CN111747417A - Preparation method of silicon dioxide particles - Google Patents
Preparation method of silicon dioxide particles Download PDFInfo
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- CN111747417A CN111747417A CN201910242419.0A CN201910242419A CN111747417A CN 111747417 A CN111747417 A CN 111747417A CN 201910242419 A CN201910242419 A CN 201910242419A CN 111747417 A CN111747417 A CN 111747417A
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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
Abstract
The invention relates to the technical field of silicon dioxide particles, and discloses a preparation method of silicon dioxide particles, which comprises the following steps: 1) adding 1-50 parts of silicon dioxide slurry, 1-100 parts of hot solution, 3-90 parts of ethanolamine solution, 3-90 parts of aliphatic amine, 3-90 parts of aromatic amine solution and 3-90 parts of polyethyleneimine solution into a mixing and stirring reaction kettle, controlling the stirring time to be 1-2 hours, improving the overall temperature inside the reaction kettle to 250 ℃ by matching between mechanical stirring and materials, and placing the mixed materials in a standing device for later use; 2) placing the stewing device in the step 1) and the mixed materials in an open place, and reducing the temperature of the materials in the stewing device to 20-35 ℃ within 2-3 hours of natural time. According to the preparation method of the silicon dioxide particles, the solid silicon dioxide is blown by using the purified gas, so that the cleanliness of the silicon dioxide particles is integrally improved, the content of impurities in the silicon dioxide particles is reduced, and the silicon dioxide particles are convenient to use.
Description
Technical Field
The invention relates to the technical field of silicon dioxide particles, in particular to a preparation method of silicon dioxide particles.
Background
Silica, chemical term, pure silica is colorless, solid at room temperature, and has the chemical formula SiO2The silicon dioxide is not dissolved in water and acid, but dissolved in hydrofluoric acid and hot concentrated phosphoric acid, can act with molten alkali, has two kinds of crystalline silicon dioxide and amorphous silicon dioxide in nature, has wide application range, is mainly used for manufacturing glass, water glass, pottery, enamel, refractory materials, aerogel felt, ferrosilicon, molding sand, simple substance silicon, cement and the like, and is also used for manufacturing glaze and matrix of porcelain in ancient times, and common stone is mainly composed of silicon dioxide and calcium carbonate.
The hollow silica particles of the present invention have a shell having a mesoporous structure with an average pore diameter of 1 to 10nm, the hollow silica particles have an average particle diameter of 0.05 to 10 μm, and 80% or more of all the particles have a particle diameter within ± 30%, and the hollow silica particles have an advantage that the interior of the silica particles contains a hydrophobic organic compound or a polymeric organic compound, but the patent has a defect that the cleanliness of the silica particles is not high, so that the silica particles themselves have too many impurities, thereby increasing inconvenience in use and being inconvenient to use.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of silicon dioxide particles, which has the advantages of high cleanliness and the like, and solves the problems that the cleanliness of the silicon dioxide particles is not high, so that the impurities of the silicon dioxide particles are too much, the inconvenience and quickness in use are increased, and the use is inconvenient.
(II) technical scheme
In order to achieve the purpose of higher cleanliness, the invention provides the following technical scheme: a method of preparing silica particles comprising the steps of:
1) adding 1-50 parts of silicon dioxide slurry, 1-100 parts of hot solution, 3-90 parts of ethanolamine solution, 3-90 parts of aliphatic amine, 3-90 parts of aromatic amine solution and 3-90 parts of polyethyleneimine solution into a mixing and stirring reaction kettle, controlling the stirring time to be 1-2 hours, improving the overall temperature inside the reaction kettle to 250 ℃ by matching between mechanical stirring and materials, and placing the mixed materials in a standing device for later use;
2) placing the stewing device in the step 1) and the mixed material in an open place, and reducing the temperature of the material in the stewing device to 20-35 ℃ within 2-3 hours of natural time;
3) placing the cooled static device and the mixed material in the step 2) in a refrigerating chamber, controlling the freezing time to be 1.5-3.5 hours, then introducing the static and frozen mixed material into a centrifugal separator, separating water and sediment in the mixed material through centrifugal separation work for 1-2 hours, and placing the separated sediment in a container for later use;
4) putting the precipitate in the step 3) into a water washer, adding 1-100 parts of 18 megaohm water, wherein the stirring speed in the water washer is 150-400m/s, and the water washing time is controlled to be 2-3 hours, and then obtaining a wet precipitate water washing object;
5) placing the wet precipitate washed matter in the step 4) in a drying device for dewatering and drying, wherein the drying time is controlled to be 2-3 hours, and the drying temperature is controlled to be 200-400 ℃, and then obtaining a dry and anhydrous mixture;
6) putting the dried anhydrous mixture obtained in the step 5) into high-temperature air blowing equipment, then introducing purified gas, carrying out surface blowing on the dried anhydrous mixture, controlling the air temperature in the device at 200-500 ℃ for 1-1.5 hours, then obtaining silica particles with dust-free surfaces, packaging the silica particles into bags, putting the bags into a storage room, and placing the bags well to obtain the silica particles.
