CN117843005A - Preparation method of nano silicon dioxide powder - Google Patents
Preparation method of nano silicon dioxide powder Download PDFInfo
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- CN117843005A CN117843005A CN202410013207.6A CN202410013207A CN117843005A CN 117843005 A CN117843005 A CN 117843005A CN 202410013207 A CN202410013207 A CN 202410013207A CN 117843005 A CN117843005 A CN 117843005A
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- silicon dioxide
- nano silicon
- dioxide powder
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 49
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 46
- 239000002243 precursor Substances 0.000 claims abstract description 40
- 239000002002 slurry Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 15
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 28
- 238000001556 precipitation Methods 0.000 claims description 16
- 235000019270 ammonium chloride Nutrition 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 8
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 239000000376 reactant Substances 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000001338 self-assembly Methods 0.000 abstract description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 description 14
- 238000001878 scanning electron micrograph Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 4
- 238000004626 scanning electron microscopy Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- -1 coatings Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of nano silicon dioxide powder. The method comprises the following steps: the sodium silicate solution and the precipitant solution are reacted, and a multi-interface reactor is used to synthesize the silicic acid precursor slurry. Washing, drying and calcining the silicic acid precursor slurry, and grinding to obtain the nano silicon dioxide powder with the particle size of 20-60nm and good uniformity. The nano silicon dioxide product prepared by the method is white powder, has good monodispersity, large specific surface area and small particle size. The method adopts a plurality of interface reactors to prepare the nano silicon dioxide, has controllable morphology and particle size, low industrialization cost, easy operation, energy conservation, environmental protection and low cost, and can realize large-scale continuous production; the nano silicon dioxide is prepared by adopting a multiphase interface reaction technology, so that all reaction liquid is separated into innumerable tiny liquid films by bubbles, reactants undergo self-assembly multiphase crystallization in the liquid films, nano-scale products can be generated, and the reaction conditions are mild.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of nano silicon dioxide powder.
Background
The nano silicon dioxide is amorphous white powder, is nontoxic, odorless and pollution-free, has a spherical microstructure and is in a flocculent and netlike quasi-particle structure. Has the characteristics of small particle size, high purity, low density, multiple micropores, large specific surface area, high surface hydroxyl content, strong ultraviolet, visible light and infrared reflecting capability and the like. And excellent stability, reinforcement, thixotropy and optical and mechanical properties, is unique in many disciplines and fields, and has an irreplaceable effect. The catalyst is widely used in various fields of additives, catalyst carriers, petrochemical industry, decolorizers, matting agents, rubber reinforcing agents, plastic fillers, coatings, medicines, environmental protection and the like in various industries.
Currently, the preparation method of nano silicon dioxide mainly comprises a dry method and a wet method, wherein the dry method comprises a gas phase decomposition method and an electric arc method, and the wet method comprises a chemical precipitation method, a gas phase deposition method, a sol-gel method, a microemulsion method and the like. However, both the gas phase method and the liquid phase precipitation method have the problems of high requirements on reaction equipment, complex process, high cost and the like. Other methods include combustion, sol-gel, carbonization, reverse micelle sol, and the like. Wherein, the preparation of superfine carbon dioxide by a carbonization reaction method has the defects of complex manufacturing process, low purity of products and the like. The combustion method has complex process; the particle size obtained by the precipitation method is large, and the structure is loose; the traditional sol-gel method has high heat treatment temperature, si-OH silanol groups on the surface of silicon dioxide are removed at high temperature, and the original particles are easy to agglomerate and grow up.
The nano silicon dioxide obtained by the preparation process has high purity and good performance, but has larger equipment investment, large energy consumption in the production process, high cost and difficult control of the reaction process.
Disclosure of Invention
Aiming at the technical problem of nano silicon dioxide powder preparation, the invention provides a preparation method of nano silicon dioxide powder, which has simple process, easy operation, low cost and continuous production; the preparation method of the invention is that all reaction liquid is separated into innumerable tiny liquid films by bubbles, reactants generate self-assembled multiphase crystallization in the liquid films, nano-scale products can be generated, and the reaction conditions are mild.
