CN115521502A - Modified white carbon black micron aggregate and preparation method and application thereof - Google Patents

Modified white carbon black micron aggregate and preparation method and application thereof Download PDF

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CN115521502A
CN115521502A CN202110715969.7A CN202110715969A CN115521502A CN 115521502 A CN115521502 A CN 115521502A CN 202110715969 A CN202110715969 A CN 202110715969A CN 115521502 A CN115521502 A CN 115521502A
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solution
aggregate
fumed silica
carbon black
white carbon
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CN115521502B (en
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周丽丽
闫丽
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Jinan Unatech New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C08K7/26—Silicon- containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00—Compositions of unspecified rubbers

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Abstract

The modified white carbon black micron aggregate is formed by aggregating sheet structures, and the sheet structures are fumed white carbon black with the surface being coated by inorganic silicon. The hydrophobicity, tap density and dispersibility of the aggregate are higher than those of fumed silica, so that the aggregate has a good low-thickening characteristic, the filling amount of the fumed silica in silicone rubber is effectively increased, the viscosity of the fumed silica and rubber is reduced, and the mechanical property and the processability of the rubber reinforced by the fumed silica are effectively improved.

Description

Modified white carbon black micron aggregate and preparation method and application thereof
Technical Field
The invention relates to the field of inorganic nano new materials, in particular to a modified white carbon black micron aggregate and a preparation method and application thereof.
Background
White carbon black, also called silica, is a white, nontoxic powder developed from non-metallic quartz sand, and is an important inorganic fine chemical product. White carbon black according to the production methodThe method can be divided into precipitation method white carbon black and gas phase method white carbon black. Wherein, the fumed silica is white amorphous flocculent nanometer silica powder (particle size less than 100 nm) generated by hydrolyzing silicon halide at high temperature, and has large specific surface area (generally more than 100 m) 2 And/g) has excellent stability, reinforcing property, thickening property and thixotropy, and is a reinforcing agent and additive which are indispensable in the industries of rubber, coating, plastics, papermaking, medicine, printing ink and the like.
The main use of white carbon black is as cross-linking reinforcing agent in silicon rubber, the main chain of silicon rubber is composed of inorganic Si-O chain, and the side group is hydrocarbon organic group, so it has excellent low-temperature performance and heat-resisting and ageing-resisting performance. However, because the intermolecular force is weaker, crystallization cannot occur under the stress condition, so that the mechanical strength is extremely weak, the rubber which is not filled with the reinforcing filler has almost no use value, after the white carbon black is added into the silicone rubber, the tensile strength, the elongation, the bonding strength, the hardness, the tearing strength and the mechanical property of the silicone rubber can be limited and improved, and the physical and mechanical properties of the silicone rubber using the fumed white carbon black as the reinforcing filler are far better than those of the silicone rubber using the precipitated white carbon black or other fillers.
However, the surface of fumed silica has active silicon hydroxyl groups, and carboxylic acid bonds are formed in the processes of water absorption and preparation, so that acid areas appear on the surface of fumed silica, the fumed silica is difficult to infiltrate and disperse in an organic phase and cannot be well compatible and dispersed with polymers in a rubber vulcanization system, the vulcanization efficiency and the reinforcement performance are reduced, and the fumed silica cannot be used in certain fields with special requirements.
Meanwhile, the tap density of the fumed silica is low, dust is easy to generate during operation, the fumed silica is not easy to add, and the viscosity of the system is easy to increase when the fumed silica is added into silicon rubber, so that the addition amount of the fumed silica in the silicon rubber is low.
Although the compatibility of the filler and the rubber can be properly improved by carrying out surface modification on the fumed silica, and the addition amount of the fumed silica in the silicone rubber is increased by a small amount, the problems of how to increase the addition amount and reduce the viscosity of a system cannot be fundamentally solved.
The surface of the fumed silica is modified, so that the dispersibility and compatibility of the fumed silica in an organic phase can be improved, the application field of the product is widened, and the additional value of the fumed silica is improved.
The surface modification of the fumed silica mainly comprises inorganic substance modification and organic substance modification, wherein the inorganic substance modification is performed by TiO 2 Coated SiO 2 The modified fumed silica almost inherits all the superior performances of the common fumed silica, and has special hydrophobicity, so that the application field of the modified fumed silica is wider.
