CN112174150A - Preparation method of precipitated white carbon black for silicone adhesive - Google Patents
Preparation method of precipitated white carbon black for silicone adhesive Download PDFInfo
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- CN112174150A CN112174150A CN202010929836.5A CN202010929836A CN112174150A CN 112174150 A CN112174150 A CN 112174150A CN 202010929836 A CN202010929836 A CN 202010929836A CN 112174150 A CN112174150 A CN 112174150A
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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
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation method of precipitated white carbon black for silicone adhesive, which comprises the following preparation steps: s1: preparing precipitated silica white by using a water glass solution; s2: adding dilute sulfuric acid into the precipitated white carbon black, adjusting the pH value, adding an organosilane dispersing agent, aging, cooling, and filtering to obtain a filter cake; s3: washing the filter cake with water, re-dispersing the washed filter cake in water, and uniformly dispersing to obtain slurry; s4: and (3) spray drying the slurry, and then crushing by high-temperature airflow to obtain the precipitated white carbon black for the silicone adhesive. According to the preparation method, the organosilane dispersing agent is added, so that the particle size of the precipitated white carbon black can be reduced, a structure similar to fumed silica is obtained, and the polarity of the particle surface is reduced, so that the precipitated white carbon black can be easily dispersed in polydimethylsiloxane.
Description
Technical Field
The invention relates to the technical field of high polymer material processing, in particular to a preparation method of precipitated white carbon black for silicone adhesive.
Background
The silicone adhesive is one of the sealants, which is produced by taking linear polysiloxane as a main raw material and is also called as an organosilicon sealant. The silicone adhesive is a key bonding sealing material for glass curtain walls, aluminum plate curtain walls and stone curtain walls. The foreign silicone adhesive production and application is of a high level and the market worldwide is essentially occupied by several large companies, such as Dow Corning, GE, Wacker, france RP, japan news, etc., in the united states. The Dow Corning product occupies the domestic major market. Since the 1990 s, the development speed of silicone adhesive in China is obviously accelerated, domestic products of acid silicone adhesive occupy more than 50% of the domestic market, and neutral silicone adhesive products are also put into the market.
The single-component silicone adhesive takes hydroxyl-terminated polydimethylsiloxane as a basic adhesive material, a neutral silicone adhesive product takes ketoxime silane as a cross-linking agent, and the neutral silicone adhesive product is uniformly mixed with a plasticizer, a filler, a catalyst, an adhesion promoter, a vulcanization accelerator and the like under an anhydrous condition, then is filled in a sealed container, is extruded when in use, and is cured into an elastomer with excellent performance after contacting moisture in the atmosphere. Silicone adhesives have an amorphous structure, weak inter-chain interactions, and poor strength without reinforcement, and therefore a certain amount of filler must be added. At present, fumed silica is the most common reinforcing filler in silicone adhesive, especially transparent neutral adhesive. The surface of the material has less silicon hydroxyl, low water content, easy dispersion and difficult generation of structurization in the mixing and storing process. However, the price of fumed silica is high, and if precipitated silica produced by a liquid phase method can be used for replacing fumed silica, the production cost of the transparent silicone adhesive is greatly reduced.
The white carbon black precipitated by the liquid phase method is mainly synthesized by a water phase, and because water and silicon hydroxyl have stronger affinity, the surface water content and the quantity of the silicon hydroxyl are higher than those of fumed silica, the white carbon black is difficult to disperse when being directly used as a reinforcing filler of silicone adhesive, and is easy to generate structurization in the mixing and storing processes, so that strict water removal is needed during use, the cost is increased, and the cost advantage of replacing the fumed silica cannot be embodied.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the preparation method of the precipitated white carbon black for the silicone adhesive, which is added with the organosilane dispersing agent, so that on one hand, the particle size of the precipitated white carbon black can be reduced, the structure similar to fumed silica is obtained, and simultaneously, the polarity of the particle surface is reduced, so that the precipitated white carbon black is easier to disperse in polydimethylsiloxane in the silicone adhesive.
The invention is realized by adopting the following technical scheme:
a preparation method of precipitated white carbon black for silicone adhesive comprises the following preparation steps:
s1: preparing precipitated silica white by using a water glass solution;
s2: adding dilute sulfuric acid into the precipitated white carbon black, adjusting the pH value, adding an organosilane dispersing agent, aging, cooling, and filtering to obtain a filter cake;
s3: washing the filter cake with water, re-dispersing the washed filter cake in water, and uniformly dispersing to obtain slurry;
s4: and (3) spray drying the slurry, and then crushing by high-temperature airflow to obtain the precipitated white carbon black for the silicone adhesive.
