CN114132938B - Silica with high oil absorption value and low specific surface area and preparation method thereof - Google Patents
Silica with high oil absorption value and low specific surface area and preparation method thereof Download PDFInfo
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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/12—Surface area
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- 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 provides a silicon dioxide with high oil absorption value and low specific surface area and a preparation method thereof,the method comprises the following steps: s1, adding water into the water glass, dissolving and aging to obtain a water glass solution, and preparing the water glass solution into a sodium silicate solution; preparing a sulfuric acid solution; s2, adding water into the reaction tank, heating, adding a sulfuric acid solution while stirring, then simultaneously dropwise adding a sodium silicate solution and the sulfuric acid solution, and controlling the pH value in the reaction process; s3, adding tetraethoxysilane, then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, stopping dropwise adding when the reaction pH value reaches 8.0-9.0, and stirring and curing; s4, simultaneously dripping a sodium silicate solution and a sulfuric acid solution; s5, dropwise adding a sulfuric acid solution, adjusting the pH value at the end point, and stirring and aging; s6, performing filter pressing and washing on the formed silicon dioxide, and performing spray drying treatment to obtain the silicon dioxide. The oil absorption value of the silicon dioxide is more than or equal to 300g/100g, and the specific surface area of the silicon dioxide is 100-200m2/g。
Description
Technical Field
The invention belongs to the technical field of silicon dioxide, and particularly relates to silicon dioxide with a high oil absorption value and a low specific surface area and a preparation method thereof.
Background
The silicon dioxide has abundant micropores and mesopores, is an amorphous porous structure and can be used as a carrier of a pharmaceutical product. With the cross permeation and fusion development of the nanotechnology in the white carbon black industry, special functional and special nano silicon dioxide 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 coating, a resin compounding agent, a chemical absorbent, a filler for manufacturing, a coating agent for special paper, a silicon dioxide used as a flow aid and an adsorbent in food, and the like. 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. In food, silicon dioxide is used as a flow aid and an adsorbent, and the silicon dioxide has a high oil absorption value and is beneficial to improving the adsorption performance.
At present, the specific surface area of silicon dioxide is not limited in relevant standards, the higher the specific surface area of silicon dioxide is, the more abundant the pore structure is, and the silicon dioxide is agglomerated with the lapse of time, so that the product viscosity is higher and higher, and the normal use of the product is affected when the viscosity is too high, so that the specific surface area of silicon dioxide needs to be reduced, the specific surface area of silicon dioxide is low, the agglomeration is reduced, and the flow aid capability is improved.
At present, silicon dioxide is mainly prepared by a gas phase method and a precipitation method, the gas phase method is high in oil absorption value and high in cost, and the precipitation method is low in price and suitable for being used in large quantities. The precipitation method is divided into a common precipitation method and a gel method, and the silica prepared by the common precipitation method has low oil absorption value (less than 250g/100g (linseed oil)); the silica prepared by the gel method has high oil absorption value (which is equal to 300g/100g (linseed oil)), but has large specific surface area (500-700 m)2In g), too large a specific surface area makes the sample agglomerate severely and cannot be used in food.
It is therefore desirable to develop a silica product having a high oil absorption value, while having a low specific surface area.
