CN115571886B - Preparation method of low-oil-absorption low-specific-surface-area silicon dioxide - Google Patents
Preparation method of low-oil-absorption low-specific-surface-area silicon dioxide Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 40
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000010521 absorption reaction Methods 0.000 title abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 63
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 53
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 230000032683 aging Effects 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000004537 pulping Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000001694 spray drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 13
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 11
- 230000001276 controlling effect Effects 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000009775 high-speed stirring Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 239000003921 oil Substances 0.000 abstract description 17
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 abstract description 2
- 229960001866 silicon dioxide Drugs 0.000 description 23
- 239000002245 particle Substances 0.000 description 13
- 239000002253 acid Substances 0.000 description 9
- 239000006229 carbon black Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007863 gel particle Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000006224 matting agent Substances 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000606 toothpaste Substances 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012628 flowing agent Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229960004029 silicic acid Drugs 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
Classifications
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- 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
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
-
- 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
- C01B33/142—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates
- C01B33/143—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates of aqueous solutions of silicates
-
- 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
- C01B33/152—Preparation of hydrogels
- C01B33/154—Preparation of hydrogels by acidic treatment of aqueous silicate solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
Abstract
The invention discloses a preparation method of low oil absorption and low specific surface area silicon dioxide, which comprises the following steps of S1, preparing water glass solution with concentration of 1.20 mol/L-1.40 mol/L; s2, preparing a dilute sulfuric acid solution with the mass concentration of 18% -30%; s3, adding water into the reaction kettle, adding the prepared water glass solution at the same time, heating to 85-90 ℃, stirring, dripping the prepared dilute sulfuric acid solution, controlling the pH at the reaction end point to be 3.0-4.0, and stirring and aging; s4, adding water at 30-40 ℃ into a reaction kettle, reducing the temperature to 65-70 ℃, simultaneously dropwise adding the prepared water glass solution and concentrated sulfuric acid, adjusting the flow rate of the sulfuric acid to control the pH value of the reaction process to 7.0-8.0, stopping adding the water glass after 120-130 min of reaction, continuously adding the concentrated sulfuric acid to complete the reaction, stirring until the pH value is 4.0-5.0, and aging to obtain silicon dioxide slurry; s5, washing, solid-liquid separation, pulping and spray drying to obtain silicon dioxide powder. The invention solves the problems of easy gel generation, large specific surface area, long production period, low yield and large influence on environment in the reaction process in the prior art.
Description
Technical Field
The invention relates to the technical field of preparation methods of white carbon black, in particular to a preparation method of silica with low oil absorption and low specific surface area.
Background
The precipitated hydrated silica is also called white carbon black, belongs to the field of inorganic silicide, and is an important inorganic chemical raw material. White carbon black has very wide application due to its special surface structure and unique physicochemical properties. As a reinforcing agent for rubber (including silicone rubber) products, mainly used in the footwear industry, tires and other light-colored rubber products; used as a carrier or a flowing agent in the industries of pesticides, feeds and the like; as abrasives and thickeners in toothpastes; as dispersants, anti-settling agents or matting agents in the coating industry; the industries such as medicine and food are widely used as adsorbents.
The precipitated silica is of an amorphous porous structure, the surface of the precipitated silica is rich in hydroxyl groups, the specific surface area is adjustable, and the larger the specific surface area is, the more the hydroxyl groups on the surface of the white carbon black are; the oil absorption value (DBP value) of the white carbon black is an important index for representing the microstructure of the white carbon black, and the larger the DBP value is, the more developed the bond dendritic structure of the three-dimensional network is, and the smaller the DBP value is, the more compact the particles are. The DBP value is 1.1-2.1 ml/g, which belongs to low oil absorption value and low structure products, has good dispersion and suspension performance, compact particles and strong friction force, and can be used as the fields of toothpaste friction agent, paint matting agent and the like. Silicon dioxide is added into the silicon rubber, and the silicon dioxide forms a three-dimensional network structure in the system, and the silicon dioxide can form a crosslinking effect with rubber macromolecules, so that the reinforcing effect of the silicon rubber can be effectively improved by adding the silicon dioxide. The higher oil absorption value leads to long raw rubber powder eating time, and the too high surface hydroxyl content leads to high addition of a structuring control agent (such as hydroxyl silicone oil), thereby increasing the production cost.