However, the conventional gas phase method for modifying the white carbon black is complex in steps, high in processing precision requirement and high in difficulty.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a modified white carbon black micron aggregate, which is formed by aggregating sheet-shaped structures, wherein the sheet-shaped structures are fumed silica with the surface coated by inorganic silicon.
The particle size of the aggregate is 1-6 μm, and the length of the sheet structure is 20-40nm.
Preferably, the aggregates have a particle size of 1 μm to 5 μm, for example 2 μm, 3 μm, 4 μm.
Preferably, the length of the sheet-like structure is from 25nm to 35nm, e.g. 20nm, 25nm, 35nm, 40nm.
Preferably, the hydrated particle size of the aggregates is from 2 μm to 4 μm.
Preferably, the aggregates are inorganic microaggregates.
Preferably, the aggregates are of powder structure.
According to the present invention, the aggregate has a transmissive electron micromirror pattern as described in fig. 1, fig. 2, fig. 4, or fig. 5.
According to the invention, the aggregates have a hydrated particle size profile as depicted in fig. 3 or fig. 6.
The invention also provides a preparation method of the white carbon black micron aggregate, which comprises the following steps:
s1, putting fumed silica into a reaction kettle, adding a silane ethanol solution, stirring until the fumed silica is completely dispersed, and heating the dispersion to 70-90 ℃, such as 75-85 ℃, such as 80 ℃.
And S2, adjusting the pH value of the solution to be acidic, and adding a sodium silicate aqueous solution to react to obtain an aggregate.
According to the invention, the mass concentration of fumed silica in the dispersion is 10-50mg/mL, preferably 20-40mg/mL, preferably 25-35mg/mL, such as 15mg/mL, 25mg/mL, 40mg/mL, 50mg/mL.
Preferably, the fumed silica is fumed hydrophobic silica.
According to the invention, the silanol solution is a solution obtained by dissolving silane in an alcohol solvent.
Preferably, the silane is one, a combination of two or more of hexamethyldisiloxane, hexamethyldisilazane, heptamethyldisilazane, octamethylcyclotetrasilazane, tetramethyldivinyldisiloxane, tetramethyldivinyldisilazane, diethoxymethylvinylsilane, dimethoxymethylphenylsilane, diethoxyphenylsilane, phenyltrimethoxysilane and phenyltriethoxysilane.
Preferably, the alcohol solvent is a C2-C5 alcohol, preferably ethanol, propanol, isopropanol, butanol, isobutanol or pentanol, for example ethanol.
According to the invention, the steps between S1 and S2 further comprise the step of adjusting the pH value of the dispersion to be alkaline and stable.
Preferably, the alkaline pH is 8 or more, preferably 9 or more, for example 9.5.
Preferably, the pH of the dispersion is adjusted using NaOH, for example, by adding NaOH solution to the dispersion to adjust the pH to 9.5.
Preferably, the concentration of the NaOH solution is 1M.
Preferably, after the pH value of the dispersion is adjusted to be alkaline and stabilized to be 9.5, the pH value of the dispersion is stirred for 0.5-1h, and the pH value is stabilized to be 9.5 during the stirring.
According to the invention, said step S2 is carried out under stirring conditions at a temperature of 80 ℃.
According to the invention, the adjustment of the pH value of the solution to acidity in step S2 is carried out using an acidic alcohol solution, which is a solution obtained by dissolving an inorganic acid in an alcohol.
Preferably, the inorganic acid is sulfuric acid or nitric acid.
Preferably, the alcohol is a C2-C5 alcohol, preferably ethanol, propanol, isopropanol, butanol, isobutanol or pentanol, for example ethanol.
For example, the acidic alcohol solution is a sulfuric acid ethanol solution, and preferably, the mass concentration of sulfuric acid in the sulfuric acid ethanol solution is 1%.
Preferably, the concentration of the sodium silicate aqueous solution is 0.15M.
According to the invention, the volume ratio of the sodium silicate aqueous solution to the sulfuric acid ethanol solution is 1.
Preferably, the adding amount of the sodium silicate solution and the sulfuric acid ethanol solution is 50-100mL/kg.
According to the invention, the reaction time after the sodium silicate aqueous solution is added in step S2 is 4-8h.
The application of the white carbon black micron aggregate is used as a rubber additive.
