed. For instance, the amount of the substance can be added in an amount such that 200 ppm or more of the Group IA or Group IIA element is present in the carbon black product ultimately formed. Other amounts include from about 200 ppm to about 5000 ppm or more and other ranges can be from about 300 ppm to about 1000 ppm, or from about 500 ppm to about 1000 ppm of the Group IA or Group HA element present in the carbon black product that is formed These levels can be with respect to the metal ion concentration. As stated, these amounts of the Group IA or Group HA element present in the carbon black product that is formed can be with respect to one element or more than one Group IA or Group HA element and would be therefore a combined amount of the Group IA or Group HA elements present in the carbon black product that is formed. The substance can be added in any fashion including any conventional means. In other words, the substance can be added in the same manner that a carbon black yielding feedstock is introduced. The substance can be added as a gas, liquid, or solid, or any combination thereof. The substance can be added at one point or several points and can be added as a single stream or a plurality of streams. The substance can be mixed in with the feedstock, fuel, and/or oxidant prior to or during their introduction.
[0036] One method by which a substance containing at least one Group IA ox Group HA element such as, for example, potassium can be introduced into fee feedstock is by the

incorporation of fee substance into the feedstock. Upon combustion, the metal ions can become uniformly incorporated into the carbon black. The charge of metal ions provides a repulsive force between individual carbon black particles. Has repulsive force can keep particles from aggregating, thus decreasing fee overall structure of the carbon black. [0037] The application of additional feedstock to the preexisting carbon black particles may be repeated any number of times until fee reaction of feedstock to carbon black ceases. Each time additional feedstock is added, fee temperature of fee entire reaction mixture generally goes down, and carbon black particle size increases. In this way fee feedstock can act as a quenching agent for fee cooling of fee carbon black.
[00381 In another embodiment of fee present invention, fee present invention also relates to a method of making a carbon black product wherein a carbon black yielding feedstock is introduced in a first stage and combined wife a stream of hot gases to form a precursor. Furfeermoie, a second carbon black yielding feedstock is subsequently introduced downstream to fee precursor, Thus this method is, up to this point, fee same as fee above-described embodiment and therefore fee same conditions and examples would apply to this process. Furthermore, in this process* fee second carbon black yielding feedstock contains at least 15 % by weight of the total amount of fee carbon black yielding feedstock utilized during fee entire process. The second carbon black yielding feedstock can contain from about 15% by weight to about 80% by weight of fee total amount of fee carbon black yielding feedstock utilized during fee entire process. Other ranges include from about 25% to about 70% or from about 30% to about 60% by weight of fee total amount by weight of fee carbon black yielding feedstock utilized during fee eaitire process, The introduction of fee second carbon black yielding feedstock can be introduced in two ot more segments, or stages wherein the segments can be downstream from the first segment This is quite different from previous multi-stage

processes where any subsequent introduction of a carbon black yielding feedstock would be a veiy low amount such as on the order of 10% by weight or lower. This large amount of the second carbon black yielding feedstock leads to beneficial carbon black products as to be described later. Also, this amount of carbon black can serve as a partial quenching of the reactions that are occurring.
f0039] As in the first described process, a substance that is or contains a Group IA or Group HA element or ion thereof can be added in the same manner as described above. These above-described details apply equally here.
[0040] In another embodiment of the present invention, the present invention relates to a process of making a carbon black product wherein a first carbon black yielding feedstock is introduced in a first stage and combined with a stream of hot gases to form a precursor as with respect to the first and second above-described processes. A second carbon black yielding feedstock is then introduced to the precursor and in this process, no oxidizing source and no fuel source are introduced after formation of the precursor. Urns, in this process, any oxidizing source and/or fuel source are only introduced prior to the introduction of the first carbon black yielding feedstock or during the introduction of the first carbon black yielding feedstock. Again, this is quite different from previous processes where typically, if a second carbon black yielding feedstock is introduced; sufficient fuel and an oxidizing source are added to promote sufficient pyrolysis of the second carbon black yielding feedstock, Again, as with the previous processes, at least one Group IA or Group DA metal containing substance can be introduced in the same manner as described above and these details apply equally here, [0041] In another embodiment of the present invention, the present invention relates to a process of making a carbon black product wherein a precursor containing a first carbon black is formed in a first temperature zone of a carbon black reactor and then a carbon black yielding

