Title of Invention

AN IMPROVED PROCESS FOR ON-LINE COTTON CRUDE MISCELLA REFINING

Abstract

Miscella Refining process for Cotton Oil" is an on-line process followed by distillation and de solventisation, the said process particularly relates to in the field of cotton crude oil refinery process, the entire refining process is being done at single step each in order to improve the yield, and finished product in terms of quality and quantity and completely avoids discharge of trade effluents from the process. The said process and its method is being implemented in large commercial scale and established commercially.

Full Text

FORM - 2 The Patent Act, 1970 (39 of 1970) Complete Specification (Section 10; Rule 13) Title: -An improved process for Cotton Oil Miscella Refining, M/s. ABHAY COATEX PRIVATE LIMITED., 31 Gur Market Old Mondha, Near Bus stand, JALNA-431203.Maharashtra State, INDIA. The following specification describes the invention, and the manner in which it is to be performed Title:-An improved process of COTTON OIL MISCELLA REFINING, Field of the invention:- The present invention relates to an improved process for cotton oil miscella refining, in the filed refining of cotton crude oil, the said process replaces the conventional or traditional method of chemical refining of cotton crude oil and avoids multi stage operations, the same is being done in single step while in crude miscella stage with a wide range of concentration, saves enormous time, resources, yield, improves product quality and operational efficiency. Based on the cotton seed storage condition and its different varieties, crude cotton oil produced has a very strong high units red colour pigments with a specific taste. Cotton Crude Miscella refining process is followed normally after completion of direct cotton Meat Extraction process, the said process particularly relates to in the field of cotton oil chemical refinery process in miscella stage (oil + solvent), the refining of cotton miscella is being done efficiently in order to improvise the yield, and finished product in terms of quality and quantity and completely avoids discharge of trade effluents from the process. Uniquely produced by-product called salty based soap stock either being added to De oiled meal while toasting or to send for clesolvenisation process by stripping method to produce soap as by product without solvent. Hence produced De oiled meal has its own nutritional merits. The said process and its method is being implemented in large commercial scale and established commercially. The process is being first of its kind in India operating successfully. Back Ground / Prior Art:- In the cotton seed producing countries, the traditional methods of cottonseed processing and chemical refining of crude oil is in traditional method which gives enormous quantity of effluents and stage wise operation which is adversely affecting and rendering a revenue loss of Rs 1000 to Rs 1500 per ton of seed processed. There is an approximately an estimated loss of over Rs.1000 Crore (USD 220 Million) annually due to adoption of conventional processing methods which are inefficient and evolves more trade effluents gives thread to environment consistently. In order to solve the draw backs associated with prior art or traditional methods of refining process an alleged invention has been made an attempt to solve the persistent problems faced by the industry for years. Traditional Process of cotton oil extraction and its disadvantage; Cottonseed crude oil can be processed either in a traditional method by way of pre heating, filtration, water / acid degumming, first cut caustic neutralization, second cut caustic neutralization, hot water washing followed by vacuum drying, in which process the loss of oil and discharge of effluent are very huge, therefore an alleged invention which saves and recovers of 1 to 3% of precious oil on seed basis along with other savings on utilities, manpower cost. No additional chemicals are needed for Effluent treatment plant operation. Objects of the invention:- The main object of the present invention is that, the alleged improved process saves the chemicals, manpower, including financial, other natural resources etc. Further very important object of the present invention is that, which discharges zero effluent discharge to the environment, resulting an environment friendly process. Being an important object of the present invention that the continuous miscella refining of cotton crude oil at miscella stage, gives an greater edge in the process to minimize the process loss, will yield higher quantities of better quality products, economical viable process with adequate safety norms. Further important object of the present invention is that there is a no saponification loss due to adopting of single step neutralization of crude miscella