Advantageous effects
By simple one-step operation, under the action of a silane modifier, an inorganic silicon growth method is utilized, so that inorganic silicon grows on the surface of fumed silica and fumed silica is wrapped in a sealing manner, meanwhile, the inorganic silicon is gathered under the mechanical action, the wrapped fumed silica forms a flaky aggregate structure, the inorganic micron aggregate which is changed from a random unstable aggregation state into a stable inorganic micron aggregate is realized, the hydrophobicity, the tap density and the dispersibility of the aggregate are all higher than those of the fumed silica, the aggregate has good low-thickening characteristic, the filling amount of the fumed silica in silicone rubber is effectively increased, the viscosity of the silicone rubber and rubber in a mixed rubber is reduced, and the mechanical property and the processing property of the rubber reinforced by the fumed silica are effectively improved.
Drawings
FIG. 1 shows a transmission electron microscope photograph of stable white carbon black micro-aggregates obtained in example 1 of the present invention under a 20nm scale;
FIG. 2 shows a transmission electron microscope photograph of the stable white carbon black micro aggregate obtained in example 1 of the present invention under a 50nm scale;
FIG. 3 shows the distribution of hydrated particle size of the stable white carbon black micro-aggregates obtained in example 1 of the present invention;
FIG. 4 shows a transmission electron microscope photograph of the stable white carbon black micro-aggregates obtained in example 2 of the present invention on a 20nm scale;
FIG. 5 shows a transmission electron microscope photograph of the stable white carbon black micro-aggregates obtained in example 2 of the present invention on a 100nm scale;
fig. 6 shows the hydrated particle size distribution of the stable white carbon black micro-aggregates obtained in example 2 of the present invention.
Detailed Description
The materials of the present invention, methods of making the same, and uses thereof, are described in further detail below with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the techniques realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
1kg of fumed silica is placed in a reaction kettle, 60L of a silanoethanol solution (hexamethyldisilazane, tetramethyldivinyldisiloxane and ethanol in a ratio of 4. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5; continuously stirring until the pH value is stable, adding 75mL of 1% sulfuric acid ethanol solution into the reaction kettle under the stirring condition of 80 ℃, stirring and dispersing, preparing 75mL of 0.15M sodium silicate aqueous solution after completely dispersing, adding into the reaction kettle, and continuously stirring and reacting for 6 hours at 80 ℃; finally, a powdery product is obtained.
Referring to fig. 1 and fig. 2, the aggregates prepared in this example have good dispersibility under SEM, the lamellar structure is clearly visible, and the length of the lamellar structure is 20-40nm.
Referring to fig. 3, the aggregates prepared in this example have good dispersibility in the solvent and a uniform particle size distribution.
Example 2
1kg of fumed silica is placed in a reaction kettle, 60L of a silanoethanol solution (hexamethyldisiloxane, tetramethyldivinyldisilazane and ethanol in a ratio of 4. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5; continuously stirring until the pH value is stable, adding 75mL of 1% sulfuric acid ethanol solution into the reaction kettle under the stirring condition of 80 ℃, stirring and dispersing, preparing 75mL of 0.15M sodium silicate aqueous solution, adding into the reaction kettle, and continuously stirring and reacting for 6 hours at 80 ℃; finally obtaining a powdery product.
Referring to fig. 4 and 5, the aggregates prepared in this example have good dispersibility under SEM, the lamellar structure is clearly visible, and the length of the lamellar structure is 20-40nm.
Referring to fig. 6, the aggregates prepared in this example have good dispersibility in the solvent and a relatively uniform particle size distribution.
Example 3
1kg of fumed silica is placed in a reaction kettle, 100L of a silane ethanol solution (heptamethyldisilazane, diethoxymethylvinylsilane and ethanol in a ratio of 3. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5, stirring until the pH value is stable, adding 50mL of 1% sulfuric acid ethanol solution into the reaction kettle under the stirring condition of 80 ℃, stirring and dispersing, preparing 50mL of 0.15M sodium silicate aqueous solution, adding into the reaction kettle after complete dispersion, and continuing stirring and reacting for 4 hours at 80 ℃; finally obtaining a powdery product.
Example 4
1kg of fumed silica is placed in a reaction kettle, 100L of a silanolate solution (octamethylcyclotetrasilazane, dimethoxymethylphenylsilane, and ethanol in a ratio of 2. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5, stirring until the pH value is stable, adding 50mL of 1% sulfuric acid ethanol solution into the reaction kettle under the condition of stirring at 80 ℃, stirring and dispersing, preparing 50mL of 0.15M sodium silicate aqueous solution, adding into the reaction kettle after complete dispersion, and continuing stirring and reacting for 4 hours at 80 ℃; finally obtaining a powdery product.
