Title of Invention

A METHOD FOR PREPARING NANO PARTICLES

Abstract

The present invention discloses a method of preparing Nano particles. The method includes steps for preparing a solution of organometallic compound in an organic solvent. Thereafter, the organometicallic compound is hydrolyzed, neutralized and precipitated using a hydrolyzing agent to form an organometallic hydroxide complex. Thereafter, the organometaillic hydrooxide complex is rigorously birred at a low temperature to form slurry of Nano crystalline particles. Finally, the slurry of Nano crystalline particles is dried to form powder of Nano particles.

Full Text

FORM 2 THE PATENTS ACT 1970 (39 OF 1970) & The Patents Rules, 2003 COMPLETE SPECIFICATION (See section 10 and rule 13) Title of the invention A method for preparing Nano particles APPLICANT Avinash Ramchandra Moghe A-1003, 10 Kasturkunj, ICS Colony, University Road, Pune- 411 007. (Maharashtra) The following spedfication particularly describes the invention and the manner in which it is to be performed Inventor: Avinash R Moghe Complete Specification FIELD OF TIIU INVENTION [0001] The present invention generally relates to Nano crystalline particles, and more particularly, to a method for producing Nano crystalline particles of metal oxide, such as anatase Titanium di oxide. BACKGROUND OF THE INVENTION [0002] Generally, nano crystalline particles, such as Titanium di oxide powder, have been conventionally prepared by a sol-gel method and by chloride process. The sol-gel method requires additional heat treatments, which makes the sol-gel method difficult to perform continuously and thereby incurs a high production cost. The chloride process used for producing Titanium di oxide requires a particular apparatus due to its high temperature and pressure reactions. Further, the chloride process requires an additional protective facility from corrosive gases (CF, FIG) produced during the process, which leads to higher production cost. Moreover, special devices are employed for applying electric fields or controlling the reactanl mixing ratio to control the shape and size of Ti02 particles. [0003] Further, patent application WO2008079311 describes a process for making suspensions of finely divided amorphous Titanium oxide particles and converting the particles to anatase Titanium di oxide. Further, the anatase Titanium di oxide is substantially amorphous. Moreover, the amorphous material may be heated to the boiling point to convert amorphous material to crystalline material, such as anatase Titanium di oxide. Inventor: Avinash R Moghe Complete Specification [0004] Accordingly, there is a need to provide a method for preparing Nano crystalline particles which is simpler. Further, there is a need to provide a method for preparing Nano particles, without forming any suspension. [0005] Furthermore, there is a need to provide a method for preparing Nano crystalline particles, by vigorous stirring. Moreover, there is a need for a method to prepare Nano crystalline particles, which is cheaper. OBJECTS OF THE INVENTION [0006] Accordingly, the object of the present invention is to provide a method for preparing Nano crystalline particles, which is simpler. [0007] Another object of the present invention is to provide a method for preparing Nano crystalline particles, which is capable of producing Nano crystalline particles without forming any suspension. [0008) Yet another object of the present invention is to provide a method for preparing Nano particles, which is capable of producing Nano crystalline particles by vigorous stirring. [0009J Further object of the present invention is to provide a method for preparing Nano crystalline particles, which is cheaper. SUMMARY OF THE INVENTION [0010] Accordingly, the present invention provides a method for preparing Nano crystalline particles. The method comprising the steps of: preparing a solution of organometallic compound in an organic solvent; hydrolyzing, neutralizing and precipitating said solution to form an organometallic hydroxide complex using hydrolyzing agent; Inventor: Avinash R Moghe Complete Specification rigorous stirring of the said organometallic hydroxide complex at a low temperature to form slurry; the slurry of Nano crystalline particles is dried to form a powder of Nano crystalline particles. [0011] Typically, wherein the Nano crystalline particles are Titanium di oxide. [0012] Typically, wherein the rigorous stirring of said organometallic hydroxide complex - happens in between 50-95°C. [0013] Typically, wherein the hydrolyzing agent is distilled water or alkaline distilled water or acidic distilled water or hydrogen peroxide or any combination thereof. [0014] Typically, wherein the hydrolysis is delayed using acids. [0015] Typically, wherein the acid is from the mineral acids group. [0016] Typically, wherein said mineral acids group comprises of Hydrochloric Acid (HC1). Nitric Acid (HN03). [0017] Typically, wherein the organic solvents are from the alcohol group. [0018] Typically, wherein the said alcohol group comprises of methanol, ethanol, isopropanol, butanol. [0019] Typically, wherein the organometallic compound is a Titanium Alkoxide. Inventor: Avinash R Moghe Complete Specification [0020] Typically, wherein said Titanium Aikoxide compounds comprise - any of Titanium (IV) isopropoxide, Titanium (TV) n-butoxide, Titanium(IV) methoxide, Titanium (IV) elhoxide, Titanium (IV) n-propoxide or any other organometallic compound of Titanium di oxide. [0021] Typically, wherein one form of the nano particles, is nano crystalline Titanium di oxide and wherein stirring is done at temperatures in between 50-95°C. [0022] In another aspect of the invention, a method for preparing nano particles, accordingly the present invention is suitable for use in the application of various processes. BRIEF DESCRIPTION OF THE DRAWING [0023] FIG 1. is a graph showing an X-ray diffraction pattern [XRD] of powder derived from the hydrolyzed gel of Ti02, which was NOT SUBJECT to HOT Stirring below 100°C. This shows an amorphous powder of Ti02, as illustrated in practical example 1. [0024] FIG 2 is a graph showing an X-ray diffraction pattern [XRD] of powder derived