CN112897539A - Spherical silicon dioxide powder and preparation method and application thereof - Google Patents

Spherical silicon dioxide powder and preparation method and application thereof Download PDF

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CN112897539A
CN112897539A CN202110151666.7A CN202110151666A CN112897539A CN 112897539 A CN112897539 A CN 112897539A CN 202110151666 A CN202110151666 A CN 202110151666A CN 112897539 A CN112897539 A CN 112897539A
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water glass
glass solution
silica gel
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CN112897539B (en
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姜海波
李春忠
曹永杰
王博慧
刘伟
寿圣球
柳坤鹏
胡金能
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East China University of Science and Technology
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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
    • 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
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/152—Preparation of hydrogels
    • C01B33/154—Preparation of hydrogels by acidic treatment of aqueous silicate solutions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/42—Gloss-reducing agents
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume
    • 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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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses spherical silicon dioxide powder and a preparation method and application thereof. The preparation method comprises the following steps: (1) under the stirring condition of a turbulent flow reactor, mixing and reacting silica gel, a first water glass solution and a first acidifying agent to ensure that the pH value of a system is 8-9, and continuously adding the first acidifying agent to react to ensure that the pH value of the system is 4-5; SiO in the silica gel2With Na in the first water glass solution2SiO3Is 1: (3-5); (2) and carrying out suction filtration, washing and drying on the mixture to obtain the catalyst. The spherical silicon dioxide has the advantages of high specific surface, large pore volume, proper average particle size and regular micro-morphology, and is suitable for being used as a flatting agent in coating. The preparation process is simple and easy to operate, the raw materials are cheap and easy to obtain, the cost is low, and the industrial production is easy to realize.

Description

Spherical silicon dioxide powder and preparation method and application thereof
Technical Field
The invention relates to spherical silicon dioxide powder and a preparation method and application thereof.
Background
Silica is one of the most abundant materials stored in nature, and is widely found in marine organisms such as diatoms and sponges, and in terrestrial plants. It is an amorphous white powder, light in weight, and is an inorganic non-metallic material with no toxicity, no smell and no pollution. The composite material has the advantages of high insulativity, high chemical purity, good dispersibility, large specific surface area and the like, so that the composite material has extremely wide application in the fields of medicines, plastics, coatings, ceramics, rubber and the like and has wide market prospect.
With the development of the automobile and household appliance industry in China, the demand of the industry on the coating is increased year by year. The high-gloss bright paint is very popular with consumers due to the advantages of bright color, brightness and the like, and is called as the leading part of the paint market for a long time. However, the high-gloss glossy paint has a relatively serious light reflection after being formed into a film, and visually produces a strong irritating feeling. The addition of a flatting agent to the coating to reduce the gloss of the coating just meets the current demand for different gloss of the coating. The artificially synthesized silicon dioxide has the advantages of good extinction effect, easy addition, easy storage, stable chemical property and the like, so that the silicon dioxide becomes the extinction agent product with the most extensive application.
The preparation method of the spherical silicon dioxide at present mainly comprises a physical method and a chemical method. Physical methods such as ball milling, high frequency plasma, etc. are not highly applicable due to low preparation efficiency and conventional methods. The chemical method includes a gas phase method, a sol-gel method, a chemical precipitation method, and the like. The gas phase method takes silane halide as a raw material,it has the disadvantages of expensive raw materials, high equipment requirement, long production flow and large energy consumption. The sol-gel method uses silicate ester and the like as raw materials, and has the defects of expensive raw materials and higher production cost. Chinese patent document CN111017933A discloses a preparation method of high specific surface area silica, and the specific surface area of the synthesized silica is claimed to be high, but the specific surface area is only limited to 320-360 m2And its average particle diameter is too small, low specific surface area and too small an average particle diameter making it unsuitable for use as a matting agent. In addition, the patent does not disclose the features of the micro-morphology, pore volume, etc. of the silica particles that greatly affect the performance of the polishing agent. Therefore, how to obtain silica with high specific surface area, high pore volume, proper particle size and regular micro-morphology is a problem to be solved in the field.