Disclosure of Invention
The invention aims to provide silicon dioxide with high oil absorption value and low specific surface area and a preparation method thereof, wherein three-stage reaction is adopted, the same dropping is carried out firstly under the acidic condition, then the same dropping is carried out, the reaction pH value is gradually increased from 3.0-4.5 to 8-9, the same dropping is carried out under the alkaline condition, the oil absorption value of the product is high, and the specific surface area is low; the silica prepared by the preparation method has an oil absorption value of more than or equal to 300g/100g and a specific surface area of 100-200m2/g。
The first purpose of the invention is to provide a preparation method of silica with high oil absorption value and low specific surface area, which comprises the following steps:
s1, adding water into the water glass, diluting, dissolving and aging for 5-8 h to obtain a water glass solution, and adding water into the aged water glass solution to dilute and prepare a sodium silicate solution; preparing a sulfuric acid solution;
s2, adding water into the reaction tank, heating to 80-95 ℃, dropwise adding a sulfuric acid solution while stirring until the pH value is 3.0-4.5, and dropwise adding a sodium silicate solution 0.5-2.0 m at the same time3And a sulfuric acid solution, wherein the pH value in the reaction process is controlled to be 3.0-4.5;
s3, adding tetraethoxysilane, then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, stopping dropwise adding when the reaction pH value reaches 8.0-9.0, and stirring and curing for 30-40 min;
s4, and simultaneously dropwise adding 6-10 m of sodium silicate solution3And a sulfuric acid solution;
s5, dropwise adding a sulfuric acid solution, adjusting the pH value of the end point to 4.0-5.0, and stirring and aging for 25-35 min;
and S6, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide with high oil absorption value and low specific surface area.
Preferably, the modulus of the water glass is 3-3.5.
Preferably, the concentration of the sodium silicate solution is 0.5-2.5 mol/L.
Preferably, the concentration of the sulfuric acid solution is 3-6 mol/L.
Preferably, the addition amount of the tetraethoxysilane is 13L-65L, and the mass percentage concentration of the tetraethoxysilane is 1-5%.
Preferably, in the step S2, the adding amount of water is 6-10 m3。
Preferably, in the step S2, the dropping speed of the sodium silicate solution is 10-15 m3/h。
Preferably, in the step S3, the dropping speed of the sodium silicate solution is 10-15 m3The dropping speed of the sulfuric acid solution is 1.0-3.0 m3/h。
Preferably, in the step S4, the dropping speed of the sodium silicate solution is 10-15 m3The dropping speed of the sulfuric acid solution is 1.0-3.0 m3/h。
The second purpose of the invention is to provide the high oil absorption value low specific surface area silicon dioxide prepared by the preparation method.
The preparation method of the silicon dioxide with high oil absorption value and low specific surface area has the following reaction principle:
the precipitated hydrated silica is similar to amorphous spherical particles of carbon black, and the individual particles are in surface contact with each other to form branched chain-like bonds, the specific surface area of the silica depends on the particle diameter and the stacking manner of the particles, and the oil absorption value of the silica depends on the complex structure of large clusters and the connection space between the clusters.
The method adopts three-stage reaction, in the first stage, water is used as a base solution, a sodium silicate solution and a sulfuric acid solution are simultaneously dripped under the high-temperature condition of 80-95 ℃, and the pH value in the reaction process is controlled to be 3.0-4.5, because the neutralization rate of the sodium silicate is high under the condition of pH value of 3.0-4.5, a large amount of particles with small particle size can be rapidly generated, and a raw material is provided for forming a large cluster with a complex structure in the second stage; meanwhile, the using amount of the sodium silicate solution in the first stage is controlled, so that the specific surface area can be reduced. In the second stage, adding tetraethoxysilane, and then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution to gradually increase the pH value of the system to 8.0-9.0, wherein the tetraethoxysilane can enable particles obtained in the first stage to quickly form a large number of silicon dioxide micelles which are complex in structure, proper in internal pore diameter and connected among clusters; and in the third stage, under an alkaline condition, the sulfuric acid and the sodium silicate solution are titrated simultaneously, the silica micelle continues to grow, the oil absorption value is obviously increased, and meanwhile, some fine holes are blocked, so that the specific surface area is reduced.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a silicon dioxide with high oil absorption value and low specific surface area and a preparation method thereof, wherein the silicon dioxide product prepared by the preparation method has high oil absorption value and low specific surface area; the silica prepared by the preparation method has an oil absorption value of more than or equal to 300g/100g and a specific surface area of 100-200m2/g。
The invention provides silicon dioxide with high oil absorption value and low specific surface area and a preparation method thereof.