Further, the concentration of silicon dioxide in the water glass solution is 10-20 wt%, and the modulus is 3.35.
Further, the concentration of the dilute sulfuric acid is 10 wt% -30 wt%.
Further, the organosilane dispersing agent consists of 3-glycidoxypropyltrimethoxysilane and long-chain alkylalkoxysilane.
Further, the long-chain alkyl alkoxy silane is one or more of hexadecyl trimethoxy silane, isobutyl trimethoxy silane, octyl trimethoxy silane and dodecyl trimethoxy silane.
Furthermore, the solid content of the 3-glycidoxypropyltrimethoxysilane in the organosilane dispersing agent is 1-3%, and the solid content of the long-chain alkylalkoxysilane is 1-3%.
Further, in step S2, the aging time is 0.5h to 1.5h, and the cooling temperature is 60 ℃ to 70 ℃.
Further, in step S4, the temperature of the high-temperature gas flow is not less than 200 ℃.
Further, the preparation method of the precipitated white carbon black for the silicone adhesive comprises the following preparation steps:
s1: preparing a water glass solution with the silicon dioxide concentration of 10-20 wt% and the modulus of 3.35 for later use;
s2: adding water and a water glass solution into a stirring reaction container at the temperature of 60-90 ℃, adding 10-30 wt% sulfuric acid, adjusting the pH value to 5-7, and obtaining a first reaction solution after the reaction is finished;
s3: adding sodium hydroxide into the first reaction solution, adjusting the pH value to 8-10, simultaneously heating to 80-100 ℃, keeping aging for 2 hours at the temperature, and obtaining a second reaction solution after aging is completed;
s4: adding dilute sulfuric acid into the second reaction solution, adjusting the pH value to 2-4, adding an organosilane dispersing agent, aging for 0.5-1.5 h, cooling to 60-70 ℃, and filtering to obtain a filter cake;
s5: washing the filter cake with water, re-dispersing the washed filter cake in a small amount of water, and uniformly dispersing to obtain slurry;
s6: and (3) spray drying the slurry, and then crushing by high-temperature airflow at the temperature of not less than 200 ℃ to obtain the precipitated white carbon black for the silicone adhesive.
Further, the particle size of the precipitated silica for the silicone adhesive is not more than 2 μm.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the preparation method disclosed by the invention, the organosilane dispersing agent is added, so that on one hand, the particle size of the precipitated white carbon black can be reduced, a structure similar to fumed silica is obtained, and simultaneously, the polarity of the particle surface is reduced, so that the precipitated white carbon black is easier to disperse in polydimethylsiloxane.
(2) The preparation method of the invention adopts a high-temperature airflow crushing mode, so that the organosilane dispersing agent can be combined with the particle surface more firmly, the surface polarity is reduced, and the moisture in the precipitated white carbon black can be effectively reduced under the high-temperature condition.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
The invention provides a preparation method of precipitated white carbon black for silicone adhesive, which comprises the following preparation steps:
s1: preparing a water glass solution with the silicon dioxide concentration of 10-20 wt% and the modulus of 3.35 for later use;
s2: adding water and a water glass solution into a stirring reaction container at the temperature of 60-90 ℃, adding 10-30 wt% sulfuric acid, adjusting the pH value to 5-7, and obtaining a first reaction solution after the reaction is finished;
s3: adding sodium hydroxide into the first reaction solution, adjusting the pH value to 8-10, simultaneously heating to 80-100 ℃, keeping aging for 2 hours at the temperature, and obtaining a second reaction solution after aging is completed;
s4: adding 10-30 wt% of dilute sulfuric acid into the second reaction solution, adjusting the pH value to 2-4, adding an organosilane dispersing agent, aging for 0.5-1.5 h, cooling to 60-70 ℃, and filtering to obtain a filter cake; the organic silane dispersing agent is added to disperse particles on one hand and carry out organic treatment on the surfaces of the particles on the other hand;
s5: washing the filter cake with water, re-dispersing the washed filter cake in a small amount of water, and uniformly dispersing to obtain slurry; wherein, the filter cake is washed by water, so that the content of sodium ions and sulfate radicals in the silicon dioxide can be reduced;
s6: spray drying the slurry, and then crushing by high-temperature airflow at the temperature of not less than 200 ℃ to obtain precipitated white carbon black with the particle size of not more than 2 mu m for the silicone adhesive; wherein the maximum temperature of the high-temperature airflow is 300 ℃, namely the temperature of the high-temperature airflow is 200-300 ℃.
