CN117680059A - Method for continuously preparing hydrophobic aerogel powder by double-fluid atomization - Google Patents
Method for continuously preparing hydrophobic aerogel powder by double-fluid atomization Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 40
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- 239000012530 fluid Substances 0.000 title claims abstract description 35
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 23
- 238000000889 atomisation Methods 0.000 title claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 26
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- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 239000005046 Chlorosilane Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 2
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- DRUOQOFQRYFQGB-UHFFFAOYSA-N ethoxy(dimethyl)silicon Chemical compound CCO[Si](C)C DRUOQOFQRYFQGB-UHFFFAOYSA-N 0.000 claims description 2
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 2
- MDLRQEHNDJOFQN-UHFFFAOYSA-N methoxy(dimethyl)silicon Chemical compound CO[Si](C)C MDLRQEHNDJOFQN-UHFFFAOYSA-N 0.000 claims description 2
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 2
- QALDFNLNVLQDSP-UHFFFAOYSA-N triethoxy-(2,3,4,5,6-pentafluorophenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=C(F)C(F)=C(F)C(F)=C1F QALDFNLNVLQDSP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000499 gel Substances 0.000 abstract description 22
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- 239000003960 organic solvent Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000000352 supercritical drying Methods 0.000 description 4
- 239000011240 wet gel Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- 239000003292 glue Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
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- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- ZXVOCOLRQJZVBW-UHFFFAOYSA-N azane;ethanol Chemical compound N.CCO ZXVOCOLRQJZVBW-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention relates to the field of hydrogel preparation methods, in particular to a method for continuously preparing hydrophobic aerogel powder by double-fluid atomization. The invention relates to a method for continuously preparing hydrophobic aerogel powder by double-fluid atomization, which comprises the following steps: a) Preparing a sol and a gel catalyst; b) Uniformly mixing the sol and the gel catalyst through a two-fluid nozzle, and atomizing into small liquid drops; c) The atomized droplets form gel particles; d) Drying the solvent in the gel particles under reduced oxygen. According to the invention, sol and catalyst are sprayed out through a two-fluid nozzle by a two-fluid atomization technology, and after the two fluids are atomized, the two fluids are mutually impacted and mixed to form small liquid drops; the droplets are rapidly heated in a spray dryer to form gel particles.
Description
Technical Field
The invention relates to the field of hydrogel preparation methods, in particular to a method for continuously preparing hydrophobic aerogel powder by double-fluid atomization.
Background
Aerogel has a three-dimensional network structure composed of unique nano holes and nano frameworks in the 30 s of the 19 th century, has many properties incomparable with those of traditional materials, and has excellent properties such as porosity, specific surface area, refractive index and thermal conductivity, so that the aerogel has wide application in the fields of materials such as catalysis, insulation and heat insulation.
Also, due to the unique nano-pore structure of aerogel, when solvent comes out from the pores, the gel skeleton is subjected to huge surface tension, and in order to keep the pore structure from collapsing, a supercritical drying method or an atmospheric drying method is often adopted. Wherein, supercritical drying eliminates the surface tension of pore liquid, and can keep pore structure from deformation due to capillary force during drying. However, supercritical drying generally requires high temperature and high pressure (CO 2 critical temperature is about 31 ℃, the pressure is about 7.3 MPa, the ethanol critical temperature is 243.1 ℃, the pressure is 6.3MPa, and the actual production process parameters are far higher than the critical value), so that the method becomes the bottleneck of large-scale production due to the characteristics of high process equipment dependence, high cost and the like.
The existing normal pressure drying process mostly needs to modify the surface of the gel skeleton, and uses a solvent with low surface tension for replacement, so that shrinkage stress caused by capillary force is reduced, the skeleton collapse is avoided, but the modification process is long, the organic solvent usage amount in the replacement process is large, and the cost is high. The biggest problem of supercritical drying and normal pressure drying is that both processes are intermittent production, wet gel is hung into a kettle, a drying process is completed in a sealed state, and the wet gel is hung out after the drying is completed. The intermittent production method limits the productivity of the aerogel, and the control of the production process and the consistency of products are difficult to ensure. Therefore, continuous production of aerogel materials is always one of the directions of research of experts at home and abroad.
Patent CN 205925659U discloses a continuous production device of aerogel powder, which comprises five parts, namely a drying process, a solvent recovery process, a crushing process, a powder collection process and an automatic packaging process. The wet gel enters a drying kettle through a feed inlet, and is uniformly dried and primarily crushed under the heating action of the resistance wire and the stirring action of the stirring paddle; conveying the dried aerogel to a crushing device, and crushing by adopting an air flow mill to obtain aerogel powder. In the drying process, after wet gel enters the drying kettle, the whole kettle material can be conveyed out after being dried, and in fact, the method is still a semi-continuous process, only the automatic conveying among kettles is solved, and in the drying process, a large amount of organic matters are heated through resistance wires and stirred through stirring paddles, so that great potential safety hazards exist.