feedstock can be introduced to the precursor* The method then involves farming a carbon black product in a second temperature zone which is located before a quench zone. In Ibis process, the first temperature zone and the second temperature zoue have a temperature difference of 200°C or more, and preferably a temperature difference of 300°C or more-Suitable ranges with respect to the temperature difference can be, for instance, from about 200°C to about 900°C or from about 400° to about 700°G Other temperature ranges with regard to the temperature difference can be used. Generally, with respect to this temperature difference, the first temperature zone has the higher temperature and the second temperature zone has the lower temperature thus creating the temperature difference though this is a preferred embodiment only, The difference in temperatures can be achieved any number of ways such as avoiding any further introduction of combustion gases or avoiding or minimizing formation of combustion gases in the second temperature zone. Other means to achieve ibis difference can be used. Again, as with the previous embodiments, a Group IA or Group HA metal containing substance can be used and introduced in the same manner as described above and the details as set forth above apply equally here. Preferably, the Group IA or Group HA metal containing substance is introduced in the first temperature zone or at least before the quench zone. As an option, the Group IA or Group DA metal containing substance can be introduced during or prior or both during and prior to the formation of the precursor. In addition, in this process, a carbon black yielding feedstock can be introduced to the precursor. [0042] With respect to the above processes, one or more features of the processes can be used in a single process. For instance, the second carbon black yielding feedstock can be used to partially quench and the first and second temperature zone difference can be 200°C or more. Any combination of process features as-described herein can be combined. {0043] In the embodiments which involve achieving a difference in temperature of 200° C

or more with respect to the first temperature zone and the second temperature zone, and in any other of the embodiments described herein, any means to reduce the temperature between the temperature zones or sxmes where the first carbon black yielding feedstock is introduced compared to where the second carbon black yielding feedstock is introduced can be used For instance, a water jacket can be used around the reactor (or parts thereof) where the second carbon black yielding feedstock is introduced or thereafter. In the alternative, or in combination, steam can be introduced at this point In addition, or in the alternative, other quench agents, such as nitrogen, water, or other suitable quench agents, can be used to achieve a reduction in temperature at the point of where the second carbon black yielding feedstock is introduced or thereafter. Preferably, there is no water jacket or other quench devices or means in the first temperature zone in any of fee embodiments of the present invention and preferably any such quenching occurs just prior, during, or right after introduction of the second carbon black yielding feedstock
[0044] Furthermore, with respect to the above processes, preferably, in the first stage where the first carbon black yielding feedstock is introduced, the goal is to maximize surface area. For instance, in the first stage, it is preferably operated to achieve a high surface area such as from about 100 to about 400 mVg based on BET,
[0045] In one embodiment of the present invention, the first carbon black yielding feedstock which forms the precursor is eventually coated by the subsequent carbon black yielding feedstock which vaporizes and coats the precursor.
[0046] Beneficial carbon black products can be formed, for instance, a carbon black having a DBP range of from about 120 to about 150 cc/lOOg with a total Group IA or Group DA metal content of from about 50 to about 150 ppna can be fonnei Other DBP ranges include from about 90 to about 120 cc/lOOg with a total Group IA or Group HA metal content

of from about 100 to about 500 ppm; a DBP range of from about 60 to about 90 cc/lOOg with a Group IA or Group HA metal containing content of from about 200 to about 1,000 ppm; a DBP range of from about 30 to about 60 cc/lOOg, with a total Group IA or Group HA content of from about 500 ppm to about 5,000 ppm. The carbon black of the present invention can have a teachable amount of the Group IA or Group HA metaL For instance, the carbon black can have a teachable Group IA or Group HA metal content of about 20% or less by weight of the Group IA or HA element present, and more preferably 15 weight % or less, 10 weight % or less, 5 weight % or less, 1 weight % or less, or Vz weight % or less. Ranges include, but are not limited to, about 0 weight % to about 20 weight % or about 0.25 weight % to about 10 weight %, The teachable amount can be detooiued by soxbiet extraction of the carbon black followed by analysis of the aqueous extract for potassium* similar in concept to ASTM methods D4527, C871, or EPA methods SW8-1311 and SW84312, In addition, the caibon black can have any porosity amount The carbon black can have a BET surfece aiea (in mVg) to t-area (in ma/g) ratio of 1.5 or less, such as 0.9 to 1.5. In general, preferably, the carbon blacks of the present invention have low levels of microporosity; Also, the carbon black can have a t-area of from about 10 m2/g to about 180 m2/g. Other ranges include from about 30 m2/g to about 150 m^/g and from about 50 m2/g to about 120 m2/g. Generally, the carbon black of the present invention contains no appreciable amount of silicon.
[0047] The carbon black of the present invention can be used in any product where conventional carbon black is used such as rubber products, tires, inks, ink jets, toners, gas diffusion electrodes, coatings, plastics, polymers, and the like,
[0048] The present invention will be further clarified by the following examples, which are intended to be purely exemplary of the present invention-

