CN112499634B - Preparation method of silica sol - Google Patents
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Abstract
The invention discloses a preparation method of silica sol, belonging to the technical field of inorganic nano materials. The invention prepares the silica sol, two reagents are screened to modify the silica sol in the preparation process, alpha-sodium alkenyl sulfonate is added, the addition of a sulfonic group side chain can effectively prevent the shrinkage agglomeration between silicon hydroxyl groups, the addition of the grafted cyclodextrin can improve the interface adsorption force on the surface of the silica dioxide and can promote the uniform dispersion of the alpha-sodium alkenyl sulfonate on the surface of particles, the two reagents have synergistic interaction, the particle size of the obtained silica sol particles is between 100 and 400 nanometers, the concentration is about 50 percent, the particle size distribution is uniform, and the stability is good. The preparation method of the silica sol has simple process and low cost, and is suitable for large-scale popularization and application.
Description
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly relates to a preparation method of silica sol.
Background
Silica sol is a nano material with excellent performance, is a colloidal solution formed by uniformly dispersing amorphous silica particles in water or an organic solvent, and is an inorganic high polymer material with extremely wide application. Silica sol is a network structure formed by countless micelles, so that the silica sol has large specific surface area, high adsorbability, special high dispersity, high fire resistance, high heat insulation and other excellent performances, and is widely applied to the precision casting industry, the textile industry, the catalytic industry, the paper making industry and the coating industry.
Silica sols having a particle size of greater than 20nm and a concentration of greater than 40% are generally referred to as large particle size high concentration silica sols. The method is applied to industries with higher requirements on catalyst carriers and high refractoriness, the concentration of the needed silica sol reaches about 40%, large-particle-size high-concentration silica sol is researched in the foreign 20 th century and 50 th century, and the process for synthesizing the large-particle-size high-concentration silica sol is mature at the end of the last century. At present, silica sol products with large particle size and high concentration, which are produced by some overseas and overseas companies in large scale, have the particle size of about 50nm and the concentration of about 35-60 percent, and also enter domestic markets in large quantities in recent years. In order to meet the requirements of domestic markets, large-particle-size silica sol is also researched in succession in China. The method combines a direct acidification method and a simple substance silicon one-step dissolution method to prepare the silica sol with required particle size. The proposed mother nucleus size influences the uniformity of sol particles, and the mother nucleus smaller than 60nm has better reaction activity and can effectively adsorb silicic acid for growth. The preparation method is to drop the prepared active silicic acid into the boiling water glass raw material to prepare the mother nucleus. And then, the mother core silicon dioxide particles are further increased by adopting a method of hydrolyzing silicon powder, so that the particle size of the silicon dioxide is increased to 50-100 nm, and the content is increased to 50%. Many researchers adopt a new means to achieve the purpose of generating sol particles with large particle size and high uniformity according to the characteristics and the reaction mechanism of the silica sol while changing the reaction conditions.
However, the existing method for preparing the silica sol has complex process and high cost, the prepared large-particle silica sol still cannot meet the actual industrial requirements, the particle size uniformity is poor, the stability is poor, the long-time storage is difficult, and great difficulty is brought to the actual application.
Disclosure of Invention
The invention provides a novel preparation method of silica sol according to the problems in the prior art, and the obtained silica sol has large particles, uniform particle size distribution, long-term storage, simple process and low cost. In order to achieve the technical purpose, the technical means adopted by the invention is as follows:
a preparation method of silica sol comprises the following steps:
1) pouring 99.999% silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a flask in sequence, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing ethyl orthosilicate and absolute ethyl alcohol to obtain solution B, dripping the solution B into the solution A, dripping ammonia water or organic amine with the mass percentage of 0.05-0.3% of the mixed solution AB, and reacting for 4 hours at 50 ℃; and (3) adding a modifier into the mixed solution obtained in the step (2), continuing to magnetically stir for 4-8h, and standing and aging for 12h after the stirring is finished to obtain the silica sol.