Disclosure of Invention
The invention provides spherical silicon dioxide powder, a preparation method and application thereof, and aims to overcome the defect that the prior art cannot provide silicon dioxide with high specific surface area, high pore volume, proper particle size and regular micro-morphology. The spherical silicon dioxide has the advantages of high specific surface, large pore volume, proper average particle size and regular micro-morphology, and is suitable for being used as a flatting agent in coating. The preparation process is simple and easy to operate, the raw materials are cheap and easy to obtain, the cost is low, and the industrial production is easy to realize.
The turbulent flow reactor, i.e. the high-speed dispersion homogenizer, generates strong hydraulic shearing and high-frequency mechanical effect under the high-speed drive of a motor, so that the material is crushed at high speed. Although it is well known to those skilled in the art that a turbulent flow reactor can disperse and homogenize an immiscible solid phase and a liquid phase uniformly and finely instantaneously, the strong shearing action generated by the high rotating speed of the turbulent flow reactor can destroy the spherical morphology of the formed silica particles, so that the skilled in the art generally cannot adopt the turbulent flow reactor to synthesize the silica, cannot expect the comprehensive performance of the silica prepared by the turbulent flow reactor to be good, and is suitable for being used as a delustering agent in coatings.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of spherical silicon dioxide powder, which comprises the following steps:
(1) mixing and reacting silica gel, a first water glass solution and a first acidifier while stirring in a turbulent flow reactor, wherein SiO in the silica gel2With Na in the first water glass solution2SiO3Is 1: (3-5) when the pH value of the system is 8-9, continuously adding the first acidifying agent to enable the pH value of the system to be 4-5, and continuously reacting to obtain a mixture;
(2) and carrying out solid-liquid separation on the mixture to obtain solid, namely the spherical silicon dioxide.
In step (1), the turbulent flow reactor may be a high-speed dispersion homogenizer conventional in the art, preferably a high-speed dispersion homogenizer model FJ-200, more preferably a high-speed dispersion homogenizer model FJ-200 manufactured by Shanghai provincial industries, Ltd.
In step (1), the silicone gel is preferably prepared by the following steps: and mixing the second water glass solution and a second acidifier for reaction until the pH value is 6-7, and aging to obtain the water glass.
Wherein the concentration of the second water glass solution is preferably 0.1-0.5mol/L, and more preferably 0.3 mol/L.
Wherein, the second acidifying agent is preferably one or more of sulfuric acid, hydrochloric acid and nitric acid, and more preferably sulfuric acid.
Wherein, the concentration of the second acidifying agent is preferably 0.8-1.0mol/L, and more preferably 0.9 mol/L.
Wherein the solvent in the second water glass solution is water.
Wherein the modulus of the second water glass solution can be 1-3.
Among them, the kind of the second acidifying agent may be conventional in the art, and is preferably one or more of sulfuric acid, hydrochloric acid and nitric acid, and more preferably sulfuric acid.
Wherein the concentration of the second acidifying agent can be 0.8-1.0mol/L, such as 0.9 mol/L.
The operation and conditions of the mixing reaction during the preparation of the silica gel may be conventional in the art and are generally carried out in a paddle stirrer.
In the preparation process of the silica gel, the temperature of the mixing reaction can be 30-60 ℃, and preferably 45 ℃.
In the preparation of the silica gel, the mixing reaction preferably further comprises stirring.
Wherein the rotation speed of the stirring can be 200-600rpm, such as 400 rpm.
In the preparation of the silica gel, the mixing reaction is preferably performed by the following steps: the acidifying agent is added to the water glass solution until a pH of 5 to 7, preferably a pH of 6, is reached.
Wherein, the dropping speed can be generally 50-65 ml/h.
The applicant finds that in the process of multiple experiments, the pH value of the system is controlled to be beyond 5-7, such as 4 or 8, in the process of preparing the silicone gel, the obtained silicone gel has poor effect, the system cannot be completely formed, and partial flowing liquid still exists.
The aging may be performed by a method conventional in the art during the preparation of the silica gel.
Wherein the aging temperature can be 30-60 ℃, for example, 45 ℃.
Wherein the aging time may be not less than 30min, for example 45 min.
In step (1), the concentration of the first water glass solution may be conventional in the art, and may be, for example, 0.1 to 0.5mol/L, preferably 0.3 mol/L.
In step (1), the solvent in the first water glass solution is generally water.
In the step (1), the modulus of the first water glass solution may be 1 to 3.
In step (1), the kind of the first acidifying agent may be conventional in the art, and is preferably one or more of sulfuric acid, hydrochloric acid and nitric acid, and more preferably sulfuric acid.
