阅读说明：本技术 一种二氧化硅颗粒的制备方法 (Preparation method of silicon dioxide particles ) 是由 许荣明 于 2019-03-28 设计创作，主要内容包括：本发明涉及二氧化硅颗粒技术领域,且公开了一种二氧化硅颗粒的制备方法,包括以下步骤：1)将二氧化硅浆料1-50份、热溶液1-100份、乙醇胺溶液3-90份、入脂肪胺3-90份、芳香胺溶液3-90份和聚乙烯亚胺溶液3-90份加入到混合搅拌反应釜中,搅拌的时间控制在1-2小时,通过机械搅拌与物料之间的配合,使得反应釜内部的整体温度提高到100-250摄氏度,将混合后的物料放置在静置器内以备使用；2)将步骤1)中的静置器连同混合物料放置在空旷处,在自然时间2-3小时内,使得静置器内的物料温度下降至20-35摄氏度。该二氧化硅颗粒的制备方法,通过使用纯化气体对固态二氧化硅进行吹拂工作,整体提高了二氧化硅颗粒的洁净度,使其内部的杂质含量降低,方便使用。(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.)

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.

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.