CN112607744A - Preparation method of silicon dioxide with high oil absorption value - Google Patents
Preparation method of silicon dioxide with high oil absorption value Download PDFInfo
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- CN112607744A CN112607744A CN202011593849.6A CN202011593849A CN112607744A CN 112607744 A CN112607744 A CN 112607744A CN 202011593849 A CN202011593849 A CN 202011593849A CN 112607744 A CN112607744 A CN 112607744A
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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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
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- 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
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- 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
- C01P2006/80—Compositional purity
Abstract
The invention provides a preparation method of high oil absorption value silicon dioxide, which comprises the following steps: (1) adding a water glass solution into water, diluting the water glass solution, and adding anhydrous sodium sulfate to obtain a reaction bottom solution; (2) adding acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant; (3) and after the reaction is finished, adding acid into the reaction medium to adjust the pH value to obtain a silicon dioxide suspension, carrying out solid-liquid separation, and carrying out aftertreatment on the obtained silicon dioxide to obtain the silicon dioxide with the high oil absorption value. The silica prepared by the preparation method has high oil absorption value, improves the added value of the product, completely meets the new requirements of the high-end market of feed-grade silica products, and can be better applied to feed production.
Description
Technical Field
The invention belongs to the field of silicon dioxide preparation, relates to a preparation method of silicon dioxide, and particularly relates to a preparation method of silicon dioxide with a high oil absorption value.
Background
With the cross permeation and fusion development of the nano technology in the precipitated silica industry, special functional and special nano silica is developed rapidly. According to different physical and chemical characteristics of the silicon dioxide, the silicon dioxide can be used as a reinforcing filler of light-colored rubber, an opening agent of plastic, a flatting agent for paint, a resin compounding agent, a chemical absorbent, a filler for papermaking, a coating agent for special paper and the like, and is applied to various fields of the chemical industry. As the nano silicon dioxide applied to the powder, the size of the oil absorption value is a key index for determining the wetting and dispersion of the nano silicon dioxide and a matrix material. Generally, the high oil absorption silica has better affinity degree with a dispersion medium and good aggregate space structure, and can better embody the nanometer characteristics and the corresponding functions in a matrix material. The Rona-Planck chemical group controls the generation speed of the nanocrystal core by continuously dripping reactants in a constant volume manner, and prepares the high oil absorption silicon dioxide with controllable primary structure. The Qibo group adopts a multi-step double-dropping method to adjust the proportion of the primary structure and the secondary structure, so as to prepare the high oil absorption silicon dioxide hybrid material.
At present, raw materials used for producing domestic feed-grade silicon dioxide are mainly solid sodium silicate, and the production technology of a sulfuric acid precipitation method is adopted, so that the equipment is simple, the product activity is low, the granules are difficult to control, the affinity is poor, the reinforcing property is low, the water-based hydroxyl bonding on the surfaces of the granules is serious, the binding force of the product is weakened, the oil absorption of the product is low, and some high-end feed applications cannot be met.
CN111470512A discloses a method for preparing silica with high oil absorption value and large pore volume, which comprises the following steps: preparing a raw material solution; acidifying the sodium silicate aqueous solution B; acidifying the sodium silicate aqueous solution A; preparing a finished product: and (3) mixing the materials in the step (II) with the materials in the step (III) according to the mass ratio of 1: (0.95-1.05), adding the mixture into a reaction vessel, adjusting the pH value to 7.0, stirring and aging, depolymerizing, filtering, washing, pulping, and drying to obtain the silica with high oil absorption value and large pore volume. Although the prepared silicon dioxide has large specific surface area, the preparation method is complex and is not suitable for industrial production.
CN108190900A discloses a preparation method of friction type silicon dioxide with low specific surface area and high oil absorption value. The preparation method comprises S1 injection8-12 m of ethanol aqueous solution3Heating to 60-70 ℃, and starting stirring; s2, simultaneously dripping water glass and sulfuric acid to perform parallel flow reaction, controlling the pH value to be 6.0-6.8 in the reaction process, simultaneously adding absolute ethyl alcohol every 5-10 min in the reaction process to keep the volume ratio of the ethyl alcohol to the water in the reaction system to be 1 (3-7), stopping dripping the sulfuric acid after the water glass is dripped, and continuing stirring; s3 stopping stirring and heating, aging for 1h, and press-filtering, washing, drying and crushing the formed silicon dioxide to obtain the silicon dioxide.