Examples
[0049] In a pilot plant, one embodiment of the carbon black of the present invention was made. In this process, a carbon black reactor, illustrated in Figure 1 and having a design similar to that set forth in U.8. Patent No. 6,403,695, was used Examples 1-7 are outlined in Table 1, In each case, a primary combustion of 140% was used herein this amounts to 40% of an oxygen rich combustion reaction. The primaiy fuel for the combustion reaction was natural gas and introduced to the reactor in Stream 1. Hie natural gas fed to Hie carbon black forming process was about ambient temperature of approximately 77°F, The liquid feedstock utilized was a commercially available feedstock having the typical properties listed in U.S. patent No. 5,190,739. In this process, the first carbon black containing feedstock was introduced- at a first stage in the presence of a stream of hot gases formed by a primary combustion. The first carbon black yielding feedstock was introduced to the process in the varying amounts as shown in Table 1. Once the first carbon black yielding feedstock in the first stage was combined with a stream of hot gases to form a precursor which contained a first carbon black, a second carbon black yielding feedstock was then subsequently introduced downstream. This second carbon black yielding feedstock was introduced without any oxidizing source or fuel source present and was introduced before the quench zone.

(0051] In Example 5, an amount of water was introduced between the two feedstock
injections in the amount of 100 kg/hr. This water was introduced as a fine spray by means of
an pressurized atomizer.
[0052] In Example 6, the second carbon black yielding feedstock was split into two equal
amounts. The fiist part was introduced at LI of Figure 1 as indicated in Table L The second
part was introduced lm downstream.
[0053] During the introduction of the first carbon black yielding feedstock, a varied
amount of potassium in the form of a potassium acetate solution was introduced in order for
the precursor to have a potassium content
[0054] The carbon black formed in the reaction was then completely quenched with water
downstream of the second carbon black yielding feedstock to form the carbon black product of
the present invention. The carbon blacks formed had a t-area, BET areas and DBP absorption
shown in Table 1.
[0055J Applicants specifically incorporate the entire contents of all cited references in this
disclosure. Further, when an amount, concentration, or other value or parameter is given as
either a range, preferred range, or a list of upper preferable values and lower preferable values,
this is to be understood as specifically disclosing all ranges formed from any pair of any upper
range limit or preferred value and any lower range limit or preferred value, regardless of
whether ranges are separately disclosed. Where a range of numerical values is recited herein,
unless otherwise stated, the range is intended to include the endpoints thereof, and all integers
*
and fractions within the range. It is not intended that the scope of the invention be limited to

the specific values recited when defining a range.
r
[0056] Other embodiments of the present invention will be apparent to those skilled in the art from consideration of the present specification and practice of the present invention disclosed herein. It is intended that the present specification and examples be considered as exemplary only with a txue scope and spirit of the invention being mdicated by the following claims and equivalents thereof.

WHAT IS CLAIMED IS:
1. A method of making a carbon black product comprising introducing to a reactor a carbon black yielding feedstock in a first stage and combining with a stream of hot gases to form a precursor consists essentially a first carbon black in a reaction stream and them subsequently introducing a second carbon black yielding feedstock to said precursor to partially quench the reaction stream containing the first carbon black and then completely quenching to form said carbon black product
2. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA or Group HA element prior to introduction of said second carbon black yielding feedstock.
3. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA or Group DA element containing substance prior to said completely quenching.
4. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA element prior to introduction of said second carbon black yielding feedstock.
5. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA element prior to said completely quenching.