In one embodiment, the organosilane dispersant consists of 3-glycidoxypropyltrimethoxysilane and a long chain alkylalkoxysilane; preferably, the solid content of the 3-glycidoxypropyltrimethoxysilane in the organosilane dispersing agent is 1-3%, and the solid content of the long-chain alkylalkoxysilane is 1-3%. Wherein the long-chain alkyl alkoxy silane is one or more of hexadecyl trimethoxy silane, isobutyl trimethoxy silane, octyl trimethoxy silane and dodecyl trimethoxy silane.
Preferably, the mass ratio of the organosilane dispersing agent to the water glass solution is 15-5: 1.
the following are specific examples of the present invention, and raw materials, equipment, and the like used in the following examples can be obtained by purchasing, unless otherwise specified.
Example 1:
100L of bottom water and 75L of a 20 wt% water glass solution were charged into a stirred reaction vessel at a temperature of 80 ℃ and sulfuric acid having a concentration of 10 wt% was added for 30 minutes until the pH of the system became 6.
After the reaction is finished, the temperature is raised to 100 ℃, and meanwhile, sodium hydroxide is added to adjust the pH value to 9, and the aging is carried out for 2 hours.
After the aging is completed, sulfuric acid is added to adjust the pH value to 3, 3-glycidoxypropyltrimethoxysilane with the solid content of 2% and hexadecyltrimethoxysilane with the solid content of 2% are added, the mixture is aged for 1.5 hours, then the temperature is cooled to 60 ℃, and the filter cake is obtained by filtration.
And re-dispersing the filter cake in a small amount of water, uniformly dispersing to obtain slurry, performing spray drying, and performing jet milling at 200 ℃ to obtain a product with the particle size of 2 microns.
1500g of 107 glue with 8 ten thousand of viscosity, 1647g of silicone oil and 500g of white carbon black in the embodiment are vacuumized for 3 hours (the pressure is lower than 0.08MPa) at the temperature of below 150 ℃, and then the mixture is discharged and cooled to prepare base glue; weighing 1000g of base adhesive, 67.2g of methyl tributyl ketoxime silane, 8g of vinyl tributyl ketoxime silane, 2.4g of KH-550 silane coupling agent, 5.6g of KH-560 silane coupling agent and 80g of white oil, vacuumizing and stirring for 30 minutes (the pressure is lower than 0.08MPa), and then filling into a cylinder to obtain the neutral transparent silicone adhesive. The results of the test according to GB-T14683-2003 'Silicone building sealant' standard are shown in the following table 1:
TABLE 1
Example 2:
100L of bottom water and 75L of a 20 wt% water glass solution were charged into a stirred reaction vessel at a temperature of 60 ℃ and sulfuric acid having a concentration of 30 wt% was added for 30 minutes until the pH of the system became 5.
After the reaction is finished, the temperature is raised to 80 ℃, and meanwhile, sodium hydroxide is added to adjust the pH value to 10, and the aging is carried out for 2 hours.
After the aging is completed, sulfuric acid is added to adjust the pH value to 2, 3-glycidoxypropyltrimethoxysilane with the solid content of 2% and dodecyl trimethoxysilane with the solid content of 2% are added, the aging is carried out for 0.5 hour, then the temperature is cooled to 60 ℃, and the filter cake is obtained by filtration.
And re-dispersing the filter cake in a small amount of water, uniformly dispersing to obtain slurry, performing spray drying, and performing air flow crushing at 210 ℃ to obtain a product with the particle size of 2 microns.
1500g of 107 glue with 8 ten thousand of viscosity, 1647g of silicone oil and 500g of white carbon black in the embodiment are vacuumized for 3 hours (the pressure is lower than 0.08MPa) at the temperature of below 150 ℃, and then the mixture is discharged and cooled to prepare base glue; weighing 1000g of base adhesive, 67.2g of methyl tributyl ketoxime silane, 8g of vinyl tributyl ketoxime silane, 2.4g of KH-550 silane coupling agent, 5.6g of KH-560 silane coupling agent and 80g of white oil, vacuumizing and stirring for 30 minutes (the pressure is lower than 0.08MPa), and then filling into a cylinder to obtain the neutral transparent silicone adhesive. The results of the test according to GB-T14683-2003 'Silicone building sealant' standard are shown in the following table 2:
TABLE 2
Test item | The result of the detection |
Appearance of the product | Transparent, viscous, bubble-like, without crusting or gelling |
Degree of sagging | Without deformation |
Open time (minutes) | 30 |
Extrudability (milliliters per minute) | 208 |
Elastic recovery rate | 95.71% |
Tensile modulus (MPa) | 0.35 |
Definite elongation adhesion | Without destruction |
Adhesion after UV irradiation | Without destruction |
Cold drawing-hot pressing adhesion | Without destruction |
Fixed-elongation cohesiveness after immersion in water | Without destruction |
Example 3:
100L of bottom water and 75L of a 20 wt% water glass solution were charged into a stirred reaction vessel at a temperature of 90 ℃ and sulfuric acid having a concentration of 20 wt% was added for 30 minutes until the pH of the system became 7.