unlike re-refining (second step caustic neutralization step) involved in traditional processing methods. Further important object of the present invention is that the process losses are at lower compare to the existing traditional processing methods as the density difference in between the crude miscella and the obtained soap are more compare to traditional process where the difference of density in between the crude oil and formed soap is very close. The density differences are being caused to minirnize the soap separation easily and lessened the process losses and renders higher recovery levels of this new process. Further important object of the present invention is that there is no emulsification losses due to non usage of exclusive process water (of hot or cold) step unlike involved in traditional processing methods where separate water washing step is involved, due to uniqueness of this final yield of neutral oil increases same time no discharge of effluents. Further important object of the present invention is that the final neutral oil quality is improved with lessened color fixed oil or lessened charred red color pigments which displays excellent bleachability characteristics and gives superior product, a new and Inventive process, Further important object of the present invention is that, it is easy to process darkish or brownish colored quality of crude miscella obtained by processing darkened or long stored cotton seed with high FFA or brownish colored - fixed oil which normally gets at end of any season which renders better yields than traditionally followed methods. However the final quality of the neutral oil will be superior to match all the specifications. Further important object of the present invention is that, no trade effluent waters are evolved from the plant due to its internal process design and parameters, this saves no usage of chemicals for treatment in ETP, being zero discharge. Further important object of the present invention is that the consumption of various utilities, chemicals, foot print required & power consumption are at lower than traditional process methods which saves_and increases the revenues to any processor. Description of the Invention- The Cotton seed crude oil or miscella contains foreign matters like free fatty acids (ranging from 1.0 to 15 % range), with moisture levels of 0.1 to 2% (w/w), impurities up to 2% (w/w) . phopotides (non-hydratable and hydratable gums) with different color pigments of red, yellow & blue, which all these impurities (both chemical & physical) are to be removed effectively.An alleged invention relates on-line Cotton Crude Miscella Refinery process, comprising the following steps. A) Crude Miscella Extraction & Adjustment of Concentration by Distillation: In a continuous solvent extraction process such extracted crude cotton oil will be distillated in a specially designed heat exchanger cum evaporator which will adjust the crude miscella concentration to a required level of 30-85% (w/w) and further forwarded to continuous on line miscella refining plant. Here the temperature of the continuous extractor will be in the range of 32 to 64°C, where as the pre heating and distillation levels are varying from 35 to 140 °C with a crude miscella at a variable flow rate. Hence distilled and evaporated miscella was produced to a required level of concentration varying from 30 to 85 % and forwarded for further processing in miscella refining unit. B) On-line Cotton Crude - Miscella Refining process: The fat-insoluble impurities in the cotton crude miscella have to pre treated well prior to the refining. The impurities will cause deterioration of oil during storage of crude oil normally. These fat - insoluble impurities such as fragments of oilseeds and cells tissues should be removed from the crude miscella before they are treated by means of specially designed & strong filtration equipments. Otherwise, in the presence of even traces of moisture, the flat splitting enzymes and lipases usually present cause hydrolysis of the glycerides with the formation of steadily increasing amounts of free fatty acids. In the presence of moisture, seed fragments and coagulated mucilage will create the necessary conditions for the growth of microorganism. Some of these may also cause splitting of the glycerides and other type of rancidity, purification or development of objectionable odors and taste. It is therefore desirable that insoluble impurities should be removed immediately after extraction of crude oil and completion of primary heating and evaporation. Moreover, the presence of the insoluble impurities tends to increase losses in subsequent miscella refining treatment. In a nutshell the Cotton Crude Miscella (or low density Solvents like n-Hexane with Crude Cotton Oil admixed externally) from the extraction plant is stored and