Detailed Description
The present invention will be described in further detail with reference to the following examples. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Example 1 high oil absorption Low specific surface area silica of the invention and preparation thereof
S1, adding water into water glass with the modulus of 3 to dilute, dissolve and age for 6 hours to obtain water glass solution, adding water into the aged water glass solution to dilute and prepare sodium silicate solution with the concentration of 2.0mol/L for later use; preparing a sulfuric acid solution with the concentration of 5mol/L for later use;
s2, adding 8m into the reaction tank3Heating water to 90 deg.C, adding dropwise sulfuric acid solution while stirring to pH 4.0, and adding dropwise sodium silicate solution 1.0m3And sulfuric acid solution, the dropping speed of the sodium silicate solution is 12m3H, controlling the pH value in the reaction process to be 4.0;
s3, adding 33.48L of tetraethoxysilane with the mass percentage concentration of 3%, and then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, wherein the dropwise adding speed of the sodium silicate solution is 12m3The dropping speed of the sulfuric acid solution is 1.0m3Stopping dripping when the pH value of the reaction reaches 8.0, and stirring and curing for 30 min;
s4, and simultaneously dropwise adding 8m of sodium silicate solution3And sulfuric acid solution, wherein the dropping speed of the sodium silicate solution is controlled to be 12m3The dropping speed of the sulfuric acid solution is 2.0m3/h；
S5, dropwise adding a sulfuric acid solution, adjusting the end point pH value to 4.0, and stirring and aging for 25 min;
and S6, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide with high oil absorption value and low specific surface area.
Example 2 high oil absorption Low surface area silica of the invention and preparation thereof
S1, adding water into the water glass with the modulus of 3.2 to dilute, dissolve and age for 8 hours to obtain a water glass solution, adding 6m of water into the aged water glass solution3Diluting to prepare a sodium silicate solution with the concentration of 1.5mol/L for later use; preparing a sulfuric acid solution with the concentration of 6mol/L for later use;
s2, adding water into the reaction tank, heating to 90 ℃, and dropwise adding sulfuric acid while stirringThe solution is adjusted to pH 4.0 and sodium silicate solution is added dropwise at the same time to a concentration of 1.5m3And sulfuric acid solution, the dropping speed of the sodium silicate solution is 13m3H, controlling the pH value in the reaction process to be 4.0;
s3, adding 22.32L of tetraethoxysilane with the mass percentage concentration of 2%, and then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, wherein the dropwise adding speed of the sodium silicate solution is 13m3The dropping speed of the sulfuric acid solution is 1.5m3Stopping dripping when the reaction pH value reaches 8.0, and stirring and curing for 35 min;
s4, and simultaneously dropwise adding 10m of sodium silicate solution3And sulfuric acid solution, wherein the dropping speed of the sodium silicate solution is controlled to be 13m3The dropping speed of the sulfuric acid solution is 3.0m3/h；
S5, dropwise adding a sulfuric acid solution, adjusting the end point pH value to 5.0, and stirring and aging for 30 min;
and S6, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide with high oil absorption value and low specific surface area.
Example 3 high oil absorption Low specific surface area silica of the invention and preparation thereof
S1, adding water into water glass with the modulus of 3.5 to dilute, dissolve and age for 6 hours to obtain water glass solution, adding water into the aged water glass solution to dilute and prepare sodium silicate solution with the concentration of 2.5mol/L for later use; preparing a sulfuric acid solution with the concentration of 4mol/L for later use;
s2, adding 10m into the reaction tank3Heating water to 95 deg.C, adding dropwise sulfuric acid solution while stirring to pH 4.0, and adding dropwise sodium silicate solution 2.0m3And sulfuric acid solution, the dropping speed of the sodium silicate solution is 11m3H, controlling the pH value in the reaction process to be 3.0;
s3, adding 44.64L of tetraethoxysilane with the mass percentage concentration of 4%, and then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, wherein the dropwise adding speed of the sodium silicate solution is 11m3The dropping speed of the sulfuric acid solution is 1.0m3Stopping dripping when the pH value of the reaction reaches 9.0, and stirring and curing for 40 min;
s4, simultaneous droppingAdding sodium silicate solution 9m3And sulfuric acid solution, wherein the dropping speed of the sodium silicate solution is controlled to be 11m3The dropping speed of the sulfuric acid solution is 2.0m3/h；
S5, dropwise adding a sulfuric acid solution, adjusting the end point pH value to 5.0, and stirring and aging for 25 min;
s6, carrying out filter pressing and washing treatment on the formed silicon dioxide, and carrying out spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide with high oil absorption value and low specific surface area.
