CN114804122A - Preparation method of ultra-pure silica sol and product thereof - Google Patents
Preparation method of ultra-pure silica sol and product thereof Download PDFInfo
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- CN114804122A CN114804122A CN202210528370.7A CN202210528370A CN114804122A CN 114804122 A CN114804122 A CN 114804122A CN 202210528370 A CN202210528370 A CN 202210528370A CN 114804122 A CN114804122 A CN 114804122A
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 193
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 178
- 239000003054 catalyst Substances 0.000 claims abstract description 51
- 239000000203 mixture Substances 0.000 claims abstract description 49
- 239000002245 particle Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012043 crude product Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000012535 impurity Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 150000001768 cations Chemical class 0.000 claims description 25
- 238000001914 filtration Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 22
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 150000001450 anions Chemical class 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 11
- 239000002893 slag Substances 0.000 claims description 11
- -1 vinylacetamine Chemical compound 0.000 claims description 10
- 150000007530 organic bases Chemical class 0.000 claims description 8
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 claims description 7
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 7
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 6
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 6
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 6
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 6
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 5
- SOYBEXQHNURCGE-UHFFFAOYSA-N 3-ethoxypropan-1-amine Chemical compound CCOCCCN SOYBEXQHNURCGE-UHFFFAOYSA-N 0.000 claims description 4
- DPBWFNDFMCCGGJ-UHFFFAOYSA-N 4-Piperidine carboxamide Chemical compound NC(=O)C1CCNCC1 DPBWFNDFMCCGGJ-UHFFFAOYSA-N 0.000 claims description 3
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 claims description 3
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims description 3
- 150000003927 aminopyridines Chemical class 0.000 claims description 3
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 3
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 3
- DNCPHSAQFYAGFK-UHFFFAOYSA-N C(=C)C(CCC)(N)N Chemical compound C(=C)C(CCC)(N)N DNCPHSAQFYAGFK-UHFFFAOYSA-N 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 14
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 6
- 229960001124 trientine Drugs 0.000 description 4
- QVYARBLCAHCSFJ-UHFFFAOYSA-N butane-1,1-diamine Chemical compound CCCC(N)N QVYARBLCAHCSFJ-UHFFFAOYSA-N 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- FJSHVOSRGPQYCV-UHFFFAOYSA-N CCCCN.C=CO Chemical compound CCCCN.C=CO FJSHVOSRGPQYCV-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QHCCDDQKNUYGNC-UHFFFAOYSA-N n-ethylbutan-1-amine Chemical compound CCCCNCC QHCCDDQKNUYGNC-UHFFFAOYSA-N 0.000 description 1
- RIWRFSMVIUAEBX-UHFFFAOYSA-N n-methyl-1-phenylmethanamine Chemical compound CNCC1=CC=CC=C1 RIWRFSMVIUAEBX-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/1412—Preparation of hydrosols or aqueous dispersions by oxidation of silicon in basic medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a preparation method of large-particle size silica sol and a product thereof, comprising the following steps: s100: weighing silicon powder, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, mixing water and the first part of silicon powder in proportion, stirring and heating to form a silicon powder mixture; s200: and respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst into a reaction container at a certain flow rate, and heating and pressurizing for reaction to obtain a silica sol crude product. The silicon powder is divided into two parts, the first part of silicon powder and water are mixed to prepare a mixture of the silicon powder and the water, the mixture of the silicon powder provides a good solution environment, and then the second part of silicon powder and a catalyst are added into the mixture of the silicon powder together, so that the particle size and the uniformity of the product are ensured; by controlling the pressure and temperature conditions, the conversion degree of the raw materials can reach the maximum (more than 95 percent conversion rate), and the consumption of a heat source can be controlled to the maximum degree; can produce the silica sol with the grain diameter of 10nm-300nm, the content of metal impurity ions is less than 1ppm, and the purity of the silica sol is high.
Description
Technical Field
The invention relates to the technical field of silica sol preparation processes, in particular to a preparation method of ultrapure silica sol and a product thereof.