agitated in homogenizers to have a uniform mixing of product obtain requisite concentration. Further the homogenized crude miscella with a known concentration will be passed through a series of flow control devices, dynamic filters, heaters, on-line dynamic mixers to get added with phosphoric acid & other bleachable additives by dosing pump. The acid mixed mixture further passes through a series of static mixtures to get further added with caustic soda of different concentration as required and further discharges into reactors which are under vacuum. On completion of prescribed retention time where the reacted mixture dosed into the centrifuge separator duly pre heated or pre-cooled (on-line) to get separated the solids from the mixture on completing the neutralization. The caustic dosed mixture gets neutralized in presence of solvent n-Hexane and the free fatty acid in Miscella stage (i.e.. Crude cotton oil with Solvent n-Hexane of food grade), in order to coagulate the phosphatides and remove the bulk of the coloring matter. Primarily these mixtures are passed through series of equipments viz., primary heater to heat the miscella directly or indirectly from 30°C to 65°C, to a Reactor vessel under agitation with vacuum, on line static mixer and Dynamic mixer. Simultaneously the reacted matter is being washed online (based on the requirement) with a very light quantity of water to remove the traces of soap stock, and the discharged water will be added back to the recovered soap stock. The washed neutralized miscella is then stripped off hexane solvent to give neutral yellow color PBSY grade or bleachable grade of Cotton Neutral Oil. However, considerable difficulty is experienced in obtaining efficient contact between the caustic soda solution and the miscella. Because of such insufficient contact, full coagulation of the phosphatides and absorption of the coloring matter does not occur in the courses of ordinary mixing, as it does in ordinary alkali refining process of crude oil. In order to overcome this problem and to achieve effective results, the miscalla refining process adopts specially designed on line static mixers in series and in parallel. Hence produced soap stock contains wide range of hexane which wiil be stripped off through a thin film falling film evaporator (operates at a temperature of 40°C to 150°C ) with scraper & condenser to recover and receive the hexane in liquid form as an on-line process. Or else the soap stock could be forwarded and desolventized along with the cotton de oiled meal toasting operation at a process temperature ranging from 40 to 150°C . Further the neutral miscella produced will be forwarded to series of distillation process vessels to evaporate and separate the hexane in order to obtain the pure neutral oil of cotton oil. Advantages of the process: 1. Due to vast difference of density of crude oil vs crude miscella against their Corresponding soap stock, the entrainment of oil in the soap stock formed in solvent medium is practically eliminated. 2. During normal course of refining of crude oil observed direct saponification. The over saponification of the glyceride oil due to the presence of excess caustic soda is also considerably reduced in miscella refining. 3. The wide specific gravity difference between the formed soap stock and the oil-hexane solution (i.e., miscella) increases the efficiency of the centrifugal separation, and it is possible to operate the separators at higher than its rated capacity with effective contact. 5. The final bleached oil color is superior to that obtained by other refining methods and can be varied increasing the percentage and strength of refining caustic without serious oil losses by saponification. 6. Soap stock from the primary centrifuges contains about 5-20% of hexane and may be Freed of solvent by mixing with meal in the desolventizing equipments are used for meal or separated through the falling film evaporator cum scraper followed by condenser. This has the additional advantage of adding fat and thus calories with additional salty taste to the animal feed. 7. The fear or danger of color fixations of cotton crude oils on storage before neutralization /refining is totally eliminated with this process. Safety aspects to be considered for smooth operations: Solvent being used in the process which has an highly explosive in nature, the entire process equipments and its accessories has to comply with explosive proof (flame proof) norms. Involvement of inert gas blanketing can be done where ever it is necessary or else the requisite safety precautions can be taken. We Claim, 1} An improved process for online cotton crude miscella Refining, comprising the following steps a) Cotton crude being distilled to a required concentration level followed by for removing fat-insoluble impurities, such as moisture traces, flat