Disclosure of Invention
In order to solve the technical problems, the application provides the preparation method of the high oil absorption value silicon dioxide, the silicon dioxide prepared by the preparation method is high in oil absorption value, the added value of the product is improved, the new requirements of the high-end market of feed-grade silicon dioxide products are completely met, and the preparation method can be better applied to feed production.
In order to achieve the technical effect, the invention adopts the following technical scheme:
the invention provides a preparation method of high oil absorption value silicon dioxide, which comprises the following steps:
(1) adding a water glass solution into water, diluting the water glass solution, and adding anhydrous sodium sulfate to obtain a reaction bottom solution;
(2) adding acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant;
(3) and after the reaction is finished, adding acid into the reaction medium to adjust the pH value to obtain a silicon dioxide suspension, carrying out solid-liquid separation, and carrying out aftertreatment on the obtained silicon dioxide to obtain the silicon dioxide with the high oil absorption value.
As a preferred embodiment of the present invention, the temperature of the water in the step (1) of adding the water glass solution is 70 to 98 ℃, such as 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, 88 ℃, 90 ℃, 92 ℃, 95 ℃ or 97 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, in step (1), the concentration of the glass solution is 20 to 40 wt%, such as 22 wt%, 25 wt%, 28 wt%, 30 wt%, 32 wt%, 35 wt%, or 38 wt%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In a preferred embodiment of the present invention, the concentration of the water glass in the diluted reaction solution in step (1) is 5 to 16 wt%, such as 6 wt%, 7 wt%, 8 wt%, 9 wt%, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, or 15 wt%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
As a preferred embodiment of the present invention, the concentration of sodium sulfate added to the reaction bottom liquid in step (1) is 10.5 to 20g/L, such as 11g/L, 12g/L, 13g/L, 14g/L, 15g/L, 16g/L, 17g/L, 18g/L or 19g/L, but is not limited to the values listed above, and other values not listed in the range of values are also applicable.
As a preferred embodiment of the present invention, the temperature of the system is maintained at 70 to 98 ℃ such as 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, 88 ℃, 90 ℃, 92 ℃, 95 ℃ or 97 ℃ during the preparation of the reaction base solution in step (1), but the temperature is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
As a preferable technical scheme of the invention, the acid in the step (2) comprises concentrated sulfuric acid;
preferably, the adding time of the concentrated sulfuric acid is 60-100 min, such as 65min, 70min, 75min, 80min, 85min, 90min or 95min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In the present invention, the concentration of water glass in the reaction bottom solution can be maintained constant by adjusting the addition rates of concentrated sulfuric acid and water glass solution. The reaction temperature was kept constant throughout the reaction of step (2).
As a preferred technical scheme of the invention, the acid in the step (3) comprises concentrated sulfuric acid.
Preferably, the pH of step (3) is adjusted to 3-5, such as 3.2, 3.5, 3.8, 4, 4.2, 4.5, or 4.8, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferred embodiment of the present invention, the post-treatment in step (3) comprises washing, slurrying and drying the silica.
In the invention, solid-liquid separation adopts filter pressing, and the filter pressing and washing steps comprise filtering and washing of a precipitated silica suspension generated by a precipitation reaction by using a diaphragm type filter press to form a filter cake, wherein the silica content is 20-23 wt%.
Preferably, the solvent used for the slurry is an organic solvent.
Preferably, the organic solvent comprises n-butanol.
Preferably, the organic solvent is added in an amount of 6 to 10% by mass of the silica, such as 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, or 9.5%, but not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the time of the slurry process is 1 to 2 hours, such as 1.1 hour, 1.2 hours, 1.3 hours, 1.4 hours, 1.5 hours, 1.6 hours, 1.7 hours, 1.8 hours, 1.9 hours, etc., but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the stirring speed of the slurry process is 50-120 rpm, such as 60rpm, 70rpm, 80rpm, 90rpm, 100rpm or 110rpm, but not limited to the enumerated values, and other unrecited values in the range of the enumerated values are also applicable.
