CN112811431A - High-throughput preparation method of monodisperse silicon dioxide microspheres - Google Patents
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 18
- 239000004005 microsphere Substances 0.000 title abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 4
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000011858 nanopowder Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 18
- 238000000034 method Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 239000007795 chemical reaction product Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000007832 Na2SO4 Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention relates to the technical field of preparation of nano powder materials, and discloses a high-flux preparation method of monodisperse silicon dioxide microspheres, wherein the silicon dioxide microspheres are prepared based on a microfluidic reactor, the microfluidic reactor comprises a reaction chamber, a multichannel spiral tube comprising at least one spiral tube is arranged in the reaction chamber, and the preparation method comprises the following steps: 1) dispersing a silicon source in a solvent to obtain a first solution; 2) dispersing a catalyst in deionized water to obtain a second solution; 3) inputting the first solution and the second solution from an inlet channel of the reaction chamber at the same time, and mixing to obtain a mixed solution; 4) and (3) reacting the mixed solution in each spiral pipe of the multi-channel spiral pipe, and separating and purifying to obtain the silicon dioxide with different particle sizes. The invention adopts a multi-flux microfluidic reaction system, so that the particle size distribution of the synthesized silicon dioxide is uniform, the production quantity of different particle sizes is greatly increased, and the production efficiency is improved.
Description
Technical Field
The invention relates to the technical field of preparation of nano powder materials, in particular to a high-flux preparation method of monodisperse silicon dioxide microspheres.
Background
Silica is one of the most important high-tech inorganic new materials, and has irreplaceable effects in the field of electronic packaging due to good performances in the aspects of dispersibility, thermal stability, insulativity and the like. Especially, the silica with different sizes shows different optical and chemical characteristics, so that the controllable synthesis of the silica with different sizes is of great significance.
Currently, there are three main methods for industrially preparing silica: gas phase processes, precipitation processes and sol-gel processes. By gas phase processes with silicon-containing halides (e.g. SiCl)4) As a raw material, silica particles are generated by high temperature in oxyhydrogen flame. The silicon dioxide prepared by the method has low surface hydroxyl content and good quality, but the process is complex and the cost is high. The precipitation method uses water glass and sulfuric acid as raw materials, and the raw materials react in a solution, and then the silicon dioxide is obtained through precipitation, filtration, washing, drying and calcination. The preparation method has simple operation and low cost, thereby being widely applied. But will produce a large amount of Na2SO4Waste water is difficult to treat and recycle, and in addition, in the reaction process, the reactant mixing efficiency is low, the mixing is not uniform, the controllability is poor, and the monodisperse silicon dioxide with uniform particle size is difficult to obtain. Sol-gel process with organosiliconate [ Si (OR)4]Hydrolyzing in acid or alkali alcohol solution to generate silica sol, and carrying out post-treatment such as centrifugal washing, drying, calcining and the like to obtain the spherical silica. The silicon dioxide prepared by the method has small and uniform particle size.
In the prior art, the silica is prepared by a sol-gel method, a stirring reaction kettle is used, the reaction space is too large, the mixing efficiency is low, the particle size distribution is wide, and the monodisperse silica is difficult to form; the single-channel microfluidic reaction system can control the uniformity of the particle size, but the reaction efficiency is low.
Disclosure of Invention
Based on the problems, the invention provides a high-throughput preparation method of monodisperse silica microspheres based on a microfluidic reactor, which can realize high-throughput preparation of silica with various monodisperse particle sizes through the adjustable multi-channel design of the microfluidic reactor, can controllably synthesize silica with different particle sizes and excellent monodisperse performance, and increase the production rate through multiple fluxes; the silicon dioxide powder obtained by the invention has uniform particle size and improves the production efficiency.
The invention adopts a multi-flux microfluidic reaction system, so that the particle size distribution of the synthesized silicon dioxide is uniform, the production quantity of different particle sizes is greatly increased, and the production efficiency is improved.