Example 5
1kg of fumed silica is placed in a reaction kettle, 100L of a silanethanol solution (octamethylcyclotetrasilazane, diethoxyphenylsilane, and ethanol, in a ratio of 2. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5, stirring until the pH value is stable, adding 50mL of 1% sulfuric acid ethanol solution into the reaction kettle under the stirring condition of 80 ℃, stirring and dispersing, preparing 50mL of 0.15M sodium silicate aqueous solution, adding into the reaction kettle after complete dispersion, and continuing stirring and reacting for 4 hours at 80 ℃; finally obtaining a powdery product.
Example 6
1kg of fumed silica is placed in a reaction kettle, 20L of a silanoethanol solution (octamethylcyclotetrasilazane, phenyltrimethoxysilane and ethanol in a ratio of 2. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5; after the pH value is stable, the reaction kettle is continuously stirred at the temperature of 80 ℃; preparing 100mL of 1% sulfuric acid ethanol solution, adding the solution into a reaction kettle, stirring and dispersing, preparing 100mL of 0.15M sodium silicate aqueous solution, adding the aqueous solution into the reaction kettle, and continuously stirring and reacting for 8 hours at 80 ℃; finally obtaining a powdery product.
Example 7
1kg of fumed silica is placed in a reaction kettle, 20L of a silane ethanol solution (octamethylcyclotetrasilazane, phenyltriethoxysilane and ethanol in a ratio of 2. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5, stirring until the pH value is stable, adding 100mL of 1% sulfuric acid ethanol solution into the reaction kettle under the condition of stirring at 80 ℃, stirring and dispersing, preparing 100mL of 0.15M sodium silicate aqueous solution, adding into the reaction kettle after complete dispersion, and continuing stirring and reacting for 8 hours at 80 ℃; finally obtaining a powdery product.
Example 8
1kg of fumed silica is placed in a reaction kettle, 60L of a silanethanol solution (hexamethyldisilazane, tetramethyldivinyldisiloxane, diethoxyphenylsilane, and ethanol, in a ratio of 2. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5, stirring until the pH value is stable, and stirring at 80 ℃; adding 75mL of 1% sulfuric acid ethanol solution into the reaction kettle, stirring and dispersing, preparing 75mL of 0.15M sodium silicate aqueous solution after completely dispersing, adding into the reaction kettle, and continuing stirring and reacting for 6h at 80 ℃; finally, a powdery product is obtained.
Example 9
1kg of fumed silica is placed in a reaction kettle, 60L of a silanoethanol solution (hexamethyldisilazane, tetramethyldivinyldisiloxane, phenyltrimethoxysilane and ethanol in a ratio of 2. When the temperature of the solution in the reaction kettle is close to 80 ℃, adding NaOH solution to adjust the pH value to 9.5, stirring until the pH value is stable, adding 75mL of 1% sulfuric acid ethanol solution into the reaction kettle under the condition of stirring at 80 ℃, stirring and dispersing, preparing 75mL of 0.15M sodium silicate aqueous solution, adding into the reaction kettle after completely dispersing, and continuing stirring and reacting for 6 hours at 80 ℃; finally, a powdery product is obtained.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The modified white carbon black micron aggregate is characterized in that the aggregate is formed by aggregating sheet-shaped structures, and the sheet-shaped structures are fumed silica with the surface being coated by inorganic silicon.
2. The modified white carbon black micron aggregate according to claim 1, wherein the particle size of the aggregate is 1-6 μm, and the length of the sheet-like structure is 20-40 nm;
preferably, the aggregates have a particle size of 1 μm to 5 μm, for example 2 μm, 3 μm, 4 μm;
preferably, the length of the sheet-like structure is from 25nm to 35nm, such as 20nm, 25nm, 35nm, 40nm;
preferably, the hydrated particle size of the aggregates is from 2 μm to 4 μm.
3. The modified white carbon black micro-aggregate according to claim 1,
the aggregate is of a powder structure;
preferably, the aggregate has a transmissive electron micromirror pattern as illustrated in fig. 1, fig. 2, fig. 4, or fig. 5;
preferably, the aggregates have a hydrated particle size profile as depicted in fig. 3 or fig. 6.
4. The preparation method of the modified white carbon black micron aggregate according to any one of claims 1 to 3, which comprises the following steps:
s1, putting fumed silica into a reaction kettle, adding a silane ethanol solution, stirring until the silane ethanol solution is completely dispersed, and heating the dispersion liquid to 70-90 ℃, such as 75-85 ℃, such as 80 ℃;
and S2, adjusting the pH value of the solution to be acidic, and adding a sodium silicate aqueous solution to react to obtain an aggregate.