Background
The silica sol is a dispersion of nano-sized silica particles in water or a solvent, and the basic component is amorphous silica having a molecular formula of mSiO 2 ·nH 2 O，SiO 2 The colloidal particles are uniformly dispersed in water or an organic solvent in the form of micelles, and the appearance of the colloidal particles is mostly milky white or light green transparent solution. The silica sol with the colloidal particle size larger than 20nm is called large-particle size silica sol industrially, the particle size of the common silica sol in the market is generally 1-100 nm, and the concentration is generally 20-50%.
The traditional preparation method of the silica sol mainly comprises the following steps: the simple substance silicon hydrolysis method, the ion exchange method and the sol-gel method are widely adopted in industry at present. The silica sol synthesized by the simple substance silicon hydrolysis method generally has the grain diameter of about 20-150nm and the concentration of 30-40 percent, but the product is difficult to meet the requirements of certain special industries on the grain diameter and the concentration of the silica sol. The particle size of the currently synthesized silica sol is 50-100nm, the concentration is 40% -50%, and the purity is less than 5000ppm, so that the requirements of various special industries on the particle size and the purity of the silica sol cannot be met, for example, the polishing of electronic materials such as silicon wafers, silicon carbide, gallium arsenide and the like needs the silica sol material with the particle size of more than 100nm and the purity of less than 1 ppm.
The particle size and purity of the silica sol product are used as one of the key indexes of the silica sol product, which not only influence the concentration, stability and color of the product, but also directly influence the performance of the product. How to prepare silica sol with large particle size and higher purity is a problem which needs to be solved urgently at present.
Disclosure of Invention
Based on the method, the invention provides a preparation method of the ultrapure silica sol, which can be used for producing the silica sol with large particle size and high purity and is simple to operate.
A preparation method of ultrapure silica sol comprises the following steps:
s100: weighing silicon powder, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, mixing water and the first part of silicon powder in proportion, stirring and heating to form a silicon powder mixture;
s200: and respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst into a reaction container at a certain flow rate, and heating and pressurizing for reaction to obtain a silica sol crude product.
According to the preparation method of the ultrapure silica sol, the silicon powder is divided into two parts, the two parts are added in two processes respectively, the first part of the silicon powder and the water are mixed to prepare a mixture of the silicon powder and the water, then the silicon powder mixture, the second part of the silicon powder and the catalyst are added in a stable flow mode, the silicon powder mixture provides a good solution environment, then the second part of the silicon powder and the catalyst are added into the silicon powder mixture together, and the catalyst participates in the whole process of infiltration and reaction of the second part of the silicon powder, so that the particle size and the uniformity of the product are ensured; by controlling the temperature condition, the conversion degree of the raw materials can reach the maximum (more than 95 percent conversion rate), and the consumption of a heat source can be controlled to the maximum degree; can produce silica sol with the grain diameter of 10nm-300nm, has small content of metal impurity ions and high purity of the silica sol, and simplifies the production procedure; the raw materials added in the process are few in variety, the uncertain factors of the reaction and the possibility of introducing other impurities are reduced, the purity and the quality of the silica sol are improved, and the particle size controllability of the silica sol is excellent.
In one embodiment, the step S200 is followed by the step S300:
and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to ensure that the concentration of other cations except the catalyst cations is less than 1ppm, so as to obtain the high-stability and ultra-pure silica sol.
In one embodiment, in the step S100, the first part of silicon powder accounts for 1/10-1/3 of the total silicon powder by mass.
In one embodiment, in the step S100, the mass ratio of the first part of silicon powder to water is 1-2: 8-30.
In one embodiment, in step S100, heating is carried out to a temperature of 60 ℃ to 100 ℃; and/or, in the step S200, heating to the temperature of 100-150 ℃.
In one embodiment, the silicon content of the silicon powder is greater than 90% by mass.
In one embodiment, the catalyst added each time accounts for less than or equal to 5% of the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst.
In one embodiment, the catalyst is one or a combination of organic bases.
In one embodiment, the organic base comprises at least one of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, 2-amino-2-methyl-1-propanol, 3-aminopropanol, vinylalcohol-butylamine, vinylalcohol-butanediamine, vinylalcohol-butanetriamine, vinylalcohol-butanetetramine, azobenzylamine, aminopyridine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, 3-ethoxypropylamine, bis (2-aminoethyl) amine, pyrimidine, piperidine, 4-piperidinecarboxamide.