In order to achieve the above purpose, the preparation method of the nano silicon dioxide powder comprises the following implementation steps:
(1) Dissolving sodium silicate raw materials in water to prepare sodium silicate solution with the concentration of 0.4mol/L-0.7mol/L, preparing ammonium chloride raw materials into ammonium chloride solution with the concentration of 2-3.75mol/L, and adding 0.07mol/L surfactant;
(2) Adding the three-component solution obtained in the step (1) into a multiphase interface reactor for parallel flow precipitation reaction, wherein the stirring speed of the parallel flow precipitation reaction is 3000r/min, the flow is 300ml/min, and the temperature is room temperature, so as to obtain nano silicon dioxide precursor slurry;
(3) Aging the nano silicon dioxide precursor slurry obtained in the step (2) at the temperature of 25-80 ℃ for 1-4 hours to obtain the nano silicon dioxide precursor aging slurry;
(4) Washing and drying the aged nano silicon dioxide precursor slurry obtained in the step (3) at the drying temperature of 40-80 ℃ for 16-24 hours to obtain nano silicon dioxide precursor solid;
(5) Roasting the nano silicon dioxide precursor solid obtained in the step (4) at the temperature of 150-700 ℃ for 2-3 hours, and grinding to obtain 20-60nm nano silicon dioxide powder, wherein the nano silicon dioxide powder is spherical and has good uniformity.
The surfactant in the step (1) is cetyl trimethyl ammonium bromide or sodium oleate solution.
The concentration of the sodium silicate solution is 0.6mol/L.
The concentration of the ammonium chloride solution is 3.75mol/L.
The grinding step in the step (5) is grinding by a mortar to powder.
And (3) washing the aged slurry of the nano silicon dioxide precursor obtained in the step (3), wherein the solid-liquid ratio in the washing step is 1:10, and washing is carried out for 6 times at normal temperature by pure water.
Adding the three-component solution into a multiphase interface reactor for parallel flow precipitation reaction, wherein the stirring speed of the parallel flow precipitation reaction is 3000r/min, the flow is 300ml/min, and the stirring speed and the flow impact the reaction solution to form bubbles; all the reaction liquid is separated into innumerable fine liquid films by bubbles, and the reactants undergo self-assembled multiphase crystallization in the liquid films.
The preparation method of the nano silicon dioxide powder has the beneficial effects that:
1. the method adopts a plurality of interface reactors to prepare the nano silicon dioxide, has controllable morphology and particle size, low industrialization cost, easy operation, energy conservation, environmental protection, low cost and large-scale continuous production;
2. the invention adopts the multiphase interface reaction technology to prepare the nano silicon dioxide, so that all reaction liquid is separated into innumerable tiny liquid films by bubbles, the reactants undergo self-assembly multiphase crystallization in the liquid films, nano-scale products can be generated, and the reaction conditions are mild.
Drawings
FIG. 1 is a SEM image (scanning electron microscope image) of the nano-silica prepared in example 1;
FIG. 2 is a SEM image (scanning electron microscope image) of the nano-silica prepared in example 2;
FIG. 3 is a SEM image (scanning electron microscope image) of the nano-silica prepared in example 3;
FIG. 4 is a SEM image (scanning electron microscope image) of the nano-silica prepared in example 4;
FIG. 5 is an XRD pattern (X-ray diffraction pattern) of the nano-silica prepared in examples 1 to 4.
Detailed Description
Example 1: the preparation method of the nano silicon dioxide powder comprises the following implementation steps:
(1) Dissolving a sodium silicate raw material in water to prepare a sodium silicate solution with the concentration of 0.6mol/L, preparing an ammonium chloride raw material into an ammonium chloride solution with the concentration of 3.75mol/L, and adding a hexadecyl trimethyl ammonium bromide solution with the concentration of 0.07mol/L prepared from hexadecyl trimethyl ammonium bromide;
(2) Adding the three-component solution obtained in the step (1) into a multiphase interface reactor for parallel flow precipitation reaction, wherein the stirring speed of the parallel flow precipitation reaction is 3000r/min, the flow is 300ml/min, and the temperature is room temperature, so as to obtain nano silicon dioxide precursor slurry;
(3) Aging the nano silicon dioxide precursor slurry obtained in the step (2) at room temperature for 2 hours to obtain the nano silicon dioxide precursor aging slurry;
(4) Washing and drying the aged slurry of the nano silicon dioxide precursor obtained in the step (3), wherein the solid-liquid ratio in the washing step is 1:10, and washing is carried out for 6 times by pure water at normal temperature; the drying temperature is 70 ℃ and the drying time is 20 hours, so as to obtain nano silicon dioxide precursor solid;
(5) Roasting the nano silicon dioxide precursor solid obtained in the step (4) at the temperature of 700 ℃ for 3 hours, and grinding to obtain 20-60nm nano silicon dioxide powder, wherein the nano silicon dioxide powder is spherical and has good uniformity; as shown in SEM images (scanning electron microscopy images) of the nano-silica of fig. 1, as shown in XRD images (X-ray diffraction images) of the nano-silica of fig. 5.