Example 4 high oil absorption Low specific surface area silica of the invention and preparation thereof
S1, adding water into water glass with the modulus of 3.2 to dilute, dissolve and age for 7 hours to obtain a water glass solution, and adding water into the aged water glass solution to dilute and prepare a sodium silicate solution with the concentration of 0.5mol/L for later use; preparing a sulfuric acid solution with the concentration of 3mol/L for later use;
s2, adding 8m into the reaction tank3Heating water to 80 deg.C, adding dropwise sulfuric acid solution while stirring to pH 3.5, and adding dropwise sodium silicate solution 0.5m3And sulfuric acid solution, the dropping speed of the sodium silicate solution is 14m3H, controlling the pH value in the reaction process to be 4.5;
s3, adding 55.8L of tetraethoxysilane with the mass percentage concentration of 5%, and then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, wherein the dropwise adding speed of the sodium silicate solution is 14m3The dropping speed of the sulfuric acid solution is 1.0m3Stopping dripping when the reaction pH value reaches 8.5, and stirring and curing for 40 min;
s4, and simultaneously dropwise adding 6m of sodium silicate solution3And sulfuric acid solution, wherein the dropping speed of the sodium silicate solution is controlled to be 14m3The dropping speed of the sulfuric acid solution is 3.0m3/h；
S5, dropwise adding a sulfuric acid solution, adjusting the end point pH value to 5.0, and stirring and aging for 25 min;
and S6, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide with high oil absorption value and low specific surface area.
Comparative example 1
The comparative example differs from example 1 only in that: in step S3, ethyl orthosilicate is not added.
Comparative example 2
The comparative example differs from example 1 only in that: the amount of ethyl orthosilicate added in step S3 was increased to 5%.
Comparative example 3
S1, adding water into water glass with the modulus of 3 to dilute, dissolve and age for 6 hours to obtain water glass solution, adding water into the aged water glass solution to dilute and prepare sodium silicate solution with the concentration of 2.0mol/L for later use; preparing a sulfuric acid solution with the concentration of 5mol/L for later use;
s2, adding 8m into the reaction tank3Heating water to 90 ℃, adding 33.48L of tetraethoxysilane with the mass percentage concentration of 3 percent, and then simultaneously dripping sodium silicate solution and sulfuric acid solution at the dripping speed of 12m3The dropping speed of the sulfuric acid solution is 1.0m3Stopping dripping when the pH value of the reaction reaches 8.0, and stirring and curing for 30 min;
s3, and simultaneously dropwise adding 8m of sodium silicate solution3And sulfuric acid solution, wherein the dropping speed of the sodium silicate solution is controlled to be 12m3The dropping speed of the sulfuric acid solution is 2.0m3/h；
S4, dropwise adding a sulfuric acid solution, adjusting the end point pH value to 4.0, and stirring and aging for 25 min;
and S5, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide.
The comparative example differs from example 1 in that: the operation of simultaneously adding the sodium silicate solution and the sulfuric acid solution in the original step S2 is omitted.
Comparative example 4
S1, adding water to the water glass with the modulus of 3 to dilute, dissolve and age for 6 hours to obtain a water glass solution, adding water to dilute the aged water glass solution to prepare a sodium silicate solution with the concentration of 2.0mol/L for later use; preparing a sulfuric acid solution with the concentration of 5mol/L for later use;
s2, adding 8m into the reaction tank3Heating water to 90 deg.c,dropwise adding sulfuric acid solution under stirring until pH is 4.0, and dropwise adding sodium silicate solution 1.0m3And sulfuric acid solution, the dropping speed of the sodium silicate solution is 12m3H, controlling the pH value in the reaction process to be 4.0;
s3, adding 33.48L of tetraethoxysilane with the mass percentage concentration of 3 percent, and simultaneously dropwise adding 8m of sodium silicate solution3And sulfuric acid solution, wherein the dropping speed of the sodium silicate solution is controlled to be 12m3The dropping speed of the sulfuric acid solution is 1.0m3/h；
S4, dropwise adding a sulfuric acid solution, adjusting the end point pH value to 4.0, and stirring and aging for 25 min;
and S5, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide.