6. The method of claim 1, further comprising introducing at least one substance containing at least one Group IA or Group HA element in an amount sufficient to have 200 ppm or more in the carbon black product prior to iatrodaction of said second caibon black yielding feedstock.
7. The method of claim 6, wherein said amount is 500 ppm or more,
8. The method of claim 5? wherein said Group IA element comprises potassium.
9. Hie method of claim 53 wherein said Group IA element is potassium.
10. A method of making a carbon black product comprising introducing a carbon black yielding feedstock in a first stage and combining with a stream of hot gases to fbim a precursor comprising a first carbon black and subsequently introducing a second carbon black yielding feedstock to said precursor* wherein said second carbon black yielding feedstock comprises at least 15% by weight of the total amount by weight of caibon black yielding feedstock utilized during said process and further comprising introducing at least one substance containing at least one Group IA or Group HA element prior to formation of said carbon black product
11- The method of claim 10, wherein said second carbon black yielding feedstock is added in two or more segments.

12. The method of claim 10, further comprising introducing at least one substance containing at least one Group IA element prior to formation of said carbon black product.
13. The method of claim 12, wherein said Group IA element comprises potassium.
14. The method of claim 12, wherein said Group IA element is potassium.
15. The method of claim 10, wherein said substance is introduced during or prior to introducing said second carbon black yielding feedstock.
16. The method of claim 10, wherein said substance is introduced prior to introducing said second carbon black yielding feedstock
17. A process of making a carbon black product comprising introducing a first carbon black yielding feedstock in a first stage and combining with a stream of hot gases to form a precursor comprising a first carbon black and subsequently introducing a second carbon black yielding feedstock to said precursor, wherein no oxidizing source and no fuel source is introduced after formation of said precursor, said process further comprising introducing a substance containing at least one Group IA or HA element
18. The method of claim 17, further comprising introducing at least one substance containing at least one Group IA element during or prior to introducing said second carbon black yielding feedstock.

19. The method of claim 17, forthfir comprising introducing at least one substance containing at least one Group IA element during or prior to formation of said precursor.
20. The method of claim 17, further comprising introducing at least one substance containing at least one Group IA or Group HA element during or prior to formation of said
precursor.
21. The mefhod of claim 17, wherein said Group IA element comprises potassium.
22. The method of claim 17, wherein said Group IA element is potassium.
23. A method of making a carbon black product comprising forming a precursor consisting essentially of a first carbon black in a first temperature zone and then introducing a carbon black yielding feedstock to said precursor and forming said carbon black product in a second temperature zone before a quench zone, wherein said first temperature zone and second temperature zone have a temperature difference (A) of 200°C or rnore,
24. The method of claim 23, wherein said temperature difference is 300°C or more,
25. The method of claim 23 , wherein said temperature differences from 200°C to about 900°C.
26. The mefhod of claim 235 wherein said temperature differences from about 400°C to
about 700°C

27. The method of claim 23, wherein said temperature difference is obtained at least in part by a cooling jacket, water spraying, and/or steam in between said first and second temperature zone.
28. The method of claim 23, wherein no quenching occurs between the forming of said precursor and introducing of said carbon black yielding feedstock
29. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA element before said quench zone.
30. The method of claim 23, farther comprising introducing at least one substance containing at least one Group IA or Group IIA element before said quench zone.
31. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA or Group HA element in said first temperature zone.
32. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA or Group HA element during formation of said precursor,
33. The method of claim 23, further comprising introducing at least one substance containing at least one Group JA or Group HA element prior to formation of said precursor.
34. The method of claim 239 further comprising introducing at least one substance containing at least one Group IA element in said first temperature zone.

35- The method of claim 23, further comprising introducing at least one substance containing at least one Group IA element during formation of said precursor.
36. The method of claim 23, further comprising introducing at least one substance containing at least one Group IA element prior to formation of said precursor.
37. The method of claim 2, wherein said substance is a salt
38. The method of claim 2, wherein said substance is a solution.
39. The method of claim 2, wherein said substance is a compound containing at least one Group IA or Group HA element
40. A carbon black having a DBP range of firom about 120 to about 150 cc/lOOg with a total Group IA or Group IIA element content of from about 50 to about 150 ppm; or
a DBP range of from about 90 to about 120 cc/lOOg with a total Group IA or Group HA content of from about 100 to about 500 ppm; or
a DBP range of from about 60 to about 90 cc/lOOg with a total Group IA or Group DA content of from about 200 to about 1,000 ppm; or
a DBP range of from about 30 to about 60 cc/lOOg with a total Group IA or Group HA content of from about 500 to about 5,000 ppm.
41. The carbon black of claim 40, wherein said carbon black has a leachable Group IA
or Group IIA element content of 20% by weight or less.