Example 2: the preparation method of the nano silicon dioxide powder comprises the following implementation steps:
(1) Dissolving sodium silicate raw materials in water to prepare sodium silicate solution with the concentration of 0.4mol/L, preparing ammonium chloride raw materials into ammonium chloride solution with the concentration of 2.5mol/L, and adding sodium oleate solution with the concentration of 0.07 mol/L;
(2) Adding the three-component solution obtained in the step (1) into a multiphase interface reactor for parallel flow precipitation reaction, wherein the stirring speed of the parallel flow precipitation reaction is 3000r/min, the flow is 300ml/min, and the temperature is room temperature, so as to obtain nano silicon dioxide precursor slurry;
(3) Aging the nano silicon dioxide precursor slurry obtained in the step (2) at the temperature of 60 ℃ for 3 hours to obtain the nano silicon dioxide precursor aging slurry;
(4) Washing and drying the aged slurry of the nano silicon dioxide precursor obtained in the step (3), wherein the solid-liquid ratio in the washing step is 1:10, and washing is carried out for 6 times by pure water at normal temperature; the drying temperature is 50 ℃ and the drying time is 18 hours, so as to obtain nano silicon dioxide precursor solid;
(5) Roasting the nano silicon dioxide precursor solid obtained in the step (4) at the temperature of 500 ℃ for 2.5 hours, and grinding to obtain 40-60nm nano silicon dioxide powder, wherein the nano silicon dioxide powder is spherical and has good uniformity; as shown in SEM images (scanning electron microscopy images) of the nano-silica of fig. 2, as shown in XRD images (X-ray diffraction images) of the nano-silica of fig. 5.
Example 3: the preparation method of the nano silicon dioxide powder comprises the following implementation steps:
(1) Dissolving a sodium silicate raw material in water to prepare a sodium silicate solution with the concentration of 0.4mol/L, preparing an ammonium chloride raw material into an ammonium chloride solution with the concentration of 2.75mol/L, and adding a hexadecyl trimethyl ammonium bromide solution with the concentration of 0.07mol/L prepared from hexadecyl trimethyl ammonium bromide;
(2) Adding the three-component solution obtained in the step (1) into a multiphase interface reactor for parallel flow precipitation reaction, wherein the stirring speed of the parallel flow precipitation reaction is 3000r/min, the flow is 300ml/min, and the temperature is room temperature, so as to obtain nano silicon dioxide precursor slurry;
(3) Aging the nano silicon dioxide precursor slurry obtained in the step (2) at the temperature of 25 ℃ for 4 hours to obtain the nano silicon dioxide precursor aging slurry;
(4) Washing and drying the aged slurry of the nano silicon dioxide precursor obtained in the step (3), wherein the solid-liquid ratio in the washing step is 1:10, and washing is carried out for 6 times by pure water at normal temperature; the drying temperature is 40 ℃ and the drying time is 24 hours, so as to obtain nano silicon dioxide precursor solid;
(5) Roasting the nano silicon dioxide precursor solid obtained in the step (4) at the temperature of 500 ℃ for 3 hours, and grinding to obtain 20-50nm nano silicon dioxide powder, wherein the nano silicon dioxide powder is spherical and has good uniformity; as shown in SEM images (scanning electron microscopy images) of the nano-silica of fig. 3, as shown in XRD images (X-ray diffraction images) of the nano-silica of fig. 5.