5. The preparation method according to claim 4, wherein the mass concentration of fumed silica in the dispersion is 10-50mg/mL, preferably 20-40mg/mL;
preferably, the fumed silica is fumed hydrophobic silica.
6. The method according to claim 4, wherein the silanol solution is a solution obtained by dissolving silane in an alcohol solvent;
preferably, the silane is one or a combination of two or more of hexamethyldisiloxane, hexamethyldisilazane, heptamethyldisilazane, octamethylcyclotetrasilazane, tetramethyldivinyldisiloxane, tetramethyldivinyldisilazane, diethoxymethylvinylsilane, dimethoxymethylphenylsilane, diethoxyphenylsilane, phenyltrimethoxysilane and phenyltriethoxysilane;
preferably, the alcohol solvent is a C2-C5 alcohol, preferably ethanol, propanol, isopropanol, butanol, isobutanol or pentanol, for example ethanol.
7. The method according to claim 4, wherein the steps between S1 and S2 further comprise the steps of adjusting the pH of the dispersion to be alkaline and stable;
preferably, the alkaline pH value is 8 or more, preferably 9 or more, for example, 9.5;
preferably, naOH is used to adjust the pH of the dispersion.
8. The method according to claim 4, wherein the step S2 of adjusting the pH of the solution to acidity is performed using an acidic alcohol solution obtained by dissolving an inorganic acid in an alcohol;
preferably, the inorganic acid is sulfuric acid or nitric acid;
preferably, the alcohol is a C2-C5 alcohol, preferably ethanol, propanol, isopropanol, butanol, isobutanol or pentanol, for example ethanol;
for example, the acidic alcohol solution is a sulfuric acid ethanol solution, and preferably, the mass concentration of sulfuric acid in the sulfuric acid ethanol solution is 1%.
9. The method according to claim 8, wherein the step S2 is performed under stirring at a temperature of 80 ℃;
preferably, the reaction time after the sodium silicate aqueous solution is added in the step S2 is 4-8h.
10. Use of the white carbon black micro-aggregates according to any one of claims 1 to 3 as a rubber additive.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4882133A (en) * 1986-03-14 1989-11-21 Sumitomo Chemical Company, Limited Method for producing a flaky material
JPH1129317A (en) * 1997-05-14 1999-02-02 Doukai Kagaku Kogyo Kk Scaly low crystalline silica and its production
JP2001262067A (en) * 2000-03-23 2001-09-26 Dokai Chemical Industries Co Ltd Curable composition for heat insulating coating material containing scaly silica particle and heat insulating cured product
US20090247655A1 (en) * 2006-10-10 2009-10-01 Korea Institute Of Industrial Technology Method for preparing permanently hydrophobic aerogel and permanently hydrophobic aerogel prepared by using the method
JP2012025596A (en) * 2010-07-20 2012-02-09 Shin-Etsu Chemical Co Ltd Method for producing agglomerated silica microparticle
CN103937293A (en) * 2014-04-28 2014-07-23 北京化工大学 Carbon-coated white carbon black
CN109354876A (en) * 2018-10-09 2019-02-19 河南骏化发展股份有限公司 A kind of preparation method of silicon rubber modified white carbon black

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4882133A (en) * 1986-03-14 1989-11-21 Sumitomo Chemical Company, Limited Method for producing a flaky material
JPH1129317A (en) * 1997-05-14 1999-02-02 Doukai Kagaku Kogyo Kk Scaly low crystalline silica and its production
JP2001262067A (en) * 2000-03-23 2001-09-26 Dokai Chemical Industries Co Ltd Curable composition for heat insulating coating material containing scaly silica particle and heat insulating cured product
US20090247655A1 (en) * 2006-10-10 2009-10-01 Korea Institute Of Industrial Technology Method for preparing permanently hydrophobic aerogel and permanently hydrophobic aerogel prepared by using the method
JP2012025596A (en) * 2010-07-20 2012-02-09 Shin-Etsu Chemical Co Ltd Method for producing agglomerated silica microparticle
CN103937293A (en) * 2014-04-28 2014-07-23 北京化工大学 Carbon-coated white carbon black
CN109354876A (en) * 2018-10-09 2019-02-19 河南骏化发展股份有限公司 A kind of preparation method of silicon rubber modified white carbon black

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