from the hydrolyzed gel of Ti02, which was SUBJECT to HOT Stirring below 100 C. This shows Nano crystalline particles of anatase phase Ti02 as illustrated in practical example 2. [0025] FIG. 3 shows TEM (microscopic view") of Nano crystalline particles anatase phase of Titanium di oxide [Ti02] this gives us an idea of particle size & particle distribution & surface Area of Nano particle of metal oxide. Inventor: Avinash R Moghe Complete Specification DETAILED DESCRIPTION OF THE INVENTION [0026] For a thorough understanding of the present invention, reference is to be made to (he following detailed description, including the appended claims, in connection with the above-described drawings. It is understood that various omissions and substitutions of equivalents are contemplated as circumstances may suggest or render expedient, but these are intended to cover the application or implementation without departing from the spirit or scope of the claims of the present invention. Also, it is to be understood that the phraseology and terminology used herein is for the purpose of description and should not be regarded as limiting. [0027] The terms, such as "first", second", "a", "an" herein do not denote a limitation of quantity, but rather denote the presence of at least one of the referenced item. [0028] The present invention provides a method for preparing Nano crystalline particles. The method includes the steps of preparing a solution of organometallic compound in an organic solvent. Thereafter, the solution is hydrolyzed, neutralized and precipitated to form an organometallic hydroxide complex by using hydrolyzing agent. Thereafter, the organometallic hydroxide complex is rigorously stirred at a low temperature to form slurry of Nano crystalline particles. Thereafter, the slurry of Nano crystalline particles is dried. [0029] As mentioned above, the solution is prepared by mixing organometallic compounds in the organic solvent. Generally, the organic solvent has a low boiling point, thereby evaporating easily. In an embodiment, the solution formed is a transparent sol-gel solution having uniformity at molecular level. Further, the sol-gel may be prepared by mixing 40 ml of Isopropyl Alcohol in a beaker containing 40 ml of Methanol at about temperature of 10-30°C (degree centigrade) and stirring on a magnetic Inventor: Avinash R Moghe Complete Specification stirrer. Further, the concentration of metal ions in the sol-gel solution may be adjusted to 1 -10% by weight, preferably 2- 5 % by weight. [0030] Further, in an embodiment, the organometallic compound may be any other compound, such as organo-inorganics, metallo-organics, and the like. In another embodiment, the organometallic compound may be a Titanium Alkoxide. The Titanium Alkoxide compounds may be selected from the group consisting of Titanium (IV) isopropoxide. Titanium (IV) n-butoxide, Titanium (IV) methoxide, Titanium (IV) ethoxide, Titanium (IV) n-propoxide and other organometallic compounds of Titanium di oxide. [0031 ] Thereafter, this solution is hydrolyzed. neutralized and precipitated to form organometallic hydroxide complex. In an embodiment, the solution is hydrolyzed by adding a controlled amount of water, preferably deionised and optionally acidified water, to the solution. Simultaneously, the solution is neutralized and precipitated by a suitable hydrolyzing agent such as Distilled Water, and/or Alkaline distilled water, or Acidic distilled water. In one embodiment, if desired the hydrolysis can be delayed by using acids such as HCI. HNO3 and the like. The solution is used as raw material for producing Nano particles of metal oxide. The hydrolyzed. neutralized and precipitated slurry is rinsed extensively with distilled water and rigorously stirred. In an embodiment the slurry is stirred at about a temperature ranging between 50°C-95°C to get slurry of Nano crystalline particles. In an embodiment, the Nano crystalline particles may be a metal oxide, such as Titanium di oxide [T1O2]. [0032] Further, the organometallic hydroxide complex may be rigorously stirred. In an embodiment, the organometallic hydroxide complex is stirred about a temperature below 100°C ranging in between 50 to 95C. The stirring process may be carried out by any conventional process of stirring known to a person skilled in the similar art. Inventor: Avinash R Moghe Complete Specification [0033] further, the slurry of Nano crystalline particles is dried. Further, the slurry of the Nano particles may be dried by any method known to a person skilled in the pertained art. [0034] After drying the slurry, a powder of Nano crystalline particles is obtained having a uniform stoichiometric control over the composition of Nano crystalline particles. Further, due to the uniformity of molecules of the solution, each of the smallest elements of the obtained powder of Nano crystal has spherical shape. [0035] The method for preparing the Nano particles of metal oxide according to the present invention may be widely and effectively applied for producing a multi-element nanocrystalline metal oxide, and in addition, the method could be applicable to a technology for forming a single element nanocrystalline metal oxide powder and the like. [0036] The invention is now described in further details with reference to some practical examples of its embodiment. The examples are provided only for better understating of the present invention. Further, it is understood that the present invention is not limited to the following practical examples, but various modifications may be made without departing from the spirit of the aforementioned and the following description and such modifications are within the scope of the invention. PRACTICAL EXAMPLE 1 [0037] To 40 ml Isopropyl alcohol in a beaker 40 ml of Methanol was added at a temperature of 10-30 degree centigrade and stirring was continued for 10 minutes on a magnetic stirrer. This was added to 10 ml of Butyl Titanate / Titanium Butoxide [Organo-metallic compound of Titanium-di-oxide having 23.6 % Ti02] and with stirring s for 10 minutes, at a temperature of 10-30°C to get a clear solution. [0038] To this clear solution 25ml of distilled water was added and