Preferably, the ethanolamine solution, the polyethyleneimine solution, the aliphatic amine and the aromatic amine solution can be replaced by one or more of an alkanolamine solution, an amide solution or a polyetherimide solution.
Preferably, the purified gas may comprise one or both of a halogen gas and a hydrogen halide gas.
Preferably, the hot solution is a hot aqueous solution of polytetrafluoroethylene.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of silicon dioxide particles, which has the following beneficial effects:
1. the preparation method of the silicon dioxide particles has the advantages that by adding the hot solution, the hot solution is the polytetrafluoroethylene hot solution, the polytetrafluoroethylene is a high molecular compound formed by polymerizing tetrafluoroethylene, the silicon dioxide particles have excellent chemical stability, corrosion resistance, sealing property, high lubrication non-adhesiveness, electric insulation property and good anti-aging endurance capacity, the chemical stability and the anti-endurance capacity of the silicon dioxide particles can be improved, by adding the silicon dioxide slurry into the hot solution, the melting of the silicon dioxide slurry and the mixing of materials can be accelerated, by adding the ethanolamine solution, the polyethyleneimine solution, the aliphatic amine and the aromatic amine solution, the four are matched to form the organic alkali solution, the organic alkali contains nitrogen atoms, by using the alkali solution, the condensation of the silicon dioxide slurry into a solid state can be accelerated, no metal substance needs to be added in the whole process, the efficiency of the preparation process of the silicon dioxide particles is improved, and the process is simplified, is convenient to use.
2. According to the preparation method of the silicon dioxide particles, solid-liquid separation is carried out on the silicon dioxide in a condensation state by using a centrifugal separator, 18 megaohm water, also called deionized water, is added, the pure water with impurities in an ionic form removed is high in cleanliness degree, the separated solid silicon dioxide is washed by using the 18 megaohm water, so that alkali in the solid silicon dioxide can be effectively removed again, and then the solid silicon dioxide is blown by using purified gas at high temperature, so that the impurities in the silicon dioxide particles can be effectively blown, the cleanliness of the silicon dioxide particles is integrally improved, the content of the impurities in the silicon dioxide particles is reduced, and the silicon dioxide particles are convenient to use.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a method of preparing silica particles comprising the steps of:
1) adding 1 part of silicon dioxide slurry, 1 part of hot solution, 3 parts of ethanolamine solution, 3 parts of aliphatine, 3 parts of aromatic amine solution and 3 parts of polyethyleneimine solution into a mixing and stirring reaction kettle, controlling the stirring time to be 1 hour, improving the overall temperature inside the reaction kettle to 100 ℃ through the cooperation between mechanical stirring and the materials, and placing the mixed materials in a standing device for later use;
2) placing the stewing device in the step 1) and the mixed material in an open place, and reducing the temperature of the material in the stewing device to 20 ℃ within 2 hours of natural time;
3) placing the cooled static device and the mixed material in the step 2) in a refrigerating chamber, controlling the freezing time to be 1.5 hours, then introducing the mixed material after static freezing into a centrifugal separator, separating water and sediment in the mixed material through centrifugal separation work for 1 hour, and placing the separated sediment in a container for later use;
4) putting the precipitate obtained in the step 3) into a water washer, adding 1 part of 18 megaohm water, wherein the stirring speed in the water washer is 150m/s, and the water washing time is controlled to be 2 hours, and then obtaining a wet precipitate water-washed object;
5) placing the wet precipitate washed matter in the step 4) in a drying device for dewatering and drying, wherein the drying time is controlled to be 2 hours, and the drying temperature is controlled to be 200 ℃, and then obtaining a dry anhydrous mixture;
6) putting the dried anhydrous mixture obtained in the step 5) into high-temperature air blowing equipment, then introducing purified gas, carrying out surface blowing on the dried anhydrous mixture, controlling the air temperature in the device to be 200 ℃ within 1 hour, then obtaining silica particles with dust-free surfaces, packaging the silica particles into bags, putting the bags into a storage room, and placing the bags well to obtain the silica particles.