In step (1), the concentration of the first acidifying agent can be from 0.8 to 1.0mol/L, for example 0.9 mol/L.
In the step (1), the silicone gelSiO 22With Na in the first water glass solution2SiO3Is preferably 1: 4.
in the step (1), in the process of the mixing reaction, the rotating speed can be 5000-10000 rpm, such as 8000 rpm.
In the step (1), the mixing reaction is preferably carried out as follows: adding the water glass solution and the acidifying agent simultaneously to the silica gel.
Wherein, the adding flow rate of the water glass solution is preferably not higher than 300ml/L, such as 250 ml/h.
In step (1), the mixture is preferably stirred for at least 10min, for example 20 min.
In the step (1), when the pH value of the system is 4-5, the chemical reaction in the system can continue to take place to prepare the silicon dioxide according to the common knowledge in the field.
In step (2), the solid-liquid separation can be performed by a method conventional in the art, such as suction filtration or centrifugation.
In the step (2), after the solid-liquid separation operation, the solid is preferably washed and dried.
The washing can be carried out by a method conventional in the art, and preferably, the solid obtained by the solid-liquid separation is washed with water until the filtrate is neutral.
The drying may be carried out by methods conventional in the art, preferably by spray drying.
Wherein, the conditions of the spray drying are preferably as follows: the feeding flow rate is 20-40 mL/min, the inlet temperature is 160-180 ℃, and the outlet temperature is 50-70 ℃.
Wherein, before the spray drying, a dispersing step is generally included.
The dispersion can be carried out by methods conventional in the art, preferably by the following steps: and dispersing the solid obtained by washing in a solvent, and stirring and mixing.
Wherein the rotation speed of stirring and mixing can be 1000-1500 rpm, such as 1300 rpm.
Wherein the time for stirring and mixing can be not less than 20min, for example 30 min.
The solvent can be conventional in the art, and is preferably an ethanol aqueous solution, and more preferably an ethanol aqueous solution with the mass percentage of ethanol not higher than 50%.
The invention also provides spherical silicon dioxide powder which is prepared by the preparation method of the spherical silicon dioxide powder.
The invention also provides an application of the spherical silicon dioxide powder as a delustering agent in coating.
In the present invention, "first" and "second" have no special meaning.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
the spherical silicon dioxide is regular in microscopic morphology, proper in particle size and narrow in particle size distribution range, the particle size can be 3-4 micrometers, and the difference between D90 and D50 can be 3-4 micrometers; the specific surface area is large, and the specific surface area of the obtained silicon dioxide can be higher than 400m2G, even up to 517.6m2(ii)/g; the pore volume is large and can be higher than 1.4cm3G, in a preferred embodiment up to 2.18cm3The oil absorption of the silica is generally higher than 280g/100g, and may even be as high as 301ml/100g, and is particularly suitable for use as a matting agent in coatings.
The preparation process of the invention is simple, the raw materials are cheap and easy to obtain, the investment cost is low, and the industrial production is easy.
Drawings
FIG. 1 is an SEM photograph of the silica obtained in example 1;
FIG. 2 is an SEM photograph of the silica obtained in example 2;
FIG. 3 is an SEM photograph of the silica obtained in example 3;
FIG. 4 is an SEM photograph of the silica obtained in comparative example 1;
FIG. 5 is an SEM photograph of the silica obtained in comparative example 2;
FIG. 6 is an SEM photograph of the silica obtained in comparative example 3;
FIG. 7 is an SEM photograph of the silica obtained in comparative example 4.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The water glass solution is produced by Jiangxi Dehong new materials Co.Ltd;
the sulfuric acid is produced by chemical reagent company Limited of the national drug group;
the ethanol solution of the present invention is produced by Shanghai Tantake Technology Co., Ltd.
The raw materials and reagents used in the invention are commercially available. And part of conventional tests are carried out according to the national standard method.
Example 1
Step 1: 20mL of 2mol/L concentrated water glass is measured and added with 380mL of deionized water to be diluted into 0.1mol/L water glass solution. At the temperature of 45 ℃ and the stirring speed of 200rpm, 1mol/L dilute sulfuric acid is dropwise added at the flow rate of 65mL/h until the pH value is reduced to 6.5, the stirring is stopped, and the mixture is kept in a water bath for standing and aging for 40min at the temperature of 45 ℃.