The invention provides a high-flux preparation method of monodisperse silicon dioxide microspheres, wherein the silicon dioxide microspheres are prepared based on a microfluidic reactor, the microfluidic reactor comprises a reaction chamber, and a multichannel spiral tube comprising at least one spiral tube is arranged in the reaction chamber, and the preparation method comprises the following steps:
1) dispersing a silicon source in a solvent to obtain a first solution;
2) dispersing a catalyst in deionized water to obtain a second solution;
3) simultaneously inputting a first solution and a second solution from an inlet channel of a reaction chamber according to a certain volume ratio, and mixing to obtain a mixed solution;
4) and (3) reacting the mixed solution in each spiral pipe of the multi-channel spiral pipe, and separating and purifying to obtain the silicon dioxide with different particle sizes.
According to the technical scheme, the first solution and the second solution are simultaneously and respectively input from two different inlet ends of the reaction chamber through the constant flow pump, are rapidly mixed through the inlet channels and then enter and are distributed into each spiral tube channel of the multi-channel spiral tube to be reacted, the outlet of each spiral tube channel is correspondingly communicated with the outlet channel, and the reaction liquid after the reaction is finished is collected into the product collector through the distributed outlet channels.
In the technical scheme of the invention, each spiral pipe of the multichannel spiral pipe is 15-150m long, and the inner diameter is 0.5-1.5 mm.
In the technical scheme of the invention, the mass ratio of the silicon source to the solvent is 0.1-1; the mass ratio of the catalyst dispersed in the deionized water is 0.1-1;
preferably, the volume ratio of the first solution to the second solution is 1 to 2.
In the technical scheme of the invention, the input speed of the first solution from the inlet end of the reaction chamber is 0.1-10mL/min, and the input speed of the second solution from the inlet end of the reaction chamber is 0.1-10 mL/min.
In the technical scheme of the invention, the multichannel spiral tube is placed in a thermostatic bath at 25-60 ℃.
In the technical scheme of the invention, the silicon source is selected from one or a mixture of more of ethyl orthosilicate, methyl orthosilicate, gamma-mercaptopropyl-trimethoxysilane and gamma- (methacryloyloxy) propyl-trimethoxysilane.
In the technical scheme of the invention, the solvent is one or a mixture of several of methanol, ethanol, propanol, isopropanol and n-butanol.
In the technical scheme of the invention, the catalyst is selected from one or a mixture of more of sodium bicarbonate, sodium hydroxide, potassium hydroxide, ammonia water and hydrochloric acid.
In the technical scheme of the invention, in the step 4), the reaction time is 0.2-4 h.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the multichannel spiral tube comprising at least one spiral tube is designed in the reaction chamber, the silicon dioxide with different particle sizes and excellent monodispersity can be controllably synthesized by controlling the number, diameter, length and the like of the spiral tubes, and the production rate is increased by multiple fluxes; the invention adopts a multi-flux microfluidic reaction system, so that the particle size distribution of the synthesized silicon dioxide is uniform, the production quantity of different particle sizes is greatly increased, and the production efficiency is improved.
Drawings
Fig. 1 is a schematic diagram of a microfluidic reactor used in the present invention for preparing silica microspheres.
FIG. 2 is an SEM photograph of a spherical nano-silica material prepared in example 1 of the present invention, wherein (a) is a SEM photograph of silica powder obtained by reaction of a spiral tube having a length of 120m and an inner diameter of 0.7mm, and (b) is a SEM photograph of silica powder obtained by reaction of a spiral tube having a length of 70m and an inner diameter of 1.2 mm;
FIG. 3 is an SEM photograph of a spherical nano-silica material prepared in example 2 of the present invention, wherein (a) is a SEM photograph of silica powder obtained by reaction of a spiral tube having a length of 150m and an inner diameter of 0.5mm, and (b) is a SEM photograph of silica powder obtained by reaction of a spiral tube having a length of 90m and an inner diameter of 1.0 mm;
FIG. 4 is an SEM photograph of a spherical nano-silica material prepared in example 3 of the present invention, wherein (a) is an SEM photograph of silica powder obtained by a reaction in a spiral tube having a length of 20m and an inner diameter of 0.5mm, and (b) is an SEM photograph of silica powder obtained by a reaction in a spiral tube having a length of 150m and an inner diameter of 1.5 mm.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
in the following examples, a high throughput preparation method of monodisperse silica microspheres, which were prepared based on a microfluidic reactor, as shown in fig. 1, the microfluidic reactor comprises a reaction chamber and a product collector, wherein a multichannel spiral pipe comprising at least one spiral pipe is arranged in the reaction chamber, heat conducting oil is arranged in the reaction chamber, the reaction chamber is arranged in a constant temperature bath at 25-60 ℃, the reaction chamber is provided with two different inlet ends for inputting, a constant flow pump is arranged on the inlet end, a first solution prepared from a silicon source and a second solution prepared from a catalyst are simultaneously input from two different inlet ends of a reaction chamber through a constant flow pump, mixed by inlet channels and then enter and are distributed into each spiral tube channel of a multi-channel spiral tube to react, the outlet of each spiral tube channel is correspondingly communicated with an outlet channel, and reaction liquid after the reaction is finished is collected into a product collector through the distributed outlet channels.