Example two:
a method of preparing silica particles comprising the steps of:
1) adding 25.5 parts of silicon dioxide slurry, 50.5 parts of hot solution, 46.5 parts of ethanolamine solution, 46.5 parts of aliphatic amine, 46.5 parts of aromatic amine solution and 46.5 parts of polyethyleneimine solution into a mixing and stirring reaction kettle, controlling the stirring time to be 1.5 hours, improving the overall temperature inside the reaction kettle to 175 ℃ through the cooperation between mechanical stirring and materials, and placing the mixed materials in a standing device for later use;
2) placing the standing device in the step 1) and the mixed material in an open place, and reducing the temperature of the material in the standing device to 27.5 ℃ within 2.5 hours of natural time;
3) placing the cooled static device and the mixed material in the step 2) in a refrigerating chamber, controlling the freezing time to be 2.5 hours, then introducing the mixed material after static freezing into a centrifugal separator, separating water and sediment in the mixed material through centrifugal separation work for 1.5 hours, and placing the separated sediment in a container for later use;
4) putting the precipitate obtained in the step 3) into a water washer, adding 50.5 parts of 18 megaohm water, wherein the stirring speed in the water washer is 275m/s, and the water washing time is controlled to be 2.5 hours, and then obtaining a wet precipitate water-washed object;
5) placing the wet precipitate washed matter in the step 4) in a drying device for dewatering and drying, wherein the drying time is controlled to be 2.5 hours, and the drying temperature is controlled to be 300 ℃, and then obtaining a dry anhydrous mixture;
6) putting the dried anhydrous mixture obtained in the step 5) into high-temperature air blowing equipment, then introducing purified gas, carrying out surface blowing on the dried anhydrous mixture, controlling the air temperature in the device to be 350 ℃ for 1.25 hours, then obtaining silica particles with dust-free surfaces, packaging the silica particles into bags, putting the bags into a storage room, and placing the bags to obtain the silica particles.
Example three:
a method of preparing silica particles comprising the steps of:
1) adding 50 parts of silicon dioxide slurry, 100 parts of hot solution, 90 parts of ethanolamine solution, 90 parts of aliphatine, 90 parts of aromatic amine solution and 90 parts of polyethyleneimine solution into a mixing and stirring reaction kettle, controlling the stirring time to be 2 hours, improving the overall temperature inside the reaction kettle to 250 ℃ through the cooperation between mechanical stirring and the materials, and placing the mixed materials in a standing device for later use;
2) placing the standing device in the step 1) and the mixed material in an open place, and reducing the temperature of the material in the standing device to 35 ℃ within 3 hours of natural time;
3) placing the cooled static device and the mixed material in the step 2) in a refrigerating chamber, controlling the freezing time to be 3.5 hours, then introducing the mixed material after static freezing into a centrifugal separator, separating water and sediment in the mixed material through centrifugal separation work for 2 hours, and placing the separated sediment in a container for later use;
4) putting the precipitate in the step 3) into a water washer, adding 100 parts of 18 megaohm water, wherein the stirring speed in the water washer is 400m/s, and the water washing time is controlled to be 3 hours, and then obtaining a wet precipitate water-washed object;
5) placing the wet precipitate washed matter in the step 4) in a drying device for dewatering and drying, wherein the drying time is controlled to be 3 hours, and the drying temperature is controlled to be 400 ℃, and then obtaining a dry anhydrous mixture;
6) putting the dried anhydrous mixture obtained in the step 5) into high-temperature air blowing equipment, then introducing purified gas, carrying out surface blowing on the dried anhydrous mixture, controlling the air temperature in the device to be 500 ℃ within 1.5 hours, then obtaining silica particles with dust-free surfaces, packaging the silica particles into bags, putting the bags into a storage room, and placing the bags to obtain the silica particles.