In the present invention, the slurrying comprises grinding the filter cake produced by the filter pressing with a multistage stirrer to form a precipitated silica suspension in a fluid form. The filter cake that obtains after the filter-pressing washing gets into multistage agitator through the belt feeder and stirs in, slowly add a certain amount of n-butanol through the pipeline simultaneously at the uniform velocity, wherein the proportion of adding of n-butanol is 6 ~ 10% of the silica total amount in the agitator, and the paddle in the multistage agitator stirs continuously, pumps the ground paste pump of multistage agitator bottom to agitator upper portion through the delivery pump simultaneously, makes whole stirring more abundant, saves whole pulp time. Slurrying the cake-shaped silicon dioxide into thick slurry with fluidity, wherein the time of the whole slurrying process lasts for 1-2 h, and the stirring speed of the stirrer is 50-120 rpm.
In the invention, the addition of the organic solvent in the slurrying process can obviously weaken the bridging action among hydroxyl groups and weaken the agglomeration phenomenon of the precipitated silicon dioxide. On the other hand, the organic solvent is added, because the surface tension of the organic solvent is smaller, the capillary force is reduced in the drying process, and the pore channels of the precipitated silica can be prevented from collapsing due to overlarge surface tension, so that the pore channels of the precipitated silica can be better preserved, and the oil absorption value is improved.
In the present invention, the drying includes drying the slurried suspension by a pressure sprayer.
As a preferable technical scheme of the invention, the preparation method of the high oil absorption value silicon dioxide comprises the following steps:
the preparation method comprises the following steps:
(1) adding 20-40 wt% of water glass solution into 70-98 ℃ water, diluting the water glass solution until the concentration of water glass in a reaction bottom solution is 5-16 wt%, adding anhydrous sodium sulfate, wherein the concentration of sodium sulfate in the reaction bottom solution is 10.5-20 g/L to obtain a reaction bottom solution, and maintaining the temperature of a system to be 70-98 ℃ in the process of preparing the reaction bottom solution;
(2) adding concentrated sulfuric acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant, wherein the adding time of the concentrated sulfuric acid is 60-100 min;
(3) and after the reaction is finished, adding concentrated sulfuric acid into the reaction medium to adjust the pH value to 3-5 to obtain a silicon dioxide suspension, carrying out solid-liquid separation, washing the obtained silicon dioxide, pulping by using n-butyl alcohol, and drying to obtain the high oil absorption value silicon dioxide.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the invention provides a preparation method of high oil absorption value silicon dioxide, which is used for preparing the high oil absorption value silicon dioxide, improving the added value of products, completely meeting the new requirements of high-end markets of feed-grade silicon dioxide products, being better applied to feed production, rewriting the history that the products are added in the feed production and depend on import, breaking the monopoly of international markets for supplying Chinese feed-grade silicon dioxide products, reducing the use cost of adding domestic feeds, meeting the production requirements of domestic feed industries and improving the overall quality of feed products;
(2) the invention provides a preparation method of high oil absorption value silicon dioxide, and the oil absorption value of the high oil absorption value silicon dioxide prepared by the preparation method is more than 3.0cm3/g，SiO2The content is more than or equal to 96 percent, and the BET specific surface area is 140-210 m2And/g, the apparent particle diameter D50 is 50-150 μm.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
A preparation method of high oil absorption value silicon dioxide comprises the following steps:
(1) adding a water glass solution with the concentration of 40 wt% into water with the temperature of 70 ℃, diluting the water glass solution until the concentration of water glass in a reaction bottom solution is 16 wt%, adding anhydrous sodium sulfate, wherein the concentration of sodium sulfate in the reaction bottom solution is 20g/L to obtain a reaction bottom solution, and maintaining the temperature of a system to be 70 ℃ in the process of preparing the reaction bottom solution;
(2) adding concentrated sulfuric acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant, wherein the adding time of the concentrated sulfuric acid is 100 min;
(3) and after the reaction is finished, adding concentrated sulfuric acid into the reaction medium to adjust the pH value to 4 to obtain a silicon dioxide suspension, carrying out solid-liquid separation, washing the obtained silicon dioxide, pulping by using n-butyl alcohol, and drying to obtain the high oil absorption value silicon dioxide.