Preferably, in the step (1), the mass ratio of the 99.999% silicon powder to the absolute ethyl alcohol to the cyclotetrasiloxane to the anionic surfactant to the deionized water is 5-10:60-80:5-8:0.6-2: 9.4-20; the mass concentration of ammonia water is 25%.
Preferably, the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol in the step (2) is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
Preferably, the modifier is added in the step (2) in an amount of 0.05 to 0.1%.
Preferably, the modifier in the step (2) is a mixture of alpha-sodium alkenyl sulfonate, grafted cyclodextrin and the like.
Preferably, the grafted cyclodextrin is prepared by the following method:
1) dispersing beta-cyclodextrin in distilled water with equal mass, stirring for 1h, heating to 35 ℃, and adding Na2CO3Adjusting the pH of the system to be alkaline;
2) adding 50 percent of dodecenyl succinic anhydride absolute ethyl alcohol solution by mass fraction and simultaneously adding Na2CO 3The solution is used for keeping the pH of a reaction system to be alkaline;
3) and (3) adjusting the pH value of the reaction liquid obtained in the step (2) to be neutral by using hydrochloric acid, extracting by using an ethanol water solution, washing, performing suction filtration, and finally drying in an oven to constant weight to obtain the grafted cyclodextrin.
Preferably, Na is used in the step (1) and the step (2)2CO3The concentration of the solution was 2 mol/L.
Preferably, the pH ranges from 7 to 9 in step (1) and step (2).
Preferably, the mass fraction of the hydrochloric acid in the step (3) is 2%.
Preferably, the temperature of the step (3) oven is greater than 55 ℃ and not more than 80 ℃.
There are three types of silicon hydroxyl groups on the surface of nano-silica: (1) isolated monosilicon hydroxyl, ≡ Si-OH; (2) isolated bis-Si hydroxy, ═ Si- (OH)2(ii) a (3) The non-isolated silicon hydroxyl groups provide a structural basis for chemical modification thereof. The specific surface free energy of the nano silicon dioxide is larger and unstable; the specific surface area is large, and more silicon hydroxyl groups exist, so that one molecule of water is easily condensed among the silicon hydroxyl groups to generate agglomeration. The colloidal particle size of the colloidal solution is generally 1-100 nm, and the colloidal solution is formed by uniformly dispersing aggregated particles of amorphous silicon dioxide in water. Because the surface of the silicon dioxide particles in the silica sol contains a large amount of hydroxyl groups, the silicon dioxide particles have higher reaction activity and can be mixed and dissolved with organic polymers after surface modification, the silicon dioxide particles are widely used in various industries such as coating, precision casting, papermaking, textile, petrochemical industry, electronics and the like
However, when the size of the nano silica particles is larger than 100nm, the nano silica particles cannot be uniformly dispersed among polymer chains, not only the reinforcing and toughening effects cannot be achieved, but also the mechanical properties of the polymer matrix can be damaged.
The particle size is one of the key indexes in the silica sol product, which not only influences the concentration and stability of the product, but also directly influences the function of the product. Large-particle and high-concentration silica sol products of overseas cross-country companies such as NISSAN, AKZONOBEL and the like enter domestic markets in recent years. However, most of domestic silica sol production enterprises can only produce common silica sol products with the particle size of 10-20 nm. The problems of small particle size, poor uniformity and the like of the silicon dioxide are always main factors for restricting domestic enterprises to produce multifunctional and high-quality silica sol products. Many researchers in China study the preparation of large-particle-size silicon dioxide, and large-particle nano silicon dioxide is obtained to a certain extent. For example, in patent CN86104144A, silicon powder and water glass are directly reacted to obtain 20-30 nm silicon dioxide; in the patent CN1155514A, water glass is used as a raw material, and the particle size of silicon dioxide is finally increased to 40-50nm by adopting constant liquid level evaporation and multiple circulating dilution ultrafiltration processes; the chemical research institute of landification corporation in Lanzhou takes water glass as raw material, and adopts a constant liquid level evaporation and dropping process to prepare silicon dioxide with the average particle size of 55-65 nm. However, the prepared silica particles are still not large enough, the uniformity is still not good, the process is complicated, the energy consumption is high, and the production cost is high.