After the reaction is finished, the temperature is maintained at 90 ℃, and meanwhile, sodium hydroxide is added to adjust the pH value to 8, and the aging is carried out for 2 hours.
After the aging is completed, sulfuric acid is added to adjust the pH value to 4, 3-glycidoxypropyltrimethoxysilane with the solid content of 2% and isobutyltrimethoxysilane with the solid content of 2% are added, the aging is carried out for 1.0 hour, then the temperature is cooled to 60 ℃, and the filter cake is obtained by filtration.
And re-dispersing the filter cake in a small amount of water, uniformly dispersing to obtain slurry, performing spray drying, and performing air flow crushing at 210 ℃ to obtain a product with the particle size of 2 microns.
1500g of 107 glue with 8 ten thousand of viscosity, 1647g of silicone oil and 500g of white carbon black in the embodiment are vacuumized for 3 hours (the pressure is lower than 0.08MPa) at the temperature of below 150 ℃, and then the mixture is discharged and cooled to prepare base glue; weighing 1000g of base adhesive, 67.2g of methyl tributyl ketoxime silane, 8g of vinyl tributyl ketoxime silane, 2.4g of KH-550 silane coupling agent, 5.6g of KH-560 silane coupling agent and 80g of white oil, vacuumizing and stirring for 30 minutes (the pressure is lower than 0.08MPa), and then filling into a cylinder to obtain the neutral transparent silicone adhesive. The results of the test according to GB-T14683-2003 'Silicone building sealant' standard are shown in the following table 3:
TABLE 3
Example 4:
100L of bottom water and 75L of a 20 wt% water glass solution were charged into a stirred reaction vessel at a temperature of 80 ℃ and sulfuric acid having a concentration of 10 wt% was added for 30 minutes until the pH of the system became 7.
After the reaction is finished, the temperature is raised to 100 ℃, and meanwhile, sodium hydroxide is added to adjust the pH value to 8, and the aging is carried out for 2 hours.
After the aging is completed, sulfuric acid is added to adjust the pH value to 3, 3-glycidoxypropyltrimethoxysilane with the solid content of 2% and octyltrimethoxysilane with the solid content of 2% are added, the aging is carried out for 1.5 hours, then the temperature is cooled to 60 ℃, and the filter cake is obtained by filtration.
And re-dispersing the filter cake in a small amount of water, uniformly dispersing to obtain slurry, performing spray drying, and performing jet milling at 200 ℃ to obtain a product with the particle size of 2 microns.
1500g of 107 glue with 8 ten thousand of viscosity, 1647g of silicone oil and 500g of white carbon black in the embodiment are vacuumized for 3 hours (the pressure is lower than 0.08MPa) at the temperature of below 150 ℃, and then the mixture is discharged and cooled to prepare base glue; weighing 1000g of base adhesive, 67.2g of methyl tributyl ketoxime silane, 8g of vinyl tributyl ketoxime silane, 2.4g of KH-550 silane coupling agent, 5.6g of KH-560 silane coupling agent and 80g of white oil, vacuumizing and stirring for 30 minutes (the pressure is lower than 0.08MPa), and then filling into a cylinder to obtain the neutral transparent silicone adhesive. The results of the test according to GB-T14683-2003 'Silicone building sealant' standard are shown in the following table 4:
TABLE 4
Comparative example 1:
100L of bottom water and 75L of a 20 wt% water glass solution were charged into a stirred reaction vessel at a temperature of 80 ℃ and sulfuric acid having a concentration of 10 wt% was added for 30 minutes until the pH of the system became 7.
After the reaction is finished, the temperature is raised to 100 ℃, and meanwhile, sodium hydroxide is added to adjust the pH value to 8, and the aging is carried out for 2 hours.
After the aging is completed, sulfuric acid is added to adjust the pH value to 3, 3-glycidoxypropyltrimethoxysilane with the solid content of 2% is added, the aging is carried out for 1.5 hours, then the temperature is cooled to 60 ℃, and the filter cake is obtained by filtering.