Chinese patent CN 104530770A discloses a preparation method of matting powder with high transparency and low oil absorption value, the invention adopts a two-step synthesis method, and simultaneously adds substances such as modifier, coupling agent, ethanol, etc., the synthesis process comprises adding acid: adding acid into sodium silicate to form gel, stopping adding acid, and heating to 48-52 ℃; and (3) adding fluorine: adding a fluorine-containing organic modifier, and simultaneously adding one or more coupling agents to carry out surface modification; and (3) secondary wrapping: heating to 55-85 ℃, adding the crosslinkable long-chain organic matter and silicon dioxide to carry out crosslinking reaction, and simultaneously adding ethanol to carry out secondary coating. The white carbon black prepared by the method can basically meet the quality requirement of the extinction powder with high transparency and low oil absorption value, but has the defects of easy gel generation, larger specific surface area, longer production period, low yield and larger environmental influence caused by adding various organic solvents in the reaction process.
Therefore, there is a need to develop a silica having a high yield, a production environment, a low oil absorption value, a low specific surface area, and a high dispersion.
Disclosure of Invention
The invention aims to provide a preparation method of low-oil-absorption low-specific-surface-area silicon dioxide, which solves the problems of easy generation of gel, larger specific surface area, longer production period, low yield and larger environmental influence caused by adding various organic solvents in the reaction process in the prior art.
In order to achieve the above object, the preparation method of the silica with low oil absorption and low specific surface area comprises the following steps:
s1, adding water into sodium silicate liquid with the modulus of 3.40-3.50 to dilute the sodium silicate liquid to prepare sodium silicate solution with the concentration of 1.20 mol/L-1.40 mol/L;
s2, adding water into concentrated sulfuric acid with the mass concentration of 98% to prepare a dilute sulfuric acid solution with the mass concentration of 18% -30%;
s3, adding 13.5-18.0 m into a stainless steel reaction kettle with a high-speed stirring device 3 Adding water into the water glass solution prepared in the step S1 for 2.0-2.4 m 3 And (2) heating the mixture to 85-90 ℃ by steam, starting stirring, dropwise adding the dilute sulfuric acid solution prepared in the step (S2) into a reaction kettle for 20-30 min, controlling the pH at the end point of the reaction to 3.0-4.0, and stirring and aging for 30min.
S4, adding water with the temperature of 30-40 ℃ into a reaction kettle, reducing the temperature to 65-70 ℃, and simultaneously dropwise adding the water glass solution prepared in the step S1 and concentrated sulfuric acid with the mass concentration of 98%, wherein the water glass flow rate is 18.0-19.0 m 3 And (3) controlling the pH value of the reaction process to be 7.0-8.0 by adjusting the flow rate of sulfuric acid, stopping adding water glass after reacting for 120-130 min, continuously adding concentrated sulfuric acid to enable the water glass in the reaction kettle to react completely, stirring to be uniform suspension, regulating the pH value of the suspension to be 4.0-5.0, and continuously aging for 10-30 min to obtain silicon dioxide slurry;
s5, washing, solid-liquid separation, pulping and spray drying the silicon dioxide slurry prepared in the step S4 to obtain silicon dioxide powder.
The preparation method of the silica with low oil absorption and low specific surface area has the following technical characteristics and beneficial effects:
(1) The preparation process of the silicon dioxide adopts two reactions, wherein one reaction is a sol reaction, and the reaction is carried out at a higher temperature of 85-90 ℃ with higher bottom alkali concentration, so that the speed of forming gel by the sol is reduced, the sol slowly forms small gel particles, the gel particles are continuously aggregated to cause the silicon dioxide particles to become large, and the silicon dioxide with low specific surface area is obtained.
(2) The pH gradually decreases from above 11.0 to 3.0-5.0 in the primary sol reaction, so that a large amount of OH-is adsorbed on the surface of the silicon dioxide particles in the early stage, the crystal grains are continuously grown, and a large amount of H is adsorbed in the later stage + Like poles repel to prevent grains from continuously gathering, so that gel particles with uniform particle sizes can be obtained; because the pore diameter of the gel particles obtained by one-time reaction is unstable, the problems of acid regulation and aging are solved, and the particles are integrated in the aging process, so that the structure of the gel particles is more stable, and the compact crystal nucleus of the particles is obtained.
(3) The pH value of the secondary precipitation reaction is controlled to be 7.0-8.0, under the weak acid neutral condition, the neutralization rate of acid and alkali in the reaction system is higher, crystal grains grow up rapidly, compact particles are formed, the specific surface area of the particles is reduced, and the stacking density of silicon dioxide is improved; the reaction is carried out at a lower temperature of 65-70 ℃, the activity of the grown silicon dioxide particles is poor, the collision among the particles can be reduced, and the branched chain structure of the silicon dioxide particles is reduced, so that the oil absorption value of the silicon dioxide is reduced.