The invention takes tetraethoxysilane as a silicon source and adopts a sol-gel method to controllably prepare the monodisperse nano silicon dioxide particles. The silica sol with large particle size and high stability has industrial production value, and the preparation of the silica sol with large particle size by adding the surfactant to improve the stability of the sol is an important direction for researching the sol with large particle size. The stability of the silica sol is greatly affected by the excessive addition of the surfactant.
Therefore, the invention prepares the silica sol, two reagents are screened to modify the silica sol in the preparation process, the alpha-sodium alkenyl sulfonate is added, the addition of the sulfonic group side chain can effectively prevent the shrinkage agglomeration between silicon hydroxyl groups, the addition of the grafted cyclodextrin can improve the interface adsorption force on the surface of the silicon dioxide, can promote the uniform dispersion of the alpha-sodium alkenyl sulfonate on the surface of the particles, the two have synergistic interaction, the particle size of the obtained silica sol particles is between 100 and 400 nanometers, the concentration is about 50 percent, the particle size distribution is uniform, and the stability is good. The preparation method of the silica sol has simple process and low cost, and is suitable for large-scale popularization and application.
Drawings
FIG. 1 is a TEM image of a silica sol obtained in example 3 of the present invention;
FIG. 2 is a graph showing a distribution of the particle size of a silica sol obtained in example 3 of the present invention.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments, but is not limited thereto.
Example 1
A preparation method of silica sol comprises the following steps:
1) pouring 99.999% of silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a single-neck flask equipped with a condenser pipe and a thermometer in sequence, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing ethyl orthosilicate and absolute ethyl alcohol to obtain solution B, pouring the solution B into the solution A, dropwise adding ammonia water or organic amine with the mass percentage of 0.05% of the mixed solution AB, and reacting for 1h at 50 ℃; and (3) adding a modifier into the mixed solution obtained in the step (2), continuing magnetically stirring for 4 hours, and standing and aging for 12 hours after the stirring is finished to obtain the silica sol.
In the step (1), the mass ratio of 99.999% of silicon powder to absolute ethyl alcohol to cyclotetrasiloxane to anionic surfactant to deionized water is 5:60:5:0.6: 9.4; the mass concentration of ammonia water is 25%. In the step (2), the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
The addition amount of the modifier in the step (2) is 0.05%.
In the step (2), the modifier is prepared by mixing alpha-sodium alkenyl sulfonate, grafted cyclodextrin and the like in mass.
The alpha-alkenyl sodium sulfonate is dodecenyl sodium sulfonate.
The grafted cyclodextrin is prepared by the following method:
1) dispersing beta-cyclodextrin in distilled water with equal mass, stirring for 1h, heating to 35 ℃, and adding Na2CO3Adjusting the pH of the system to be alkaline;
2) adding 50 percent of dodecenyl succinic anhydride absolute ethyl alcohol solution by mass fraction and simultaneously adding Na2CO3The solution is used for keeping the pH of a reaction system to be alkaline;
3) and (3) adjusting the pH value of the reaction liquid obtained in the step (2) to be neutral by using hydrochloric acid, extracting by using an ethanol water solution, washing, performing suction filtration, and finally drying in an oven to constant weight to obtain the grafted cyclodextrin.
Na in step (1) and step (2)2CO3The concentration of the solution was 2 mol/L.
The pH range in the step (1) and the step (2) is 7-9.
The mass fraction of the hydrochloric acid in the step (3) is 2%.
The temperature of the oven in the step (3) is more than 55 ℃ and is not more than 80 ℃.
Example 2
A preparation method of silica sol comprises the following steps:
1) pouring 99.999% of silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a single-neck flask equipped with a condenser pipe and a thermometer in sequence, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing tetraethoxysilane and absolute ethyl alcohol to obtain a solution B, pouring the solution B into the solution A, dropwise adding ammonia water or organic amine with the mass percentage of 0.15% of the mixed solution AB, and reacting for 1h at 50 ℃; and (3) adding a modifier into the mixed solution obtained in the step (2), continuing to magnetically stir for 6 hours, and standing and aging for 12 hours after the stirring is finished to obtain the silica sol.