Patent CN109529735B discloses a method for continuously preparing aerogel composite material by microwave equipment, the aerogel precursor and fiber are compounded to form gel, and then the gel is transferred to a solvent replacement, a hydrophobic modification device and a drying device in sequence by a conveyor belt, and finally the finished product is obtained. The method can realize continuous production of the composite material, but a large amount of inflammable and explosive organic solvents are stored in the solvent replacement and hydrophobic modification devices, the gel is filled and discharged in each device by pushing up the baffle plate by the material, the gel material and the conveyor belt are continuously moved, the solvent or the organic gas is easy to leak due to too small contact force between the baffle plate and the material, and the gel with too large contact force is damaged; in addition, in order to accelerate the speed and safety of each procedure, nano wave absorbing factors are required to be added into the aerogel, flame retardants are required to be added into the solvent, and metal impurities in the fiber materials are required to be inspected so as to avoid ignition in a microwave device, thus the cost and difficulty of aerogel production are obviously increased, and large-scale production cannot be performed.
Patent CN103408028B provides a production process of silica gel as super heat insulating material, which comprises the steps of hydrogel preparation, organogel generation, double-tower distillation, hydrophobization treatment, spray drying, product detection and the like. The main technology is that hydrogel is cut into pieces, put into a distillation kettle, and water in the hydrogel is replaced by azeotropic organic matters through distillation; the gel containing the organic azeotrope is subjected to filter pressing to recover organic matters, and after the filter cake is pulped, a silane coupling agent is added for hydrophobization treatment, and then the mixture is pumped into a spray dryer for drying. The technology has the problems that 1) the filter pressing and pulping processes contain a large amount of organic solvents, all the processes need to be carried out in an anaerobic environment, otherwise, the danger coefficient is large, the equipment is required to be customized explosion-proof equipment, and the investment is high; 2) In the filter pressing process, the organic solvent comes out of the nano-pores of the gel, capillary force exists as well, and the framework structure of the gel can still be damaged; 3) The feeding and discharging materials in the distillation process are also intermittent and cannot be continuously produced; 4) The gel slurry easily plugs the dryer feed inlet.
Disclosure of Invention
The invention hopes to provide a method for continuously preparing hydrophobic aerogel powder by double-fluid atomization, which comprises the following specific scheme:
a method for continuously preparing hydrophobic aerogel powder by double-fluid atomization, which comprises the following steps:
a) Preparing a sol and a gel catalyst;
b) Uniformly mixing the sol and the gel catalyst through a two-fluid nozzle, and atomizing into small liquid drops;
c) The atomized droplets form gel particles;
d) Drying the solvent in the gel particles under reduced oxygen.
The sol in the step a) comprises one or more of silica, alumina, titanium oxide and zirconia sol; the gel catalyst is one or more of acid, alkali and electrolyte.
The sol in the step a) comprises a low-surface tension solvent, wherein the low-surface tension solvent is one or more of methanol, ethanol, acetone, butanone, n-hexane, hexamethyldisiloxane and hexamethyldisilazane.
The pH of the small liquid drops in the step b) is 4.8-10.0, and the gel time in the step c) is 1-120s.
The atomization in step b) is performed in an environment with an oxygen concentration of less than 3%.
The drying temperature in the step d) is 30-200 ℃ and the pressure is normal pressure.
The drying mode in the step d) is hot air circulation drying, and the drying mode comprises a fluid heating unit (the heat source for fluid heating is one or more of steam, electricity, microwaves, air energy and geothermal energy), a hot air circulation unit, a powder separation unit and a fluid recovery unit.
The hot air circulation unit circulates the dried hot air, and the hot air medium comprises inert gas and hydrophobizing agent.
The hydrophobizing reagent is one or more of gas-phase siloxane reagents, silazane reagents and chlorosilane reagents; the inert gas is nitrogen and/or carbon dioxide.
The siloxane hydrophobizing agent is one or more of hexamethyldisiloxane, trimethylmethoxysilane, trimethylethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethylmethoxysilane, dimethylethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, phenyltriethoxysilane and pentafluorophenyltriethoxysilane.