splitting enzymes, lipases, coloring pigments etc., by filtration. b) The said crude miscella obtained at step (a) mixed with adequate quantity of phosphoric acid along with bleaching additives to coagulate the hydratable and non-hydratable phophotide gums / Color pigments, in miscella stage (crude cotton oil with solvent n-Hexane) further added with caustic soda solution to neutralize the free fatty acids to produce neutralized miscella (neutral oil with n- Hexane) and the separated solids are the by products and called as soap stock. c) The salty by product solid soap stocks obtained at step (b) are further received in a specially designed storage day tank further to process. In order to obtain a good quality of neutral oil free from soap stock traces the discharged neutral miscella will be further neutralized with citric acid online. During the process these mixtures are meant to pass through heater, reactor vessel under agitation, on line static mixer and Dynamic mixer, a high speed centrifugal separator / decanter where the solid impurities are separated and discharged out from the neutralized miscella followed by rinsing using very little volume of water on-line to remove the traces of salty soaps and recover the Cotton neutralized miscella at the discharge end of separator / decanter. d) The neutralized miscella obtained at step © is then stripped off hexane solvent to produce neutral yellow color cotton Oil by passing through a series of distillation process equipments., e) By product soap stock obtained at step (b) may contain certain quantity of hexane solvent which is being separated and collected through a falling film evaporator-cum-scraper attached with condenser or through the de- solventisation toasting method by adding to de oiled meal, by evaporation, condensed and reflux back to system, 2) The process as claimed in claim 1, wherein the inert gas nitrogen purged at different Milli bar level in order to avoid any explosion and on safety reasons, 3) The process as claimed in above claims wherein the Crude Miscella enters into the filtration, pre heating, reaction mixtures / vessels under agitation, acid / additive mixing mixers of dynamic and static mixer type, centrifugal separators by adding various in organic chemical reagents for treatment viz., phosphoric acid, bleaching additives, alkali caustic solution, neutralizing agent like citric acid intermixed at an adequate temperature for separation of impurities and to have reaction. 4) The process as claimed in claim I to 3 additive used is hydrogen peroxide, and the extracted crude cotton oil distillated heat exchanger cum evaporator which will adjust the crude miscella concentration to a required level of 30-85% (w/w) will forward to continuous on- line miscella refining plant, the temperature of the continuous extractor in the range of 32 to 64°C, where as the pre heating and distillation levels are varying from 35 to 140 °C with a crude miscella at a variable flow rate, to produce a required level of concentration varying from 30 to 85 % , 5) A process as claimed in claim 1, wherein the insoluble impurities shall be removed immediately after extraction of crude miscella and completion of primary heating and evaporation, and the temperature maintained in the range of 30°C to 65°C, of the Reactor vessel under agitation with vacuum, on line static mixer and Dynamic mixer, 6) A process as claimed in above claims wherein the produced soap stock contains wide range of hexane which will stripped - off through a thin type falling film evaporator operates at a temperature of 40°C to 150°C with scraper & condenser to recover and receive the hexane in liquid form as an on-line process, 7) A process as claimed in claim 6 wherein the soap stock forwarded and desolventized along with the cotton de oiled meal toasting operation at a temperature ranging from 40 to 150CC, followed by series of distillation process vessels to evaporate and separate the hexane in order to obtain the pure neutral oil of cotton oil. 8) An improved process for on-line cotton crude miscella Refining (neutralization) , such as here in described.

Documents:

2420-mum-2010-abstract.doc

2420-mum-2010-abstract.pdf

2420-MUM-2010-CLAIMS(AMENDED)-(18-3-2013).pdf

2420-mum-2010-claims.doc

2420-mum-2010-claims.pdf

2420-mum-2010-correspondence.pdf

2420-mum-2010-description(complete).pdf

2420-MUM-2010-FORM 1(18-3-2013).pdf

2420-mum-2010-form 1.pdf

2420-MUM-2010-FORM 18(14-01-2011).pdf

2420-MUM-2010-FORM 2(TITLE PAGE)-(18-3-2013).pdf

2420-mum-2010-form 2(title page).pdf

2420-mum-2010-form 2.doc

2420-mum-2010-form 2.pdf

2420-mum-2010-form 5.pdf

2420-MUM-2010-FORM 9(14-1-2011).pdf

2420-MUM-2010-REPLY TO EXAMINATION REPORT(18-3-2013).pdf

2420-MUM-2010-SPECIFICATION(AMENDED)-(18-3-2013).pdf

2420-MUM-2010-SPECIFICATION(MARKED COPY)-(18-3-2013).pdf