Step 2: the silica gel obtained in step 1 was broken up by stirring in a turbulent flow reactor at 5000 rpm. 150mL of 0.1mol/L water glass solution and 1mol/L dilute sulfuric acid were added at flow rates of 250mL/h and 150mL/h, respectively, to adjust the pH of the system to 9. And continuously dropwise adding a dilute sulfuric acid solution to reduce the pH of the solution to 4, stopping heating, and continuously stirring for 15 min.
And 3, carrying out suction filtration and washing on the mixture obtained in the step 2. Subsequently, the mixture was dispersed in 50% ethanol aqueous solution at 1000rpm for 30 min. The suspension was spray dried with a feed flow rate of 40mL/min, an inlet temperature of 160 ℃ and an outlet temperature of 50 ℃.
Example 2
The method is the same as example 1, except that:
in the step 1: the modulus of the water glass is 1, and the concentration of the diluted base solution is 0.3 mol/L. The temperature was 30 ℃, the stirring rate was 400rpm, and the dropping rate of dilute sulfuric acid was 50 mL/h. The temperature of the standing and aging is 30 ℃, and the time of the standing and aging is 30 min.
In the step 2: the rotational speed in the turbulent flow reactor was 8000 rpm. When the pH value is reduced to 4.5 from 9, the heating is stopped, and the stirring is continued for 20 min.
In the step 3: the rotation speed during dispersion was 1300rpm, and the dispersion time was 30 min. The feed flow rate during spray drying was 30mL/min, the inlet temperature was 170 ℃ and the outlet temperature was 60 ℃.
Example 3
The method is the same as example 1, except that:
in the step 1: the modulus of the water glass solution is 3, and the concentration of the water glass solution is 0.5 mol/L. The reaction temperature was 60 ℃, the stirring rate was 600rpm, and the dropping rate of dilute sulfuric acid was 60 mL/h.
Standing and aging at 60 deg.C for 30 min.
In the step 2: when the rotation speed of the turbulent flow reactor is 10000rpm and the pH value is reduced from 9 to 5, the heating is stopped and the stirring is continued for 30 min.
In the step 3: the dispersing agent is pure ethanol, the rotating speed during dispersing is 1500rpm, the dispersing time is 30min, the feeding flow rate of spray drying is 20mL/min, the inlet temperature is 180 ℃, and the outlet temperature is 70 ℃.
Comparative example 1
The method is the same as example 1, except that:
in step 2, the stirring was carried out at 600rpm using a paddle stirrer without high-speed stirring in a turbulent flow reactor, and the other conditions and operations were the same as in example 1.
Comparative example 2
The method is the same as example 1, except that:
the reaction was carried out by using other equipment capable of achieving the required rotation speed without using a turbulent flow reactor, and the other operations and condition settings were the same as those of example 1.
Comparative example 3
The method is the same as example 1, except that:
in step 2, the turbulent reactor was operated at 4000rpm and the other operations and conditions were the same as in example 1.
Comparative example 4
In step 2, the turbulent reactor was set to 12000rpm, and the operation and conditions were the same as in example 1.
Effects of the embodiment
The microscopical characterization of the silica obtained in examples and comparative examples was carried out by using a scanning electron microscope model S-3400, manufactured by Hitachi, Japan. As is evident from FIGS. 1 to 7, the materials obtained in examples 1 to 3 had smooth surfaces, regular sphericity, and narrow particle size distribution.
The silica obtained in examples and comparative examples was subjected to a particle size test using a model LS230 laser particle sizer manufactured by Beckmann Coulter, USA, to obtain an average particle size. The average particle size D50 of the silicon dioxide obtained in the embodiments 1-3 is 3-4 μm, the particle size is moderate, and D90-D50 is 3-4 μm and is suitable for being used as a delustering agent. The average particle size of the silicon dioxide synthesized by the comparative example is greatly changed, the particle size distribution range is wide, and the performance is unstable.
The specific surface area and pore volume of the silica materials obtained in examples and synthesis examples were measured by nitrogen adsorption using a specific surface area analyzer model ASAP-2480 manufactured by Shanghai Mimmerley Rick instruments Ltd. The specific surface area of the silicon dioxide synthesized by the examples 1-3 is higher than 400m2/g, especially the specific surface area of the silicon dioxide synthesized by the example 1 is as high as 517.6m2/g, which is far more than that of the silicon dioxide synthesized by the comparative example. The pore volume of the silicon dioxide synthesized in the examples 1-3 is higher than 1.497cm3/g, especially the pore volume of the silicon dioxide obtained in the examples 2 and 3 is more than 2cm3/g, which is much higher than that of the silicon dioxide synthesized in the comparative example.