The invention has the beneficial effects that: by adding the hot solution which is a polytetrafluoroethylene hot solution, the polytetrafluoroethylene is a high molecular compound formed by polymerizing tetrafluoroethylene, and has excellent chemical stability, corrosion resistance, sealing property, high lubrication non-stick property, electric insulation property and good ageing resistance, the chemical stability and the ageing resistance of the silicon dioxide particles can be improved, by adding the silicon dioxide slurry into the hot solution, the melting of the silicon dioxide slurry and the mixing of materials can be accelerated, by adding the ethanolamine solution, the polyethyleneimine solution, the aliphatic amine and the aromatic amine solution, the four are matched to form the organic alkali solution, the organic alkali contains nitrogen atoms, by using the alkali solution, the condensation of the silicon dioxide slurry into a solid state can be accelerated, no metal substance needs to be added in the whole process, the efficiency of the silicon dioxide particle preparation process is improved, and the process is simplified, the silicon dioxide cleaning device is convenient to use, solid-liquid separation is carried out on the silicon dioxide in a condensation state by using a centrifugal separator, 18 megaohm water is added, the 18 megaohm water is also called deionized water, pure water in an ion form after impurities are removed, the cleaning degree is high, the separated solid silicon dioxide is washed by using the 18 megaohm water, alkali in the solid silicon dioxide can be effectively removed again, then the solid silicon dioxide is blown by using purified gas at high temperature, impurities in silicon dioxide particles can be effectively blown, the cleanliness of the silicon dioxide particles is integrally improved, the content of the impurities in the silicon dioxide particles is reduced, and the silicon dioxide cleaning device is convenient to use.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A method for preparing silica particles, comprising the steps of:
1) adding 1-50 parts of silicon dioxide slurry, 1-100 parts of hot solution, 3-90 parts of ethanolamine solution, 3-90 parts of aliphatic amine, 3-90 parts of aromatic amine solution and 3-90 parts of polyethyleneimine solution into a mixing and stirring reaction kettle, controlling the stirring time to be 1-2 hours, improving the overall temperature inside the reaction kettle to 250 ℃ by matching between mechanical stirring and materials, and placing the mixed materials in a standing device for later use;
2) placing the stewing device in the step 1) and the mixed material in an open place, and reducing the temperature of the material in the stewing device to 20-35 ℃ within 2-3 hours of natural time;
3) placing the cooled static device and the mixed material in the step 2) in a refrigerating chamber, controlling the freezing time to be 1.5-3.5 hours, then introducing the static and frozen mixed material into a centrifugal separator, separating water and sediment in the mixed material through centrifugal separation work for 1-2 hours, and placing the separated sediment in a container for later use;
4) putting the precipitate in the step 3) into a water washer, adding 1-100 parts of 18 megaohm water, wherein the stirring speed in the water washer is 150-400m/s, and the water washing time is controlled to be 2-3 hours, and then obtaining a wet precipitate water washing object;
5) placing the wet precipitate washed matter in the step 4) in a drying device for dewatering and drying, wherein the drying time is controlled to be 2-3 hours, and the drying temperature is controlled to be 200-400 ℃, and then obtaining a dry and anhydrous mixture;
6) putting the dried anhydrous mixture obtained in the step 5) into high-temperature air blowing equipment, then introducing purified gas, carrying out surface blowing on the dried anhydrous mixture, controlling the air temperature in the device at 200-500 ℃ for 1-1.5 hours, then obtaining silica particles with dust-free surfaces, packaging the silica particles into bags, putting the bags into a storage room, and placing the bags well to obtain the silica particles.
2. The method for preparing silica particles according to claim 1, wherein the solution of ethanolamine, the solution of polyethyleneimine, the solution of aliphatic amine and the solution of aromatic amine can be replaced by one or more of the solution of alkanolamine, the solution of amide or the solution of polyetherimide.
3. The method of claim 1, wherein the purified gas comprises one or both of a halogen gas and a hydrogen halide gas.
4. The method of claim 1, wherein the hot solution is a hot aqueous solution of polytetrafluoroethylene.
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| CN201910242419.0A CN111747417A (en) | 2019-03-28 | 2019-03-28 | Preparation method of silicon dioxide particles |
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| CN201910242419.0A CN111747417A (en) | 2019-03-28 | 2019-03-28 | Preparation method of silicon dioxide particles |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1317401A (en) * | 1970-07-09 | 1973-05-16 | Grace W R & Co | Process for producing silica of high pore volume |
| CN101460400A (en) * | 2006-06-02 | 2009-06-17 | 德古萨诺瓦拉科技股份公司 | Pelletized silica |
| CN103114333A (en) * | 2012-12-18 | 2013-05-22 | 常州英中纳米科技有限公司 | Preparation method of monocrystalline spherical silicon dioxide particles |
| CN107512736A (en) * | 2017-09-11 | 2017-12-26 | 上海理工大学 | A kind of preparation method and applications of mesoporous SiO2/MoS2 materials |
-
2019
- 2019-03-28 CN CN201910242419.0A patent/CN111747417A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1317401A (en) * | 1970-07-09 | 1973-05-16 | Grace W R & Co | Process for producing silica of high pore volume |
| CN101460400A (en) * | 2006-06-02 | 2009-06-17 | 德古萨诺瓦拉科技股份公司 | Pelletized silica |
| CN103114333A (en) * | 2012-12-18 | 2013-05-22 | 常州英中纳米科技有限公司 | Preparation method of monocrystalline spherical silicon dioxide particles |
| CN107512736A (en) * | 2017-09-11 | 2017-12-26 | 上海理工大学 | A kind of preparation method and applications of mesoporous SiO2/MoS2 materials |
Non-Patent Citations (1)
| Title |
|---|
| 胡彦伟等: "化学沉淀法制备纳米SiO_2颗粒", 《化工学报》 * |
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Application publication date: 20201009 |