Wherein, each spiral pipe of the multi-channel spiral pipe is 15-150m long, and the inner diameter is 0.5-1.5 mm.
Example 1:
the high-throughput preparation method of the monodisperse silica microsphere of the embodiment comprises the following steps:
step 4, enabling the mixed solution to pass through two spiral pipes which are respectively 120m long, 0.7mm inner diameter and 70m long and 1.2mm inner diameter, placing the spiral pipes in a square groove at 40 ℃ for reaction, wherein the reaction time is 0.5h, and after the reaction is finished, collecting the two spiral pipes into a product collector through corresponding outlet channels to obtain two emulsions;
5. and (3) carrying out vacuum filtration on the reaction product, washing the reaction product for 3 times by using pure water and ethanol respectively, and carrying out vacuum drying at 50 ℃ to obtain the final silicon dioxide powder.
6. The following were obtained by measurement: the silica powder obtained by the reaction in a spiral tube having a length of 120m and an inner diameter of 0.7mm had a particle size of 300nm, and the SEM image of the obtained silica powder is shown in FIG. 2 (a); SEM image of the silica powder obtained by reacting silica powder having a particle size of 450nm with a spiral tube having a length of 70m and an inner diameter of 1.2mm is shown in FIG. 2 (b).
Example 2:
the high-throughput preparation method of the monodisperse silica microsphere of the embodiment comprises the following steps:
step 4, the mixed solution is processed through two spiral pipes with the length of 150m, the inner diameter of 0.5mm and the length of 90m and the inner diameter of 1.0mm, the spiral pipes are placed in a square groove with the temperature of 30 ℃ for reaction, and the reaction time is 0.8h to obtain two emulsions;
and 5, carrying out vacuum filtration on the reaction product, washing the reaction product for 3 times by using pure water and ethanol respectively, and carrying out vacuum drying at 50 ℃ to obtain the final silicon dioxide powder.
And 6, obtaining the following through measurement: the silica powder obtained by the reaction in a spiral tube having a length of 150m and an inner diameter of 0.5mm had a particle size of 400nm, and the SEM image of the obtained silica powder is shown in FIG. 3 (a); SEM image of the silica powder obtained by reacting silica powder having a particle size of 900nm with a spiral tube having a length of 90m and an inner diameter of 1.0mm is shown in FIG. 3 (b).
Example 3:
the high-throughput preparation method of the monodisperse silica microsphere of the embodiment comprises the following steps:
step 4, the mixed solution is processed through two spiral pipes with the length of 150m, the inner diameter of 0.5mm and the length of 30m and the inner diameter of 1.5mm, the spiral pipes are placed in a square groove with the temperature of 50 ℃ for reaction, and the reaction time is 2 hours, so that two emulsions are obtained;
and 5, carrying out vacuum filtration on the reaction product, washing the reaction product for 3 times by using pure water and ethanol respectively, and carrying out vacuum drying at 50 ℃ to obtain the final silicon dioxide powder.
And 6, obtaining the following through measurement: the silica powder obtained by the reaction in a spiral tube having a length of 20m and an inner diameter of 0.5mm had a particle size of 350nm, and the SEM image of the obtained silica powder is shown in FIG. 4 (a); SEM image of the silica powder obtained by reacting silica powder having a particle size of 800nm with a spiral tube having a length of 150m and an inner diameter of 1.5mm is shown in FIG. 4 (b).