stirring was continued for 10 minutes. The clear sol-gel solution is hydrolised and turned into a very uniform slurry of organometallic hydroxide complex of Ti02. [0039] This milky white hydrolyzed organometallic hydroxide complex is dried in to form a very uniform soft, cake of powder of the metal oxide [Ti02]. [0040] The obtained cake of the said oxide was crushed into fine powder. Then X-ray diffraction pattern [XRD] was taken, as shown in Fig.l. PRACTICAL EXAMPLE 2 [0041] To 40 ml Isopropyl alcohol in a beaker 40 ml of Methanol was added at a temperature of 10-30°C and stirring was continued for 10 minutes on a magnetic stirrer. This was added to 10 ml of Butyl Titanate / Titanium Butoxide [Organometallic compound of Titanium di oxide having 23.6 % Ti02] and with stirring for 10 minutes, at about a temperature of 10-30°C to get a clear solution. [0042] To this clear solution 25ml.of distilled water was added and stirring was continued for 10 minutes. The clear sol-gel solution is hydrolyzed and turned into a very uniform, slurry of organometallic hydroxide complex of Ti02. [0043] This milky white hydrolyzed organometallic hydroxide complex is then rigorously stirred in a hot water bath at a temperature 50-95°C, to get a slury of Nano crystalline particles/ [0044] The Nano crystalline particles thus obtained are dried to form a very uniform soft cake of nanocrystalline powder of the said metal oxide [Ti02] [0045] The obtained cake of Nano crystalline particles of the said oxide was crushed into fine powder. Then X-ray diffraction pattern [XRD] was taken, as shown in Fig.2 EVALUATION TEST 1 [0046] FIG.l is a graph showing an X-ray diffraction pattern [XRD] of powder derived from the hydrolyzed gel of Ti02, which was not subject to hot stirring below 100°C. This shows an amorphous powder of Ti02, as illustrated in practical example 1. EVALUATION TEST 2 [0047] FIG. 2 is a graph showing an X-ray diffraction pattern [XRD] of powder derived from the hydrolyzed gel of Ti02, which was SUBJECT to HOT Stirring below 100 C. This shows crystalline nanoparticles as in practical example 2. The X-ray diffraction pattern [XRD] in Fig. 2 shows that Nanocrystalline powder of Ti02- has anatase- phase. [0048] FIG. 3 is TEM photograph of Nanocrystalline, anatase Ti02 of practical example 2 having particle size of 5-20 nano-meters and with a specific surface area of 100-200 m.sup.2 g. having a uniform, crystalline, nano-particles, spherical in shape which is very suitable for forming UV/ Visible light photo-catalyst and for various other applications. ADVANTAGES [0049] The present invention is constituted as mentioned above. By applying the present method, a precise stoichiometric control of the nanocrystalline metal oxide can be easily made in any component system. In addition, conversion of amorphous phase to nano - crystalline phase can be achieved efficiently and speedily at a Inventor: AvinashRMoghe Complete Specillcation remarkably lower temperature [50-95]. Hence with lower energy and cost, than required by conventional ceramic processing techniques reported so far, one can commercially produce Nanocrysialline metal oxide powder on a very large scale, with this innovative new technique. [0050] The nanocrysialline powder of metal oxide produced using such a technique mentioned above has particle size of 5-20 nm size and with a specific surface area of 100-200 m.sup.2 /g. Ti02 anatase phase is developed at temperatures below 100°C. This innovative technique has been developed, which gives uniform nano-particles of metaloxide material with several superior characterstics, than similar materials prepared by the conventional ceramic process reported so far. The shape & size of nanocrystalline particle can be controlled as desired, by controlling the process parameters. [0051 ] It will be appreciated that various modifications can be made in the preferred embodiments without departing from the principles of the invention. These and other modifications in the nature of the invention or the preferred embodiments will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation. Inventor: Avinash Ramchandra Moghe Complete Specification 1/ WE CLAIM: 1. A method for preparing Nano particles, the method comprising the steps of: preparing a solution of orgahometallic compound in an organic solvent; 5 hydrolyzing, neutralizing and precipitating said solution to form an organometallic hydroxide complex using hydrolyzing agent; rigorous stirring of the said organometallic hydroxide complex at a low temperature to form a slurry of Nano particles; and the slurry of Nano particles is dried to form a powder of Nano particles. 2. The method as in claim 1, wherein the Nano particles are a (metal) oxide material. 3. The method as in claim 1, wherein the organometallic hydroxide complex is rigorously stirred at about a temperature ranging between 50-95°C. 15 4. The method as in claim 1, wherein the hydrolyzing agent is an agent, such as distilled water, alkaline distilled water, acidic distilled water, hydrogen peroxide or any combination thereof and the like. .20 5. The method as in claim 1, wherein the hydrolysis is delayed by using acid. 6. The method as in claim 5, wherein the acid is selected from a group of mineral acids containing Hydrochloric Acid (HC1), and Nitric Acid (HN03). 25 7. The method as in claim 1, wherein the organic solvents are from the alcohol group. 8. The method as ia claim 7, wherein the alcohol is selected from the group comprising of methanol, ethanol, isopropanol and butanol. 30 Inventor: Avinash Ramchandra Moghe Complete Specification 9. The method as in claim 1, wherein the organometallic compound is a Titanium Alkoxide. 10. The method as in claim 9 , wherein the Titanium Alkoxide compounds is selected from the group comprising of Titanium(IV) isopropoxide, Titanium(IV) n-butoxide, Titanium(IV) methoxide, Titanium(lV) ethoxide, Titanium(IV) n-propoxide and other organometallic compound of Titanium di oxide. 11. The method as in claim 1, wherein one form of the nano particles is nano crystalline Titanium di oxide and wherein stirring is done at temperatures in between 50- 95°C. Name : Avinash Ramchandra Moghe Date: Day of 2008