The filtration and washing of the precipitated silica suspension produced by the precipitation reaction, with a membrane filter press, resulted in the formation of a filter cake having a silica content of 23% by weight.
And grinding a filter cake generated by filter pressing by using a multistage stirrer to form a precipitated silica suspension in a fluid state.
Filter cakes obtained after filter pressing and washing enter a multistage stirrer through a belt conveyor to be stirred, a certain amount of n-butyl alcohol is slowly added through a pipeline at a constant speed, wherein the adding proportion of the n-butyl alcohol is 10% of the total amount of silicon dioxide in the stirrer, blades in the multistage stirrer are used for continuously stirring, and meanwhile, slurry at the bottom of the multistage stirrer is pumped to the upper part of the stirrer through a feeding pump to carry out circulating grinding. The cake-shaped silica is slurried into a thick slurry with fluidity, the time of the whole slurrying process lasts for 2h, and the stirring speed of the stirrer is 120 rpm.
Example 2
A preparation method of high oil absorption value silicon dioxide comprises the following steps:
(1) adding a 20 wt% water glass solution into 98 ℃ water, diluting the water glass solution until the concentration of water glass in a reaction bottom solution is 5 wt%, adding anhydrous sodium sulfate, wherein the concentration of sodium sulfate in the reaction bottom solution is 10.5g/L to obtain a reaction bottom solution, and maintaining the temperature of a system to be 98 ℃ in the process of preparing the reaction bottom solution;
(2) adding concentrated sulfuric acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant, wherein the adding time of the concentrated sulfuric acid is 60 min;
(3) and after the reaction is finished, adding concentrated sulfuric acid into the reaction medium to adjust the pH value to 3 to obtain a silicon dioxide suspension, carrying out solid-liquid separation, washing the obtained silicon dioxide, pulping by using n-butyl alcohol, and drying to obtain the high oil absorption value silicon dioxide.
The filtration and washing of the precipitated silica suspension produced by the precipitation reaction, with a membrane filter press, resulted in the formation of a filter cake having a silica content of 20% by weight.
And grinding a filter cake generated by filter pressing by using a multistage stirrer to form a precipitated silica suspension in a fluid state.
Filter cakes obtained after filter pressing and washing enter a multistage stirrer through a belt conveyor to be stirred, a certain amount of n-butyl alcohol is slowly added through a pipeline at a constant speed, wherein the adding proportion of the n-butyl alcohol is 6% of the total amount of silicon dioxide in the stirrer, blades in the multistage stirrer are used for continuously stirring, and meanwhile, slurry at the bottom of the multistage stirrer is pumped to the upper part of the stirrer through a feeding pump to carry out circulating grinding. The cake-shaped silica was slurried into a thick slurry with fluidity, the time of the whole slurrying process was 1h, and the stirring speed of the stirrer was 50 rpm.
Example 3
A preparation method of high oil absorption value silicon dioxide comprises the following steps:
(1) adding 30 wt% of water glass solution into 92 ℃ water, diluting the water glass solution until the concentration of water glass in a reaction bottom solution is 13 wt%, adding anhydrous sodium sulfate, wherein the concentration of sodium sulfate in the reaction bottom solution is 14g/L to obtain a reaction bottom solution, and maintaining the temperature of a system to be 92 ℃ in the process of preparing the reaction bottom solution;
(2) adding concentrated sulfuric acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant, wherein the adding time of the concentrated sulfuric acid is 80 min;
(3) and after the reaction is finished, adding concentrated sulfuric acid into the reaction medium to adjust the pH value to 4 to obtain a silicon dioxide suspension, carrying out solid-liquid separation, washing the obtained silicon dioxide, pulping by using n-butyl alcohol, and drying to obtain the high oil absorption value silicon dioxide.
The filtration and washing of the precipitated silica suspension produced by the precipitation reaction, with a membrane filter press, resulted in the formation of a filter cake having a silica content of 22% by weight.