(4) Organic solvents such as a cross-linking agent, a coupling agent and the like are not used in the reaction process, the production process is environment-friendly, and the influence on the environment is small.
(5) The surface modification process is not needed, the secondary precipitation reaction is not needed to be heated again, and the reaction period can be shortened.
(6) The secondary precipitation uses a larger water glass flow rate, and the reaction time is longer, so that the yield of the single-kettle silicon dioxide can be greatly improved.
The preparation method of the silica with low oil absorption value and low specific surface area is simple and easy to implement, has high yield, does not generate a large amount of gel in the preparation process, and has the advantages of small oil absorption value, low specific surface area and uniform particle size distribution.
Detailed Description
The method for preparing the low oil absorption and low specific surface area silica according to the present invention will be described in further detail with reference to the following embodiments.
Example 1
S1, preparing reaction water glass: taking sodium silicate liquid with the modulus of 3.45, and adding water to dilute the sodium silicate liquid into the concentration of 1.20-1.40 mol/L;
s2, preparing acid for reaction: taking concentrated sulfuric acid with the mass ratio concentration of 98%, and adding water to prepare dilute sulfuric acid with the mass concentration of 25%;
s3, 90m direction 3 Adding 13.5m into a stainless steel reaction kettle with a high-speed stirring device 3 Water is added into the water glass prepared in the step S1 at the same time, 2.0m 3 Heating steam to 85 ℃, starting stirring, dropwise adding the dilute sulfuric acid solution prepared in the step S1 into a reaction kettle for 30min, controlling the pH at the reaction end point to be 3.5, and stirring and aging for 30min;
s4, adding a certain amount of water with the temperature of 30-40 ℃ into the reaction kettle, reducing the temperature to 65 ℃, and simultaneously dropwise adding the water glass solution prepared in the step S1 and the concentrated sulfuric acid with the mass concentration of 98%, wherein the water glass flow rate is 18.5m 3 And (3) regulating the flow rate of sulfuric acid, controlling the pH value of the reaction process to be 7.5, stopping adding water glass after 120min of reaction, continuously adding concentrated sulfuric acid to completely react the water glass in the reaction kettle, stirring to obtain a uniform suspension, regulating the pH value of the suspension to be 4.0, and continuously aging for 30min to obtain silicon dioxide slurry;
s5, washing, solid-liquid separation, pulping and spray drying the silicon dioxide slurry prepared in the step S4 to obtain silicon dioxide powder.
Example 2
S1, preparing reaction water glass: taking sodium silicate liquid with the modulus of 3.50, and adding water to dilute the sodium silicate liquid into the concentration of 1.20-1.40 mol/L;
s2, preparing acid for reaction: taking concentrated sulfuric acid with the mass ratio concentration of 98%, and adding water to prepare dilute sulfuric acid with the mass concentration of 30%;
s3, 90m direction 3 Adding 16.5m into a stainless steel reaction kettle with a high-speed stirring device 3 Water is added into the water glass prepared in the step S1 at the same time, 2.4m 3 Heating the steam to 90 ℃, stirring, and dripping into the reaction kettleThe dilute sulfuric acid solution prepared in the step S1 is dropwise added for 25min, the pH of the reaction end point is controlled to be 3.5, and the mixture is stirred and aged for 30min;
s4, adding a certain amount of water with the temperature of 30-40 ℃ into the reaction kettle, reducing the temperature to 70 ℃, and simultaneously dropwise adding the water glass solution prepared in the step S1 and the concentrated sulfuric acid with the mass concentration of 98%, wherein the water glass flow rate is 19.0m 3 And (3) regulating the flow rate of sulfuric acid, controlling the pH value of the reaction process to be 7.0, stopping adding water glass after 125 minutes of reaction, continuously adding concentrated sulfuric acid to completely react the water glass in the reaction kettle, stirring to obtain a uniform suspension, regulating the pH value of the suspension to be 4.5, and continuously aging for 20 minutes to obtain silicon dioxide slurry;
s5, washing, solid-liquid separation, pulping and spray drying the silicon dioxide slurry prepared in the step S4 to obtain silicon dioxide powder.