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A high-flux preparation method of monodisperse silica microspheres is characterized in that the silica microspheres are prepared based on a microfluidic reactor, the microfluidic reactor comprises a reaction chamber, and a multichannel spiral tube comprising at least one spiral tube is arranged in the reaction chamber, and the preparation method comprises the following steps:
1) dispersing a silicon source in a solvent to obtain a first solution;
2) dispersing a catalyst in deionized water to obtain a second solution;
3) simultaneously inputting a first solution and a second solution from an inlet channel of a reaction chamber according to a certain volume ratio, and mixing to obtain a mixed solution;
4) and (3) reacting the mixed solution in each spiral pipe of the multi-channel spiral pipe, and separating and purifying to obtain the silicon dioxide with different particle sizes.
2. The high-flux preparation method of the monodisperse silica microspheres according to claim 1, wherein the first solution and the second solution are simultaneously and respectively input from two different inlet ends of the reaction chamber through a constant flow pump, are rapidly mixed through an inlet channel, enter and are distributed into each spiral tube channel of the multi-channel spiral tube for reaction, an outlet channel is correspondingly communicated with an outlet of each spiral tube channel, and the reaction solution after the reaction is completed is collected into a product collector through the distributed outlet channels.
3. The high throughput preparation method of monodisperse silica microspheres according to claim 2, wherein each spiral tube of the multi-channel spiral tube has a length of 15-150m and an inner diameter of 0.5-1.5 mm.
4. The high-throughput preparation method of monodisperse silica microspheres according to claim 1, wherein the mass ratio of the silicon source to the solvent is 0.1-1; the mass ratio of the catalyst dispersed in the deionized water is 0.1-1;
preferably, the volume ratio of the first solution to the second solution is 1 to 2.
5. The high throughput preparation method of monodisperse silica microspheres according to claim 1, wherein the first solution is fed at a rate of 0.1-10mL/min from the inlet end of the reaction chamber, and the second solution is fed at a rate of 0.1-10mL/min from the inlet end of the reaction chamber.
6. The high-throughput preparation method of monodisperse silica microspheres according to claim 1, wherein the multichannel spiral tube is placed in a thermostatic bath at 25-60 ℃.
7. The high-throughput preparation method of monodisperse silica microspheres according to claim 1, wherein the silicon source is selected from one or more of ethyl orthosilicate, methyl orthosilicate, gamma-mercaptopropyl trimethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane.
8. The high-throughput preparation method of monodisperse silica microspheres according to claim 1, wherein the solvent is selected from one or a mixture of methanol, ethanol, propanol, isopropanol and n-butanol.
9. The high-throughput preparation method of monodisperse silica microspheres, according to claim 1, wherein the catalyst is selected from one or more of sodium bicarbonate, sodium hydroxide, potassium hydroxide, ammonia water and hydrochloric acid.
10. The high-throughput preparation method of monodisperse silica microspheres according to claim 1, wherein in step 4), the reaction time is 0.2-4 h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113277522A (en) * | 2021-06-17 | 2021-08-20 | 航天特种材料及工艺技术研究所 | Light silica aerogel with ultrahigh transparency and ultralow haze, and preparation method and application thereof |
| CN113444274A (en) * | 2021-07-16 | 2021-09-28 | 宁夏清研高分子新材料有限公司 | Low dielectric liquid crystal polymer resin and preparation method and application thereof |
| CN115337920A (en) * | 2022-08-15 | 2022-11-15 | 诺丁汉大学卓越灯塔计划(宁波)创新研究院 | Catalyst carrier and preparation method thereof |
| CN115818652A (en) * | 2022-11-23 | 2023-03-21 | 中国科学院深圳先进技术研究院 | Silicon dioxide filler for chip-level underfill adhesive and preparation method and application thereof |
| CN116986603A (en) * | 2023-09-26 | 2023-11-03 | 中南大学 | Method for preparing spherical nano silicon dioxide by utilizing fluorosilicate |
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| CN108117083A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of method of continuous controllable preparation nano silicon dioxide spheric granules |
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