Example 4:
the preparation method of the nano silicon dioxide powder comprises the following implementation steps:
(1) Dissolving a sodium silicate raw material in water to prepare a sodium silicate solution with the concentration of 0.7mol/L, preparing an ammonium chloride raw material into an ammonium chloride solution with the concentration of 3.75mol/L, and adding a hexadecyl trimethyl ammonium bromide solution with the concentration of 0.07mol/L prepared from hexadecyl trimethyl ammonium bromide;
(2) Adding the three-component solution obtained in the step (1) into a multiphase interface reactor for parallel flow precipitation reaction, wherein the stirring speed of the parallel flow precipitation reaction is 3000r/min, the flow is 300ml/min, and the temperature is room temperature, so as to obtain nano silicon dioxide precursor slurry;
(3) Aging the nano silicon dioxide precursor slurry obtained in the step (2) at the temperature of 80 ℃ for 1h to obtain the nano silicon dioxide precursor aging slurry;
(4) Washing and drying the aged slurry of the nano silicon dioxide precursor obtained in the step (3), wherein the solid-liquid ratio in the washing step is 1:10, and washing is carried out for 6 times by pure water at normal temperature; the drying temperature is 80 ℃ and the drying time is 16 hours, so as to obtain nano silicon dioxide precursor solid;
(5) Roasting the nano silicon dioxide precursor solid obtained in the step (4) at the temperature of 700 ℃ for 2 hours, and grinding to obtain 20-60nm nano silicon dioxide powder, wherein the nano silicon dioxide powder is spherical and has good uniformity; as shown in SEM images (scanning electron microscopy images) of the nano-silica of fig. 1, as shown in XRD images (X-ray diffraction images) of the nano-silica of fig. 5.
Claims (6)
1. A preparation method of nano silicon dioxide powder is characterized in that: the implementation steps are as follows:
(1) Dissolving sodium silicate raw materials in water to prepare sodium silicate solution with the concentration of 0.4mol/L-0.7mol/L, preparing ammonium chloride raw materials into ammonium chloride solution with the concentration of 2-3.75mol/L, and adding 0.07mol/L surfactant;
(2) Adding the three-component solution obtained in the step (1) into a multiphase interface reactor for parallel flow precipitation reaction, wherein the stirring speed of the parallel flow precipitation reaction is 3000r/min, the flow is 300ml/min, and the temperature is room temperature, so as to obtain nano silicon dioxide precursor slurry;
(3) Aging the nano silicon dioxide precursor slurry obtained in the step (2) at the temperature of 25-80 ℃ for 1-4 hours to obtain the nano silicon dioxide precursor aging slurry;
(4) Washing and drying the aged nano silicon dioxide precursor slurry obtained in the step (3) at the drying temperature of 40-80 ℃ for 16-24 hours to obtain nano silicon dioxide precursor solid;
(5) Roasting the nano silicon dioxide precursor solid obtained in the step (4) at the temperature of 150-700 ℃ for 2-3 hours, and grinding to obtain 20-60nm nano silicon dioxide powder, wherein the nano silicon dioxide powder is spherical and has good uniformity.
2. The method for preparing nano silicon dioxide powder according to claim 1, wherein: the surfactant in the step (1) is cetyl trimethyl ammonium bromide or sodium oleate solution.
3. The method for preparing nano silicon dioxide powder according to claim 1, wherein: the concentration of the sodium silicate solution is 0.6mol/L.
4. The method for preparing nano silicon dioxide powder according to claim 1, wherein: the concentration of the ammonium chloride solution is 3.75mol/L.
5. The method for preparing nano silicon dioxide powder according to claim 1, wherein: the grinding step in the step (5) is grinding by a mortar to powder.
6. The method for preparing nano silicon dioxide powder according to claim 1, wherein: and (3) washing the aged slurry of the nano silicon dioxide precursor obtained in the step (3), wherein the solid-liquid ratio in the washing step is 1:10, and washing is carried out for 6 times at normal temperature by pure water.
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| CN202410013207.6A CN117843005A (en) | 2024-01-04 | 2024-01-04 | Preparation method of nano silicon dioxide powder |
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