-a high stability, ultra-pure silica sol prepared by the method of preparing a large particle size silica sol according to any of the above, and a product prepared from the high stability, ultra-pure silica sol.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a preparation method of high-stability and ultra-pure silica sol, which comprises the following steps:
s100: weighing silicon powder, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, mixing water and the first part of silicon powder in proportion, stirring and heating to form a silicon powder mixture.
In one embodiment, the first portion of silicon powder is 1/10-1/3 of the total silicon powder mass. The first part of silicon powder is mixed with water to form a mixture, which mainly provides a solution environment for the next step, and the silicon powder mixture has a promotion effect on the positive and negative of the subsequent silicon powder and water, so that the conversion rate is improved.
In one embodiment, in the step S100, the mass ratio of the first part of silicon powder to water is 1-2: 8-30.
Optionally, the silicon content of the silicon powder is greater than 90% by mass to reduce the influence of impurities, and preferably, the silicon content of the silicon powder is greater than 95% by mass.
In one embodiment, the heating in step S100 is performed to a temperature of 60 ℃ to 100 ℃, which facilitates uniform dispersion of the silicon powder without agglomeration, and the silicon powder is uniformly dispersed in water.
S200: and respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst into a reaction container at a certain flow rate, and heating and pressurizing for reaction to obtain a silica sol crude product.
In one embodiment, the content of the catalyst added each time in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst is less than or equal to 5%, and when the adding amount of the catalyst is more than 5 wt%, the catalyst can locally and rapidly react to form clusters and be dispersed unevenly, which is not favorable for controlling the particle size of the silica sol. According to the method, the adding amount proportion of the silicon powder mixture, the second part of silicon powder and the catalyst can be calculated respectively, and the particle size range can be controlled.
In one embodiment, the catalyst is one or a combination of organic bases. The organic base is a nitrogen-containing organic base, for example, the organic base may include at least one of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, 2-amino-2-methyl-1-propanol, 3-aminopropanol, vinylacetamine, butylethylamine, vinylbutanetriamine, butylethyltetramine, benzylmethylamine, aminopyridine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, 3-ethoxypropylamine, bis (2-aminoethyl) amine, pyrimidine, piperidine, 4-piperidinecarboxamide.
In one embodiment, the heating in step S200 is heating to a temperature of 100 ℃ to 150 ℃.
In step S200, a suitable reaction time can be selected according to the actual situation, and generally, the reaction time is selected to be 8 to 12 hours.
In one embodiment, the step S200 is followed by a step S300, and the step S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable other cations except the catalyst cations to be less than 1ppm, so as to obtain the ultrapure silica sol.
The preparation method of the ultrapure silica sol comprises the steps of dividing the silicon powder into two parts, adding the two parts in two processes respectively, mixing the first part of the silicon powder with water to prepare a mixture of the silicon powder and the water, adding the mixture of the silicon powder, the second part of the silicon powder and the catalyst in a stable flow manner, wherein the mixture of the silicon powder provides a good solution environment, adding the second part of the silicon powder and the catalyst into the mixture of the silicon powder together, and enabling the catalyst to participate in the whole process from infiltration to reaction of the second part of the silicon powder, so that the particle size and the uniformity of the product are ensured.
By controlling the pressure and temperature conditions, the conversion degree of the raw materials can reach the maximum (more than 95 percent conversion rate), and the consumption of a heat source can be controlled to the maximum degree; the large-particle size silica sol prepared by the preparation method of the large-particle size silica sol has the particle size of 5nm-300nm, low content of metal impurity ions and high purity, and simplifies the production procedure; the raw materials added in the preparation process are few in variety, the uncertain factors of the reaction and the possibility of introducing other impurities are reduced, the purity and the quality of the silica sol are improved, and the particle size controllability of the silica sol is excellent. The large-particle-size silica sol prepared by the preparation method of the ultrapure silica sol can be used for preparing corresponding silica sol products in various fields.
The following is an example description.
Example 1
The preparation method of the large-particle size silica sol of the embodiment comprises the following steps:
s100: weighing silicon powder with the silicon content of 96%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 1/5 of the total silicon powder, and mixing the first part of silicon powder and water according to the mass ratio of 1: 20, stirring and heating to 60 ℃ to form a silicon powder mixture.