The comparative example differs from example 1 in that: the operation of simultaneously dripping the sodium silicate solution and the sulfuric acid solution and the subsequent aging treatment in the prior step S3 are omitted.
Comparative example 5
S1, adding water into water glass with the modulus of 3 to dilute, dissolve and age for 6 hours to obtain water glass solution, adding water into the aged water glass solution to dilute and prepare sodium silicate solution with the concentration of 2.0mol/L for later use; preparing a sulfuric acid solution with the concentration of 5mol/L for later use;
s2, adding 8m into the reaction tank3Heating water to 90 deg.C, adding dropwise sulfuric acid solution while stirring to pH 4.0, and adding dropwise sodium silicate solution 1.0m3And sulfuric acid solution, the dropping speed of the sodium silicate solution is 12m3H, controlling the pH value in the reaction process to be 4.0;
s3, adding 33.48L of tetraethoxysilane with the mass percentage concentration of 3%, and then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, wherein the dropwise adding speed of the sodium silicate solution is 12m3The dropping speed of the sulfuric acid solution is 1.0m3Stopping dripping when the pH value of the reaction reaches 8.0, and stirring and curing for 30 min;
s4, dropwise adding a sulfuric acid solution, adjusting the end point pH value to 4.0, and stirring and aging for 25 min;
and S5, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide.
The comparative example differs from example 1 in that: the original step S4 is omitted.
Comparative example 6
The comparative example differs from example 1 only in that: the dropping amount of the sodium silicate solution in the step S2 was increased to 3m3。
Comparative example 7
The comparative example differs from example 1 only in that: the dropping amount of the sodium silicate solution in the step S2 was reduced to 0.3m3。
Experimental example-Performance testing of silica
The silica prepared in examples 1 to 4 and comparative examples 1 to 5 were subjected to tests of oil absorption value, specific surface area and apparent particle diameter (D50), and the results of the tests are shown in table 1.
The test method comprises the following steps:
determining the oil absorption value of the precipitated silica according to HG/T3072-2008;
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.
TABLE 1 Performance test results for silica products
| Group of | Oil absorption number (g/100g) | Specific surface area (m)2/g) | Apparent particle diameter D50(μm) |
| Example 1 | 351 | 140 | 15 |
| Example 2 | 364 | 132 | 13 |
| Example 3 | 384 | 183 | 18 |
| Example 4 | 320 | 155 | 20 |
| Comparative example 1 | 347 | 85 | 5 |
| Comparative example 2 | 345 | 230 | 25 |
| Comparative example 3 | 285 | 303 | 6 |
| Comparative example 4 | 250 | 511 | 10 |
| Comparative example 5 | 302 | 353 | 8 |
| Comparative example 6 | 321 | 264 | 24 |
| Comparative example 7 | 230 | 221 | 16 |
As can be seen from table 1, it is,
(1) in the embodiments 1-4 of the invention, the oil absorption value of the silicon dioxide is above 320g/100g, and the minimum specific surface area reaches 132m2The method has the advantages that the oil absorption value of the silicon dioxide prepared by the preparation method is high (more than or equal to 300g/100g), and the specific surface area is small (100-2The method of the invention can effectively improve the oil absorption value of the silicon dioxide and reduce the specific surface area; comparative examples 1 to 7, in which the reaction steps were reduced, the amount of ethyl orthosilicate added or the amount of sodium silicate solution used was changed, all had adverse effects on the oil absorption value, specific surface area and apparent particle size of the silica product.