In the step (1), the mass ratio of 99.999% of silicon powder to absolute ethyl alcohol to cyclotetrasiloxane to anionic surfactant to deionized water is 8:70:7:1.2: 15; the mass concentration of ammonia water is 25%. In the step (2), the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
The addition amount of the modifier in the step (2) is 0.08%.
In the step (2), the modifier is prepared by mixing alpha-sodium alkenyl sulfonate, grafted cyclodextrin and the like in mass.
The alpha-sodium alkenyl sulfonate is tetradecene sodium alkenyl sulfonate.
The grafted cyclodextrin is prepared by the following method:
1) dispersing beta-cyclodextrin in distilled water with equal mass, stirring for 1h, heating to 35 ℃, and adding Na2CO3Adjusting the pH of the system to be alkaline;
2) adding 50 percent of dodecenyl succinic anhydride absolute ethyl alcohol solution by mass fraction and simultaneously adding Na2CO3The solution is used for keeping the pH of a reaction system to be alkaline;
3) and (3) adjusting the pH value of the reaction liquid obtained in the step (2) to be neutral by using hydrochloric acid, extracting by using an ethanol water solution, washing, performing suction filtration, and finally drying in an oven to constant weight to obtain the grafted cyclodextrin.
Na in step (1) and step (2)2CO3The concentration of the solution was 2 mol/L.
The pH range in the step (1) and the step (2) is 7-9.
The mass fraction of the hydrochloric acid in the step (3) is 2%.
The temperature of the oven in the step (3) is more than 55 ℃ and is not more than 80 ℃.
Example 3
A preparation method of silica sol comprises the following steps:
1) pouring 99.999% of silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a single-neck flask equipped with a condenser pipe and a thermometer in sequence, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing tetraethoxysilane and absolute ethyl alcohol to obtain a solution B, pouring the solution B into the solution A, dropwise adding ammonia water or organic amine with the mass percentage of 0.3% of the mixed solution AB, and reacting for 1h at 50 ℃; and (3) adding a modifier into the mixed solution obtained in the step (2), continuing magnetically stirring for 8 hours, and standing and aging for 12 hours after the stirring is finished to obtain the silica sol.
In the step (1), the mass ratio of 99.999% of silicon powder to absolute ethyl alcohol to cyclotetrasiloxane to anionic surfactant to deionized water is 10:80:8:2: 20; the mass concentration of ammonia water is 25%. In the step (2), the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
The addition amount of the modifier in the step (2) is 0.1%.
In the step (2), the modifier is prepared by mixing alpha-sodium alkenyl sulfonate, grafted cyclodextrin and the like in mass.
The alpha-sodium alkenyl sulfonate is sodium hexadecenyl sulfonate.
The grafted cyclodextrin is prepared by the following method:
1) dispersing beta-cyclodextrin in distilled water with equal mass, stirring for 1h, heating to 35 ℃, and adding Na2CO3Adjusting the pH of the system to be alkaline;
2) adding 50 percent of dodecenyl succinic anhydride absolute ethyl alcohol solution by mass fraction and simultaneously adding Na2CO3The solution is used for keeping the pH of a reaction system to be alkaline;
3) and (3) adjusting the pH value of the reaction liquid obtained in the step (2) to be neutral by using hydrochloric acid, extracting by using an ethanol water solution, washing, performing suction filtration, and finally drying in an oven to constant weight to obtain the grafted cyclodextrin.
Na in step (1) and step (2)2CO3The concentration of the solution was 2 mol/L.
The pH range in the step (1) and the step (2) is 7-9.
The mass fraction of the hydrochloric acid in the step (3) is 2%.
The temperature of the oven in the step (3) is more than 55 ℃ and is not more than 80 ℃.