42. The carbon black of claim 40, wherein said carbon black has a leachable Group IA or Group HA element content of 10 weight % or less.
43. The carbon black of claim 40, wherein said carbon black has a ratio of a BET
surface area in m2/g to t-area in m2/g of 1,5 or less.
44. The carbon black of claim 40, wherein said carbon black has a leachable Group IA or Group IIA content of about 0.25 weight % to about 5 weight %,
45. The carbon black of claim 40, wherein said carbon black has a t-area of from about 10 ma/g to about 180 m2/g.
46. The method of claim 103 wherein said substance is a salt
47. The method of claim 103 wherein said substance is a solution.
48. The method of claim 10, wherein said substance is a compound containing at least one Group IA or Group HA element
49. The method of claim 17, wherein said substance is a salt
50. The method of claim 17, wherein said substance is a solution.

51* The method of claim 17, wherein said substance is a compound containing at least one Group IA or Group HA element.
52. The method of any of claims 1 -39 and 46-51, ftrther comprising conducting a partial
intermediate quenching prior to introducing said second carbon "black yielding feedstock.
53, The process of claim 10, wherein said second carbon hlack yielding feedstock is
from 30% to 60% by weight of the total amount by weight of carbon black yielding
feedstock.

Documents:

4054-CHENP-2006 AMENDED PAGES OF SPECIFICATION 12-12-2012.pdf

4054-CHENP-2006 AMENDED CLAIMS 03-02-2012.pdf

4054-CHENP-2006 AMENDED CLAIMS 07-02-2013.pdf

4054-CHENP-2006 AMENDED CLAIMS 12-12-2012.pdf

4054-CHENP-2006 ASSIGNMENT 07-02-2013.pdf

4054-CHENP-2006 ASSIGNMENT 12-12-2012.pdf

4054-CHENP-2006 OTHER PATENT DOCUMENT 07-02-2013.pdf

4054-CHENP-2006 CORRESPONDENCE OTHERS 03-02-2012.pdf

4054-CHENP-2006 CORRESPONDENCE OTHERS 05-02-2013.pdf

4054-CHENP-2006 CORRESPONDENCE OTHERS 07-02-2013.pdf

4054-CHENP-2006 EXAMINATION REPORT REPLY RECEIVED 12-12-2012.pdf

4054-CHENP-2006 FORM-1 12-12-2012.pdf

4054-CHENP-2006 FORM-3 12-12-2012.pdf

4054-CHENP-2006 OTHER PATENT DOCUMENT 12-12-2012.pdf

4054-CHENP-2006 POWER OF ATTORNEY 03-02-2012.pdf

4054-chenp-2006-abstract.pdf

4054-chenp-2006-claims.pdf

4054-chenp-2006-correspondnece-others.pdf

4054-chenp-2006-description(complete).pdf

4054-chenp-2006-drawings.pdf

4054-chenp-2006-form 1.pdf

4054-chenp-2006-form 26.pdf

4054-chenp-2006-form 3.pdf

4054-chenp-2006-form 5.pdf

4054-chenp-2006-pct.pdf

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Patent Number

255480

Indian Patent Application Number

4054/CHENP/2006

PG Journal Number

09/2013

Publication Date

01-Mar-2013

Grant Date

26-Feb-2013

Date of Filing

03-Nov-2006

Name of Patentee

CABOT CORPORATION

Applicant Address

TWO SEAPORT LANE, SUITE 1300, BOSTON, MASSACHUSSETTS 02210-2019, USA

Inventors:

#	Inventor's Name	Inventor's Address
1	SIFLEET, WILLIAM, L	120 SOUTH MEADOW ROAD, CLINTON, MA 01510, USA
2	DAVIS, SHELDON, B	9 SPENCER DRIVE, NASHUA, NJ 03062, USA
3	TERRDE, FRTANCOIS, MARIE	51, RUE PAUL LOUIS COURIER, F-92500 RUEIL MALMAISON, FRANCE
4	GAUDET, GREGORY, T	119 NONSET PATH, ACTON, MA 01720, USA
5	KUTSOVSKY, YAKOV, E	9 SORENSON COURT, ARLINGTON, MA 02474, USA

PCT International Classification Number

C09C 1/00

PCT International Application Number

PCT/US05/15189

PCT International Filing date

2005-05-03

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1	10/838,530	2004-05-04	U.S.A.