And grinding a filter cake generated by filter pressing by using a multistage stirrer to form a precipitated silica suspension in a fluid state.
Filter cakes obtained after filter pressing and washing enter a multistage stirrer through a belt conveyor to be stirred, a certain amount of n-butyl alcohol is slowly added through a pipeline at a constant speed, wherein the adding proportion of the n-butyl alcohol is 8% of the total amount of silicon dioxide in the stirrer, blades in the multistage stirrer are used for continuously stirring, and meanwhile, slurry at the bottom of the multistage stirrer is pumped to the upper part of the stirrer through a feeding pump to carry out circulating grinding. The cake-shaped silica was slurried into a thick slurry with fluidity, the time of the whole slurrying process lasted for 1.8h, and the stirring speed of the stirrer was 100 rpm.
Example 4
A preparation method of high oil absorption value silicon dioxide comprises the following steps:
(1) adding 25 wt% of water glass solution into 75 ℃ water, diluting the water glass solution until the concentration of water glass in a reaction bottom solution is 8 wt%, adding anhydrous sodium sulfate, wherein the concentration of sodium sulfate in the reaction bottom solution is 12g/L to obtain a reaction bottom solution, and maintaining the temperature of a system at 75 ℃ in the process of preparing the reaction bottom solution;
(2) adding concentrated sulfuric acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant, wherein the adding time of the concentrated sulfuric acid is 90 min;
(3) and after the reaction is finished, adding concentrated sulfuric acid into the reaction medium to adjust the pH value to 3.5 to obtain a silicon dioxide suspension, carrying out solid-liquid separation, washing the obtained silicon dioxide, pulping by using n-butyl alcohol, and drying to obtain the high oil absorption value silicon dioxide.
The filtration and washing of the precipitated silica suspension produced by the precipitation reaction with a membrane filter press resulted in the formation of a filter cake having a silica content of 21% by weight.
And grinding a filter cake generated by filter pressing by using a multistage stirrer to form a precipitated silica suspension in a fluid state.
Filter cakes obtained after filter pressing and washing enter a multistage stirrer through a belt conveyor to be stirred, a certain amount of n-butyl alcohol is slowly added through a pipeline at a constant speed, wherein the adding proportion of the n-butyl alcohol is 9% of the total amount of silicon dioxide in the stirrer, blades in the multistage stirrer are used for continuously stirring, and meanwhile, slurry at the bottom of the multistage stirrer is pumped to the upper part of the stirrer through a feeding pump to carry out circulating grinding. The cake-shaped silica was slurried into a thick slurry with fluidity, the time of the whole slurrying process lasted for 1.5h, and the stirring speed of the stirrer was 80 rpm.
Comparative example 1
This comparative example was conducted under the same conditions as in example 1 except that the slurry was prepared by grinding a filter cake obtained by pressure filtration using a multistage stirrer to give a precipitated silica suspension in a fluid state.
Comparative example 2
This comparative example is the same as example 1 except that n-butanol was replaced with water in the slurry process.
The silicas obtained in examples 1 to 4 and comparative examples 1 and 2 were tested for oil absorption, surface area, silica content and apparent particle size, and the results are shown in Table 1.
The test method comprises the following steps:
SiO of the precipitated silica was determined according to HG/T3062-2Content (c);
the BET specific surface area of the precipitated silica was determined in accordance with GB/T19587-2017;
the particle size of the precipitated silica (D50) was determined according to GB/T32698-2016;
the precipitated silica oil absorption value was determined according to HG/T3072-2008.
TABLE 1
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of high oil absorption value silicon dioxide is characterized by comprising the following steps:
(1) adding a water glass solution into water, diluting the water glass solution, and adding anhydrous sodium sulfate to obtain a reaction bottom solution;
(2) adding acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant;
(3) and after the reaction is finished, adding acid into the reaction medium to adjust the pH value to obtain a silicon dioxide suspension, carrying out solid-liquid separation, and carrying out aftertreatment on the obtained silicon dioxide to obtain the silicon dioxide with the high oil absorption value.
2. The method according to claim 1, wherein the temperature of the water during the addition of the water glass solution in the step (1) is 70 to 98 ℃.