Comparative example 1
A preparation method of silica sol comprises the following steps:
1) pouring 99.999% of silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a single-neck flask equipped with a condenser pipe and a thermometer in sequence, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing tetraethoxysilane and absolute ethyl alcohol to obtain a solution B, pouring the solution B into the solution A, dropwise adding ammonia water or organic amine with the mass percentage of 0.3% of the mixed solution AB, and reacting for 1h at 50 ℃; and (3) adding a modifier into the mixed solution obtained in the step (2), continuing magnetically stirring for 8 hours, and standing and aging for 12 hours after the stirring is finished to obtain the silica sol.
In the step (1), the mass ratio of 99.999% of silicon powder to absolute ethyl alcohol to cyclotetrasiloxane to anionic surfactant to deionized water is 10:80:8:2: 20; the mass concentration of ammonia water is 25%. In the step (2), the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
The addition amount of the modifier in the step (2) is 0.1%.
In the step (2), the modifier is alpha-sodium alkenyl sulfonate.
The alpha-sodium alkenyl sulfonate is sodium hexadecenyl sulfonate.
Na in step (1) and step (2)2CO3The concentration of the solution was 2 mol/L.
The pH range in the step (1) and the step (2) is 7-9.
The mass fraction of the hydrochloric acid in the step (3) is 2%.
The temperature of the oven in the step (3) is more than 55 ℃ and is not more than 80 ℃.
Comparative example 2
A preparation method of silica sol comprises the following steps:
1) pouring 99.999% of silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a single-neck flask equipped with a condenser pipe and a thermometer in sequence, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing tetraethoxysilane and absolute ethyl alcohol to obtain a solution B, pouring the solution B into the solution A, dropwise adding ammonia water or organic amine with the mass percentage of 0.3% of the mixed solution AB, and reacting for 1h at 50 ℃; and (3) adding a modifier into the mixed solution obtained in the step (2), continuing magnetically stirring for 8 hours, and standing and aging for 12 hours after the stirring is finished to obtain the silica sol.
In the step (1), the mass ratio of 99.999% of silicon powder to absolute ethyl alcohol to cyclotetrasiloxane to anionic surfactant to deionized water is 10:80:8:2: 20; the mass concentration of ammonia water is 25%. In the step (2), the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
The addition amount of the modifier in the step (2) is 0.1%.
The modifier in the step (2) is grafted cyclodextrin.
The grafted cyclodextrin is prepared by the following method:
1) dispersing beta-cyclodextrin in distilled water with equal mass, stirring for 1h, heating to 35 ℃, and adding Na2CO3Adjusting the pH of the system to be alkaline;
2) adding 50 percent of dodecenyl succinic anhydride absolute ethyl alcohol solution by mass fraction and simultaneously adding Na2CO3The solution is used for keeping the pH of a reaction system to be alkaline;
3) and (3) adjusting the pH value of the reaction liquid obtained in the step (2) to be neutral by using hydrochloric acid, extracting by using an ethanol water solution, washing, performing suction filtration, and finally drying in an oven to constant weight to obtain the grafted cyclodextrin.
Na in step (1) and step (2)2CO3The concentration of the solution was 2 mol/L.
The pH range in the step (1) and the step (2) is 7-9.
The mass fraction of the hydrochloric acid in the step (3) is 2%.
The temperature of the oven in the step (3) is more than 55 ℃ and is not more than 80 ℃.
Comparative example 3
A preparation method of silica sol comprises the following steps:
1) pouring 99.999% of silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a single-neck flask equipped with a condenser pipe and a thermometer in sequence, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing tetraethoxysilane and absolute ethyl alcohol to obtain a solution B, pouring the solution B into the solution A, dropwise adding ammonia water or organic amine with the mass percentage of 0.3% of the mixed solution AB, and reacting for 1h at 50 ℃; and continuing magnetic stirring for 8 hours, and standing and aging for 12 hours after the magnetic stirring is finished to obtain the silica sol.
In the step (1), the mass ratio of 99.999% of silicon powder to absolute ethyl alcohol to cyclotetrasiloxane to anionic surfactant to deionized water is 10:80:8:2: 20; the mass concentration of ammonia water is 25%. In the step (2), the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
The basic performance of the silica sols obtained in the examples and comparative examples was tested
Particle size measurement
Taking 2ml of sol, testing the particle size and distribution of the sol by using a laser particle size distribution instrument at 25 ℃, selecting ethanol as a solvent, balancing for 120s, testing for 30 times each time, and testing for 3 times in total.