And re-dispersing the filter cake in a small amount of water, uniformly dispersing to obtain slurry, performing spray drying, and performing jet milling at 200 ℃ to obtain a product with the particle size of 2 microns.
1500g of 107 glue with 8 ten thousand of viscosity, 1647g of silicone oil and 500g of white carbon black in the embodiment are vacuumized for 3 hours (the pressure is lower than 0.08MPa) at the temperature of below 150 ℃, and then the mixture is discharged and cooled to prepare base glue; weighing 1000g of base adhesive, 67.2g of methyl tributyl ketoxime silane, 8g of vinyl tributyl ketoxime silane, 2.4g of KH-550 silane coupling agent, 5.6g of KH-560 silane coupling agent and 80g of white oil, vacuumizing and stirring for 30 minutes (the pressure is lower than 0.08MPa), and then filling into a cylinder to obtain the neutral transparent silicone adhesive. The results of the test according to GB-T14683-2003 'Silicone building sealant' standard are shown in the following table 5:
TABLE 5
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. The preparation method of the precipitated white carbon black for the silicone adhesive is characterized by comprising the following preparation steps:
s1: preparing precipitated silica white by using a water glass solution;
s2: adding dilute sulfuric acid into the precipitated white carbon black, adjusting the pH value, adding an organosilane dispersing agent, aging, cooling, and filtering to obtain a filter cake;
s3: washing the filter cake with water, re-dispersing the washed filter cake in water, and uniformly dispersing to obtain slurry;
s4: and (3) spray drying the slurry, and then crushing by high-temperature airflow to obtain the precipitated white carbon black for the silicone adhesive.
2. The method for preparing precipitated silica for silicone adhesive according to claim 1, wherein the silica concentration in the water glass solution is 10-20 wt% and the modulus is 3.35.
3. The method for preparing precipitated silica white for silicone adhesive according to claim 1, wherein the concentration of the dilute sulfuric acid is 10 wt% to 30 wt%.
4. The method for preparing precipitated silica for silicone adhesive according to claim 1, wherein the organosilane dispersing agent is composed of 3-glycidoxypropyltrimethoxysilane and long-chain alkylalkoxysilane.
5. The method for preparing precipitated silica for silicone adhesive according to claim 4, wherein the long-chain alkylalkoxysilane is one or more of hexadecyltrimethoxysilane, isobutyltrimethoxysilane, octyltrimethoxysilane, and dodecyltrimethoxysilane.
6. The method for preparing precipitated silica for silicone adhesive according to claim 4, wherein the organosilane dispersing agent contains 3-glycidoxypropyltrimethoxysilane and long-chain alkylalkoxysilanes in amounts of 1-3% and 1-3%, respectively.
7. The method for preparing precipitated silica for silicone adhesive according to claim 1, wherein in step S2, the aging time is 0.5h to 1.5h, and the cooling temperature is 60 ℃ to 70 ℃.
8. The method for preparing precipitated silica for silicone adhesive according to claim 1, wherein in step S4, the temperature of the high temperature air stream is not less than 200 ℃.
9. The preparation method of the precipitated silica white for silicone adhesive according to claim 1, comprising the following preparation steps:
s1: preparing a water glass solution with the silicon dioxide concentration of 10-20 wt% and the modulus of 3.35 for later use;
s2: adding water and a water glass solution into a stirring reaction container at the temperature of 60-90 ℃, adding 10-30 wt% sulfuric acid, adjusting the pH value to 5-7, and obtaining a first reaction solution after the reaction is finished;
s3: adding sodium hydroxide into the first reaction solution, adjusting the pH value to 8-10, simultaneously heating to 80-100 ℃, keeping aging for 2 hours at the temperature, and obtaining a second reaction solution after aging is completed;
s4: adding dilute sulfuric acid into the second reaction solution, adjusting the pH value to 2-4, adding an organosilane dispersing agent, aging for 0.5-1.5 h, cooling to 60-70 ℃, and filtering to obtain a filter cake;
s5: washing the filter cake with water, re-dispersing the washed filter cake in a small amount of water, and uniformly dispersing to obtain slurry;
s6: and (3) spray drying the slurry, and then crushing by high-temperature airflow at the temperature of not less than 200 ℃ to obtain the precipitated white carbon black for the silicone adhesive.
10. The method for preparing precipitated silica for silicone adhesive according to any one of claims 1 to 9, wherein the particle size of the precipitated silica for silicone adhesive is not greater than 2 μm.
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