3. The method according to claim 1 or 2, wherein the concentration of the glass solution in the step (1) is 20 to 40 wt%.
4. The method according to any one of claims 1 to 3, wherein the concentration of water glass in the diluted reaction solution in the step (1) is 5 to 16 wt%.
5. The method according to any one of claims 1 to 4, wherein the concentration of sodium sulfate added to the reaction bottom liquid in step (1) is 10.5 to 20 g/L.
6. The method according to any one of claims 1 to 5, wherein the temperature of the system is maintained at 70 to 98 ℃ during the preparation of the reaction base liquid in the step (1).
7. The production method according to any one of claims 1 to 6, wherein the acid of step (2) comprises concentrated sulfuric acid;
preferably, the adding time of the concentrated sulfuric acid is 60-100 min.
8. The production method according to any one of claims 1 to 7, wherein the acid in the step (3) comprises concentrated sulfuric acid;
preferably, the pH value is adjusted to 3-5 in the step (3).
9. The method according to any one of claims 1 to 8, wherein the post-treatment of step (3) comprises washing, slurrying and drying the silica;
preferably, the solvent used for slurrying is an organic solvent;
preferably, the organic solvent comprises n-butanol;
preferably, the adding amount of the organic solvent is 6-10% of the mass of the silicon dioxide;
preferably, the time of the pulping process is 1-2 h;
preferably, the stirring speed of the pulping process is 50-120 rpm.
10. The method of any one of claims 1 to 9, comprising the steps of:
(1) adding 20-40 wt% of water glass solution into 70-98 ℃ water, diluting the water glass solution until the concentration of water glass in a reaction bottom solution is 5-16 wt%, adding anhydrous sodium sulfate, wherein the concentration of sodium sulfate in the reaction bottom solution is 10.5-20 g/L to obtain a reaction bottom solution, and maintaining the temperature of a system to be 70-98 ℃ in the process of preparing the reaction bottom solution;
(2) adding concentrated sulfuric acid and a water glass solution into the reaction bottom liquid obtained in the step (1) to keep the concentration of water glass in the reaction bottom liquid constant, wherein the adding time of the concentrated sulfuric acid is 60-100 min;
(3) and after the reaction is finished, adding concentrated sulfuric acid into the reaction medium to adjust the pH value to 3-5 to obtain a silicon dioxide suspension, carrying out solid-liquid separation, washing the obtained silicon dioxide, pulping by using n-butyl alcohol, and drying to obtain the high oil absorption value silicon dioxide.
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| CN113603127A (en) * | 2021-08-18 | 2021-11-05 | 江苏一夫科技股份有限公司 | Method for concentrated sulfuric acid treatment of calcium chloride wastewater and co-production of chemical gypsum |
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| CN107324346A (en) * | 2017-07-27 | 2017-11-07 | 广州市飞雪材料科技有限公司 | A kind of preparation method of high-specific surface area high oil absorption value silica |
| CN111807395A (en) * | 2018-05-28 | 2020-10-23 | 福建远翔新材料股份有限公司 | Preparation method of low-oil-absorption nano silicon dioxide for high-elasticity silicone rubber |
| CN110562991A (en) * | 2019-10-15 | 2019-12-13 | 龙星化工股份有限公司 | Production method of white carbon black for high-oil-absorption carrier |
| CN111017939A (en) * | 2020-01-14 | 2020-04-17 | 福建省三明正元化工有限公司 | Preparation method of high-dispersion silicon dioxide |
| CN111392739A (en) * | 2020-03-27 | 2020-07-10 | 广州市飞雪材料科技有限公司 | Preparation method and application of high-dispersity thickening type silicon dioxide |
| CN111484025A (en) * | 2020-04-14 | 2020-08-04 | 广州市飞雪材料科技有限公司 | Preparation method of silicon dioxide for low-specific-surface-area high-density thickening toothpaste |
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| CN113603127A (en) * | 2021-08-18 | 2021-11-05 | 江苏一夫科技股份有限公司 | Method for concentrated sulfuric acid treatment of calcium chloride wastewater and co-production of chemical gypsum |
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