Methods, instruments and tools for testing the oil absorption value of silica are described in GB 10528-1989.
TABLE 1 test data for spherical silica powders
Figure BDA0002931687040000091

Claims (10)

1. A preparation method of spherical silicon dioxide comprises the following steps:
(1) mixing and reacting silica gel, a first water glass solution and a first acidifier while stirring in a turbulent flow reactor, wherein SiO in the silica gel2With Na in the first water glass solution2SiO3Is 1: (3-5) when the pH value of the system is 8-9, continuously adding the first acidifying agent to enable the pH value of the system to be 4-5, and continuously reacting to obtain a mixture;
(2) and carrying out solid-liquid separation on the mixture to obtain solid, namely the spherical silicon dioxide.
2. The method of preparing spherical silica according to claim 1, wherein the turbulent flow reactor is a FJ-200 type high-speed dispersion homogenizer.
3. The method for preparing spherical silica according to claim 1, wherein the preparation of the silica gel comprises the steps of: mixing the second water glass solution and a second acidifying agent for reaction until the pH value is 6-7, and aging to obtain the water glass;
wherein the concentration of the second water glass solution is preferably 0.1-0.5mol/L, and more preferably 0.3 mol/L;
the second acidifying agent is preferably one or more of sulfuric acid, hydrochloric acid and nitric acid, more preferably sulfuric acid;
the concentration of the second acylating agent is preferably 0.8 to 1.0mol/L, more preferably 0.9 mol/L.
4. The method for preparing spherical silica according to claim 3, wherein the temperature of the mixing reaction is 30-60 ℃, preferably 45 ℃ during the preparation of the silica gel;
and/or in the preparation process of the silica gel, the mixing reaction process further comprises a stirring step, wherein the stirring speed is 200-600rpm, such as 400 rpm;
and/or in the preparation process of the silica gel, the mixing reaction is carried out according to the following steps: dropwise adding the second acidifying agent into the second water glass solution until the pH value is 5-7, preferably 6;
and/or the temperature of the aging is 30-60 ℃, such as 45 ℃;
and/or the aging time is not less than 30min, such as 45 min.
5. The method for preparing spherical silica according to claim 1, wherein the concentration of the first water glass solution is 0.1 to 0.5mol/L, preferably 0.3 mol/L;
and/or the first acidifying agent is one or more of sulfuric acid, hydrochloric acid and nitric acid, preferably sulfuric acid;
and/or the concentration of the first acidifying agent is 0.8-1.0mol/L, preferably 0.9 mol/L.
6. The method for preparing spherical silica according to claim 1, wherein the stirring is performed at a speed of 5000 to 10000rpm, such as 8000 rpm.
7. The method for preparing spherical silica according to claim 1, wherein the mixing reaction is carried out by the following steps: adding said first water glass solution and said first acidifying agent to said silica gel as SiO in said silica gel2With Na in the first water glass solution2SiO3Is 1: (3-5) when the pH value of the system is 8-9, continuously adding the first acidifying agent to enable the pH value of the system to be 4-5;
wherein, the adding flow rate of the water glass solution is not higher than 300 ml/L.
8. The method for preparing spherical silica according to claim 1, wherein the obtained solid is further washed and dried;
wherein, the drying is preferably spray drying;
wherein, before the spray drying, a dispersion step is also included; the dispersed solvent is preferably ethanol water, and more preferably ethanol water with the mass percent of ethanol not higher than 50%;
and/or the feeding flow rate of the spray drying is 20-40 mL/min;
and/or the inlet temperature of the spray drying is 160-180 ℃;
and/or the outlet temperature of the spray drying is 50-70 ℃.
9. A spherical silica powder produced by the production method according to any one of claims 1 to 8.
10. Use of the spherical silica powder according to claim 9 as matting agent in coatings.
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CN116004109A (en) * 2023-01-06 2023-04-25 湖北航天化学技术研究所 Skin-feel coating, skin-feel film and preparation method and application thereof

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