Example 3
S1, preparing reaction water glass: taking sodium silicate liquid with the modulus of 3.40, and adding water to dilute the sodium silicate liquid into the concentration of 1.20-1.40 mol/L;
s2, preparing acid for reaction: taking concentrated sulfuric acid with the mass ratio concentration of 98%, and adding water to prepare dilute sulfuric acid with the mass ratio concentration of 18%;
s3, 90m direction 3 Adding 18.0m into a stainless steel reaction kettle with high-speed stirring 3 Water is added into the water glass prepared in the step S1 at the same time, 2.4m 3 Heating steam to 88 ℃, starting stirring, dropwise adding the dilute sulfuric acid solution prepared in the step S1 into a reaction kettle for 20min, controlling the pH at the reaction end point to be 4.0, and stirring and aging for 30min;
s4, adding a certain amount of water with the temperature of 30-40 ℃ into the reaction kettle, reducing the temperature to 65 ℃, and simultaneously dropwise adding the water glass solution prepared in the step S1 and the concentrated sulfuric acid with the mass concentration of 98%, wherein the water glass flow rate is 18.0m 3 And (3) regulating the flow rate of sulfuric acid, controlling the pH value of the reaction process to 8.0, stopping adding water glass after the reaction time is 130min, continuously adding concentrated sulfuric acid to completely react the water glass in the reaction kettle, stirring to obtain a uniform suspension, regulating the pH value of the suspension to 5.0, and continuously aging for 10min to obtain the silicon dioxide slurry;
s5, washing, solid-liquid separation, pulping and spray drying the silicon dioxide slurry prepared in the step S4 to obtain silicon dioxide powder.
Comparative example 1
Step S3 controls the pH at the end of the reaction to 8.0, and the other conditions are the same as in example 1.
Comparative example 2
Step S4 controls the pH of the reaction process to 10.5, and the reaction temperature is 90 ℃ and other conditions are the same as in example 1.
Comparative example 3
Step S4 was performed for 80min under the same conditions as in example 1.
The technical indexes of the white carbon black product detection prepared in the embodiment are compared with those of the comparative example and the technical requirements, and the following table is provided:
as can be seen from the above table, the oil absorption values of the silica prepared in examples 1 to 3 of the present invention are 1.87 to 1.95cm 3 Per gram, specific surface area 116-125 m 2 The oil absorption and specific surface area were significantly reduced as compared to the comparative examples, with the overall technical index of example 2 being the best, and being the best. The silica of examples 1 to 3 of the present invention meets the technical requirements of low oil absorption value and low specific surface area silica.
It should be noted that, the above embodiments are not intended to limit the present invention, and those skilled in the art may still modify the technical solutions described in the foregoing embodiments or perform equivalent substitution on some technical features thereof; any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A preparation method of silicon dioxide is characterized in that: the operation steps are as follows:
s1, adding water into sodium silicate liquid with the modulus of 3.40-3.50 to dilute the sodium silicate liquid to prepare sodium silicate solution with the concentration of 1.20 mol/L-1.40 mol/L;
s2, adding water into concentrated sulfuric acid with the mass concentration of 98% to prepare a dilute sulfuric acid solution with the mass concentration of 18% -30%;
s3, adding 13.5-18.0 m into a stainless steel reaction kettle with a high-speed stirring device 3 Adding water into the water glass solution prepared in the step S1 for 2.0-2.4 m 3 And (2) heating the mixture to 85-90 ℃ by steam, starting stirring, dropwise adding the dilute sulfuric acid solution prepared in the step (S2) into a reaction kettle for 20-30 min, controlling the pH at the end point of the reaction to 3.0-4.0, and stirring and aging for 30min.
S4, adding water with the temperature of 30-40 ℃ into a reaction kettle, reducing the temperature to 65-70 ℃, and simultaneously dropwise adding the water glass solution prepared in the step S1 and concentrated sulfuric acid with the mass concentration of 98%, wherein the water glass flow rate is 18.0-19.0 m 3 And (3) controlling the pH value of the reaction process to be 7.0-8.0 by adjusting the flow rate of sulfuric acid, stopping adding water glass after reacting for 120-130 min, continuously adding concentrated sulfuric acid to enable the water glass in the reaction kettle to react completely, stirring to be uniform suspension, regulating the pH value of the suspension to be 4.0-5.0, and continuously aging for 10-30 min to obtain silicon dioxide slurry;
s5, washing, solid-liquid separation, pulping and spray drying the silicon dioxide slurry prepared in the step S4 to obtain silicon dioxide powder.
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