S200: and respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst into a reaction container at a certain flow rate, wherein the content of the catalyst added in each time in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst is less than or equal to 5%, and reacting at the temperature of 100 ℃ to obtain a silica sol crude product.
The catalyst is prepared from the following components in a mass ratio of 1: 3 and triethylenetetramine.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable the cation to be less than 1ppm, thereby obtaining the ultrapure silica sol.
Example 2
The preparation method of the large-particle size silica sol of the embodiment comprises the following steps:
s100: weighing silicon powder with the silicon content of more than 95%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 1/4 of the total silicon powder, and mixing the first part of silicon powder and water according to the mass ratio of 2: 25, stirring and heating to 60 ℃ to form a silicon powder mixture;
s200: respectively adding the silicon powder mixture, the second part of silicon powder and a catalyst triethylene tetramine into a reaction vessel at a certain flow rate, wherein the content of the catalyst added each time in the total mass of the silicon powder mixture, the second part of silicon powder and the organic base is less than or equal to 5%, and reacting at the temperature of 110 ℃ to obtain a silica sol crude product.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable other cations except sodium ions to be less than 1ppm, thereby obtaining the ultrapure silica sol.
Example 3
The preparation method of the large-particle size silica sol of the embodiment comprises the following steps:
s100: weighing silicon powder with the silicon content of more than 95%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 2/7 of the total mass of the silicon powder, and mixing the first part of silicon powder and water according to the mass ratio of 1.5: 12, stirring and heating to 80 ℃ to form a silicon powder mixture.
S200: respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst 2-amino-2-methyl-1-propanol into a reaction container at a certain flow rate, wherein the content of the catalyst 2-amino-2-methyl-1-propanol added each time in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst 2-amino-2-methyl-1-propanol is less than or equal to 5%, and reacting at the temperature of 120 ℃ and the reaction pressure of less than 0.1mpa to obtain a silica sol crude product.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable the cation to be less than 1ppm, thereby obtaining the ultrapure silica sol.
Example 4
The preparation method of the large-particle size silica sol of the embodiment comprises the following steps:
s100: weighing silicon powder with the silicon content of more than 95%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 2/10 of the total silicon powder, and mixing the first part of silicon powder and water according to the mass ratio of 1: 30, stirring and heating to 100 ℃ to form a silicon powder mixture;
s200: and respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst into a reaction container at a certain flow rate, wherein the content of the catalyst in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst is less than or equal to 5 percent each time, and reacting at the temperature of 100 ℃ and the reaction pressure of less than 0.1mpa to obtain a silica sol crude product.
The catalyst is prepared from the following components in percentage by mass: 1 of 2-amino-2-methyl-1-propanol and 3-ethoxypropylamine.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable other cations except sodium ions and potassium ions to be less than 50ppm, so as to obtain the ultrapure silica sol.
Example 5
The preparation method of the ultrapure silica sol comprises the following steps:
s100: weighing silicon powder with the silicon content of more than 95%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 1/10 of the total silicon powder, and mixing the first part of silicon powder and water according to the mass ratio of 2: 27 are mixed, stirred, and heated to a temperature of 70 c to form a silicon powder mixture.
S200: and respectively adding the silicon powder mixture, the second part of silicon powder and a catalyst of vinyl alcohol butyl tetramine into a reaction vessel at a certain flow rate, wherein the content of the catalyst of vinyl alcohol butyl tetramine in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst of vinyl alcohol butyl tetramine added each time is less than or equal to 5%, and reacting at the temperature of 130 ℃ to obtain a silica sol crude product.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable the cation content to be less than 1ppm, so as to obtain the silica sol with large particle size.
Example 6
The preparation method of the ultrapure silica sol of the present embodiment comprises the following steps:
s100: weighing silicon powder with the silicon content of more than 95%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 1/4 of the total silicon powder, and mixing the first part of silicon powder and water according to the mass ratio of 1: 8, stirring and heating to 90 ℃ to form a silicon powder mixture.
S200: respectively adding the silicon powder mixture, the second part of silicon powder and a catalyst of vinyl alcohol butanediamine into a reaction container at a certain flow rate, wherein the content of the catalyst of vinyl alcohol butanediamine in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst of vinyl alcohol butanediamine is less than or equal to 1% each time, and reacting at the temperature of 150 ℃ to obtain a silica sol crude product.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable the cation to be less than 1ppm, thereby obtaining the ultrapure silica sol.