(2) Specifically, compared with example 1, comparative example 1 and comparative example 2 have no influence or little influence on the specific surface area and the apparent particle size of the silica product by adding the ethyl orthosilicate; comparative example 3 omitted the operation of simultaneously adding sodium silicate solution and sulfuric acid solution in the first-stage conventional step S2 of the present invention, comparative example 4 omitted the operation of simultaneously adding sodium silicate solution and sulfuric acid solution and the subsequent aging treatment in the second-stage conventional step S3 of the present invention, comparative example 5 omitted the third-stage conventional step S4 of the present invention, and comparative example 6 and comparative example 7 changed the amount of sodium silicate solution added in the first-stage reaction step S2 of the present invention, and the resulting silica product was reduced in oil absorption property and increased in specific surface area.
In conclusion, the three-stage reaction method can greatly improve the oil absorption value of the silicon dioxide and reduce the specific surface area of the silicon dioxide, and in addition, the steps of the three-stage reaction and the addition amount of the ethyl orthosilicate have influence on the apparent particle size of the silicon dioxide.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
1. A preparation method of silica with high oil absorption value and low specific surface area is characterized by comprising the following steps:
s1, adding water into the water glass, diluting, dissolving and aging for 5-8 h to obtain a water glass solution, and adding water into the aged water glass solution to dilute and prepare a sodium silicate solution; preparing a sulfuric acid solution;
s2, adding water into the reaction tank, heating to 80-95 ℃, dropwise adding a sulfuric acid solution while stirring until the pH value is 3.0-4.5, and dropwise adding a sodium silicate solution 0.5-2.0 m at the same time3And a sulfuric acid solution, wherein the pH value in the reaction process is controlled to be 3.0-4.5;
s3, adding tetraethoxysilane, then simultaneously dropwise adding a sodium silicate solution and a sulfuric acid solution, stopping dropwise adding when the reaction pH value reaches 8.0-9.0, and stirring and curing for 30-40 min;
s4, and simultaneously dropwise adding 6-10 m of sodium silicate solution3And a sulfuric acid solution;
s5, dropwise adding a sulfuric acid solution, adjusting the pH value of the end point to 4.0-5.0, and stirring and aging for 25-35 min;
s6, performing filter pressing and washing treatment on the formed silicon dioxide, and performing spray drying treatment on the silicon dioxide slurry to obtain the silicon dioxide with high oil absorption value and low specific surface area;
the addition amount of the tetraethoxysilane is 13L-65L, and the mass percentage concentration of the tetraethoxysilane is 2-4%.
2. The method according to claim 1, wherein the water glass has a modulus of 3 to 3.5.
3. The preparation method according to claim 1, wherein the concentration of the sodium silicate solution is 0.5-2.5 mol/L.
4. The method according to claim 1, wherein the concentration of the sulfuric acid solution is 3 to 6 mol/L.
5. The method according to claim 1, wherein in step S2, the amount of water added is 6-10 m3。
6. The preparation method according to claim 1, wherein in the step S2, the dropping speed of the sodium silicate solution is 10-15 m3/h。
7. The preparation method according to claim 1, wherein in the step S3, the dropping speed of the sodium silicate solution is 10-15 m3The dropping speed of the sulfuric acid solution is 1.0-3.0 m3/h。
8. The preparation method according to claim 1, wherein in the step S4, the dropping speed of the sodium silicate solution is 10-15 m3The dropping speed of the sulfuric acid solution is 1.0-3.0 m3/h。
9. Silica having a high oil absorption value and a low specific surface area, which is obtained by the method according to any one of claims 1 to 8.
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| DE4427137B4 (en) * | 1993-10-07 | 2007-08-23 | Degussa Gmbh | precipitated silica |
| IN188702B (en) * | 1995-06-01 | 2002-10-26 | Degussa | |
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| CN102548898A (en) * | 2009-09-03 | 2012-07-04 | 罗地亚管理公司 | Novel method for preparing precipitated silica |
| CN108190900A (en) * | 2018-03-29 | 2018-06-22 | 广州市飞雪材料科技有限公司 | A kind of low specific surface area high oil absorption value friction type silica and preparation method thereof |
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