According to the invention, sol and catalyst are sprayed out through a two-fluid nozzle by a two-fluid atomization technology, and after the two fluids are atomized, the two fluids are mutually impacted and mixed to form small liquid drops; the droplets are rapidly heated in a spray dryer to form gel particles; the small particles are contacted with inert gas containing a higher concentration of hydrophobizing agent, on one hand, the hydrophobizing modification of the silicon hydroxyl groups is rapidly completed, and on the other hand, part of the solvent with high surface tension in the small particles is rapidly replaced by the hydrophobizing agent with low surface tension; when the gel particles fall to a certain height, the concentration of the hydrophobizing agent in the environment becomes low, and the solvent and the hydrophobizing agent in the holes are carried out by inert gas to form dry and hydrophobic aerogel particles. And collecting the particles according to different particle sizes in a gravity separation or centrifugal separation mode to obtain aerogel powder with uniform particle sizes.
The invention has the following advantages:
1. a truly continuous production can be achieved.
2. The invention only needs normal pressure, so the equipment only needs normal pressure equipment, and the material inlet and outlet are easily sealed by flange connection.
3. The production process is simple, and better aerogel particle size distribution and drying effect can be obtained.
4. The production equipment is in an inert gas environment, and the organic hydrophobizing reagent exists in a saturated steam state, so that the reagent amount is small, the energy consumption is low, and the production efficiency is high.
5. By selecting an appropriate atomizer and using process parameters, the droplet size range can be controlled between 10 and 500 μm, and the requirements of different fields and applications can be met.
Drawings
FIG. 1 is a schematic illustration of a method for continuously preparing hydrophobic aerogel powders by two-fluid atomization in accordance with the present invention.
Detailed Description
Example 1
a) Preparing silica sol, wherein the solvent is methanol, and the gel catalyst is methanol solution of NaOH;
b) After the spray dryer is replaced by nitrogen and heated, the oxygen concentration is lower than 3%, and the temperature is 120+/-5 ℃;
atomizing the silica-methanol sol and the gel catalyst according to the proportion of 1:0.05 through a two-fluid nozzle, and uniformly mixing to form small liquid drops with the diameter of 200-500 mu m, so as to ensure that the PH of the small liquid drops is 5.8+/-0.3;
c) The atomized liquid drops form gel particles, and the gel time is 3-10 s;
d) Keeping the oxygen concentration of the spray dryer below 3%, and drying by hot air circulation to keep the temperature of 120+/-5 ℃ and the pressure at normal pressure after heating nitrogen; methyl trimethoxy silane is adopted as a hydrophobizing reagent, gasified and then enters a spray dryer, and mixed gas is formed by the gasified methyl trimethoxy silane, nitrogen and methanol steam after passing through the spray dryer, and the mixed gas is condensed to remove the solvent, and then is heated and dried in a recycling way.
Small gel particles are formed in the catalyzed sol liquid drops 10s, and methanol is used while the surface silicon hydroxyl is processed by hydrophobizationThe formed gas and nitrogen form mixed gas, gel particles are dried and continuously fall under the action of gravity to gradually form dry hydrophobic aerogel powder, the dry hydrophobic aerogel powder falls to the bottom of a dryer, and small particle powder comes out from a powder discharge port 1 under the influence of air flow; the powder with larger relative particles is discharged from the powder discharge port 2 to obtain aerogel powder with different particle diameters, and the specific surface area of the powder is 600-650 m 2 Per gram, density 50kg/m 3 The average diameter of the powder 1 is 5-10 μm, and the average diameter of the powder 2 is 50-60 μm.
Examples 2 to 5
The following examples were used to study the effect of xx on product properties, all other things being equal to example 1, with the following differences:
sol type | Solvent(s) | Gel catalysis Agent | Droplet PH Value of | Gel time | Experimental results | |
Example 2 | Silica alumina Glue | N-hexane | Ammonia water solution | 6.0 | 5s | Specific surface area of 500-600 m 2 Per gram, density 50kg/m 3 Powder 1 average The diameter is 5-10 μm, and the average diameter of the powder 2 is 50-60 μm. |
Example 3 | Titanium oxide solution Glue | Ethanol | Ammonia water solution | 4.8 | 90s | Specific surface area of 500-800 m 2 Per gram, density 38kg/m 3 Powder 1 average The diameter is 10-20 mu m, and the average diameter of the powder 2 is 60-80 mu m. |
Example 4 | Silica solution Glue | Hexamethyl group Disiloxane (DIS) Alkyl (C) | Sulfuric acid | 5.2 | 3s | Specific surface area 550 to 650m 2 Per gram, density 55kg/m 3 Powder 1 average The diameter is 10-20 mu m, and the average diameter of the powder 2 is 30-80 mu m. |
Example 5 | Alkaline silicon solution Glue | Ethanol | Electrolyte composition | 8.6 | 110s | Specific surface area of 300-450 m 2 Per gram, density 87kg/m 3 Powder 1 average The diameter is 20-30 μm, and the average diameter of the powder 2 is 120-200 μm. |
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The method for continuously preparing the hydrophobic aerogel powder by double-fluid atomization is characterized by comprising the following steps of:
a) Preparing a sol and a gel catalyst;
b) Uniformly mixing the sol and the gel catalyst through a two-fluid nozzle, and atomizing into small liquid drops;
c) The atomized droplets form gel particles;
d) Drying the solvent in the gel particles under reduced oxygen.
2. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 1, wherein the method comprises the following steps: the sol in the step a) comprises one or more of silica, alumina, titanium oxide and zirconia sol; the gel catalyst is one or more of acid, alkali and electrolyte.
3. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 1, wherein the method comprises the following steps: the sol in the step a) comprises a low-surface tension solvent, wherein the low-surface tension solvent is one or more of methanol, ethanol, acetone, butanone, n-hexane, hexamethyldisiloxane and hexamethyldisilazane.
4. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 1, wherein the method comprises the following steps: the pH of the small liquid drops in the step b) is 4.8-10.0, and the gel time in the step c) is 1-120s.
5. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 1, wherein the method comprises the following steps: the atomization in step b) is performed in an environment with an oxygen concentration of less than 3%.
6. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 1, wherein the method comprises the following steps: the drying temperature in the step d) is 30-200 ℃ and the pressure is normal pressure.
7. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 1, wherein the method comprises the following steps: the drying mode in the step d) is hot air circulation drying, and the drying mode comprises a fluid heating unit, a hot air circulation unit, a powder separation unit and a fluid recovery unit.
8. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 7, wherein: the hot air circulation unit circulates the dried hot air, and the hot air medium comprises inert gas and hydrophobizing agent.
9. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 8, wherein: the hydrophobizing reagent is one or more of gas-phase siloxane reagents, silazane reagents and chlorosilane reagents; the inert gas is nitrogen and/or carbon dioxide.
10. The method for continuously preparing hydrophobic aerogel powder by double fluid atomization according to claim 9, wherein: the siloxane hydrophobizing agent is one or more of hexamethyldisiloxane, trimethylmethoxysilane, trimethylethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethylmethoxysilane, dimethylethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, phenyltriethoxysilane and pentafluorophenyltriethoxysilane.
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CN117776191A (en) * | 2023-12-26 | 2024-03-29 | 浙江岩谷科技有限公司 | Method for continuously preparing in-situ hydrophobic silica aerogel powder by double-fluid atomization |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105271260A (en) * | 2014-06-11 | 2016-01-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing hydrophobic silica aerogel through normal-pressure drying process |
CN110604932A (en) * | 2019-09-29 | 2019-12-24 | 贵州梅岭电源有限公司 | Method for preparing potassium perchlorate powder by using closed-loop circulating spray dryer |
CN111659326A (en) * | 2020-06-12 | 2020-09-15 | 浙江岩谷科技有限公司 | Modification method of hydrophobic aerogel material |
US20230115794A1 (en) * | 2020-05-13 | 2023-04-13 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for producing aerogels and aerogels obtained using said method |
CN117023593A (en) * | 2023-05-17 | 2023-11-10 | 华东理工大学 | Dry modification method for preparing hydrophobic silica aerogel by using atomized silane modifier |
-
2023
- 2023-12-21 CN CN202311773426.6A patent/CN117680059A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105271260A (en) * | 2014-06-11 | 2016-01-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing hydrophobic silica aerogel through normal-pressure drying process |
CN110604932A (en) * | 2019-09-29 | 2019-12-24 | 贵州梅岭电源有限公司 | Method for preparing potassium perchlorate powder by using closed-loop circulating spray dryer |
US20230115794A1 (en) * | 2020-05-13 | 2023-04-13 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for producing aerogels and aerogels obtained using said method |
CN111659326A (en) * | 2020-06-12 | 2020-09-15 | 浙江岩谷科技有限公司 | Modification method of hydrophobic aerogel material |
CN117023593A (en) * | 2023-05-17 | 2023-11-10 | 华东理工大学 | Dry modification method for preparing hydrophobic silica aerogel by using atomized silane modifier |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN117776191A (en) * | 2023-12-26 | 2024-03-29 | 浙江岩谷科技有限公司 | Method for continuously preparing in-situ hydrophobic silica aerogel powder by double-fluid atomization |
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