Example 7
The preparation method of the large-particle size silica sol of the embodiment comprises the following steps:
s100: weighing silicon powder with the silicon content of more than 95%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 1/3 of the total silicon powder, and mixing the first part of silicon powder and water according to the mass ratio of 1: 15, stirring and heating to 100 ℃ to form the silicon powder mixture.
S200: and respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst tetraethylammonium hydroxide into a reaction container at a certain flow rate, wherein the content of the catalyst tetraethylammonium hydroxide added each time in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst tetraethylammonium hydroxide is less than or equal to 5%, and reacting at the temperature of 100 ℃ to obtain a silica sol crude product.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable the cation to be less than 1ppm, thereby obtaining the ultrapure silica sol.
Example 8
The preparation method of the large-particle size silica sol of the embodiment comprises the following steps:
s100: weighing silicon powder with the silicon content of more than 95%, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, wherein the first part of silicon powder accounts for 3/10 of the total silicon powder, and mixing water and the first part of silicon powder according to the mass ratio of 1.5: 30, stirring and heating to 100 ℃ to form the silicon powder mixture.
S200: respectively adding the silicon powder mixture, the second part of silicon powder and a catalyst of vinyl alcohol butyl triamine into a reaction container at a certain flow rate, wherein the content of the catalyst of vinyl alcohol butyl triamine added each time in the total mass of the silicon powder mixture, the second part of silicon powder and the catalyst of vinyl alcohol butyl triamine is less than or equal to 5%, and reacting at the temperature of 105 ℃ and under the reaction pressure of less than 0.1mpa to obtain a crude silica sol product.
S300: and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to enable the cation to be less than 1ppm, thereby obtaining the ultrapure silica sol.
The silica sols prepared in examples 1 to 8 were subjected to a performance test, the test results of which are shown in table 1:
the technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of ultrapure silica sol is characterized by comprising the following steps:
s100: weighing silicon powder, dividing the silicon powder into a first part of silicon powder and a second part of silicon powder, mixing water and the first part of silicon powder in proportion, stirring and heating to form a silicon powder mixture;
s200: and respectively adding the silicon powder mixture, the second part of silicon powder and the catalyst into a reaction container at a certain flow rate, and heating and pressurizing for reaction to obtain a silica sol crude product.
2. The method for preparing ultrapure silica sol according to claim 1, wherein said step S200 is followed by a step S300 of:
and (3) centrifugally filtering the silica sol crude product to remove silica slag, and then filtering by adopting a membrane to remove anion and cation impurities to ensure that the concentration of other cations except the catalyst cations is less than 1ppm, thereby obtaining the ultrapure silica sol.
3. The method of claim 1, wherein in the step S100, the first portion of silicon powder accounts for 1/10-1/3 of the total silicon powder mass.
4. The method according to any one of claims 1 to 3, wherein in the step S100, the mass ratio of the first portion of silicon powder to water is 1-2: 8-30.
5. The method for preparing ultrapure silica sol according to any one of claims 1 to 3, wherein in step S100 the heating is carried out to a temperature of 60 ℃ to 100 ℃; and/or the presence of a gas in the gas,
in the step S200, the temperature is heated to 100-150 ℃.
6. The method according to any one of claims 1 to 3, wherein the mass content of silicon in the silicon powder is greater than 90%.
7. The method of any one of claims 1 to 3, wherein the catalyst is added at each time in an amount of 5% or less based on the total mass of the silicon powder mixture, the second silicon powder, and the catalyst.
8. The method for preparing a large-particle-size silica sol according to any one of claims 1 to 3, wherein the catalyst is one or a combination of several kinds of organic bases.
9. The method of claim 8, wherein the organic base comprises at least one of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, 2-amino-2-methyl-1-propanol, 3-aminopropanol, vinylacetamine, vinylbutanediamine, vinylbutanetriamine, vinylbutanetetramine, azobenzylamine, aminopyridine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, 3-ethoxypropylamine, bis (2-aminoethyl) amine, pyrimidine, piperidine, 4-piperidinecarboxamide.
10. A silica sol of particle homogeneity produced by the method of any one of claims 1 to 9, and an article produced using the ultrapure silica sol.
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