Documents:

2478-mum-2008-abstract.doc

2478-mum-2008-abstract.pdf

2478-MUM-2008-CLAIMS(AMENDED)-(22-12-2011).pdf

2478-MUM-2008-CLAIMS(AMENDED)-(9-11-2012).pdf

2478-mum-2008-claims.doc

2478-mum-2008-claims.pdf

2478-MUM-2008-CORRESPONDENCE(14-5-2012).pdf

2478-MUM-2008-CORRESPONDENCE(2-6-2009).pdf

2478-MUM-2008-CORRESPONDENCE(9-11-2012).pdf

2478-mum-2008-description (complete).doc

2478-mum-2008-description (complete).pdf

2478-mum-2008-drawing.pdf

2478-mum-2008-form 1.pdf

2478-MUM-2008-FORM 13(14-5-2012).pdf

2478-MUM-2008-FORM 13(22-12-2011).pdf

2478-MUM-2008-FORM 13(9-11-2012).pdf

2478-mum-2008-form 18(2-6-2009).pdf

2478-mum-2008-form 2(titel page).pdf

2478-mum-2008-form 2.doc

2478-mum-2008-form 2.pdf

2478-MUM-2008-FORM 26 (22-12-2011).pdf

2478-MUM-2008-FORM 26(14-5-2012).pdf

2478-MUM-2008-FORM 26(2-6-2009).pdf

2478-MUM-2008-FORM 26(22-12-2011).pdf

2478-mum-2008-form 3.pdf

2478-mum-2008-form 5.pdf

2478-MUM-2008-MARKED COPY(14-5-2012).pdf

2478-MUM-2008-REPLY TO EXAMINATION REPORT(22-12-2011).pdf

2478-MUM-2008-SPECIFICATION(AMENDED)-(22-12-2011).pdf

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