TEM test
Silica sol was dropped on the copper mesh, dried under an infrared lamp for 15 minutes, and then the internal structure thereof was observed by a transmission electron microscope.
The silicon content was determined after drying the silica sol at 125 ℃ for 5 hours.
The specific test results are shown in the following table:
table 1 results of performance testing
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Claims (8)
1. A preparation method of silica sol is characterized by comprising the following steps:
1) sequentially pouring silicon powder, absolute ethyl alcohol, cyclotetrasiloxane, anionic surfactant TMA and deionized water into a flask, and stirring for 15min by adopting magnetic force to obtain solution A;
2) mixing ethyl orthosilicate and absolute ethyl alcohol to obtain solution B, dripping the solution B into the solution A, dripping ammonia water or organic amine with the mass percentage of 0.05-0.3% of the mixed solution AB, and reacting for 4 hours at 50 ℃; adding a modifier into the obtained mixed solution, continuing to magnetically stir for 4-8h, and standing and aging for 12h after the stirring is finished to obtain silica sol;
in the step 2), the modifier is prepared by mixing alpha-sodium alkenyl sulfonate, grafted cyclodextrin and the like in mass;
the grafted cyclodextrin is prepared by the following method:
(1) dispersing beta-cyclodextrin in distilled water with equal mass, stirring for 1h, heating to 35 ℃, and adding Na2CO3Adjusting the pH of the system to be alkaline;
(2) adding 50 percent of dodecenyl succinic anhydride absolute ethyl alcohol solution by mass fraction and simultaneously adding Na2CO 3The solution is used for keeping the pH of a reaction system to be alkaline;
(3) and (3) adjusting the pH value of the reaction liquid obtained in the step (2) to be neutral by using hydrochloric acid, extracting by using an ethanol water solution, washing, performing suction filtration, and finally drying in an oven to constant weight to obtain the grafted cyclodextrin.
2. The method for preparing the silica sol according to claim 1, wherein the mass ratio of the silicon powder, the absolute ethyl alcohol, the cyclotetrasiloxane, the anionic surfactant TMA and the deionized water in the step 1) is 5-10:60-80:5-8:0.6-2: 9.4-20; the mass concentration of ammonia water is 25%.
3. The method for preparing silica sol according to claim 1, wherein the volume ratio of tetraethoxysilane to absolute ethyl alcohol in the step 2) is 1:5, and the volume ratio of the solution A to the solution B is 2: 1.
4. The method for producing a silica sol according to claim 1, wherein the modifier is added in the amount of 0.05 to 0.1% in the step 2).
5. The method for producing the silica sol according to claim 1, wherein Na is used in the step (1) and the step (2)2CO3The concentration of the solution was 2 mol/L.
6. The method for producing a silica sol according to claim 1, wherein the pH in the step (1) and the step (2) is in the range of 7 to 9.
7. The method for producing a silica sol according to claim 1, wherein the hydrochloric acid in the step (3) is contained in an amount of 2% by mass.
8. The method for preparing silica sol according to claim 1, wherein the temperature of the oven in the step (3) is more than 55 ℃ and not more than 80 ℃.
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| CN103030151A (en) * | 2012-12-05 | 2013-04-10 | 广东惠和硅制品有限公司 | Neutral large-particle-size high-concentration and high-purity silica solution, and preparation and use of the same |
| CN103896289A (en) * | 2014-04-19 | 2014-07-02 | 济南银丰化工有限公司 | Method for preparing silica sol with large grain size |
| CN104495857A (en) * | 2014-12-10 | 2015-04-08 | 深圳市力合材料有限公司 | Method for rapidly preparing large-particle-size silica sol |
| CN106744998A (en) * | 2017-01-17 | 2017-05-31 | 清华大学 | A kind of controllable amorphous monodisperse nano silicon dioxide raw powder's production technology of granularity |
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