CN116396450A - Aerogel composite modification method - Google Patents
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- CN116396450A CN116396450A CN202310386597.7A CN202310386597A CN116396450A CN 116396450 A CN116396450 A CN 116396450A CN 202310386597 A CN202310386597 A CN 202310386597A CN 116396450 A CN116396450 A CN 116396450A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 83
- 239000002131 composite material Substances 0.000 title claims abstract description 10
- 238000002715 modification method Methods 0.000 title claims description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- 239000000839 emulsion Substances 0.000 claims abstract description 55
- 239000003999 initiator Substances 0.000 claims abstract description 51
- 239000000843 powder Substances 0.000 claims abstract description 33
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 7
- 239000000178 monomer Substances 0.000 claims abstract description 7
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 7
- -1 vinyl siloxane Chemical class 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 17
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 5
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 5
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004965 Silica aerogel Substances 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
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- JDXQSTLUHNAVMN-UHFFFAOYSA-M sodium propane-2-sulfonate prop-2-enamide Chemical compound [Na+].NC(=O)C=C.CC(C)S([O-])(=O)=O JDXQSTLUHNAVMN-UHFFFAOYSA-M 0.000 claims description 3
- AERRGWRSYANDQB-UHFFFAOYSA-N azanium;dodecane-1-sulfonate Chemical compound [NH4+].CCCCCCCCCCCCS([O-])(=O)=O AERRGWRSYANDQB-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 239000004925 Acrylic resin Substances 0.000 abstract description 3
- 229920000178 Acrylic resin Polymers 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 238000006482 condensation reaction Methods 0.000 abstract description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 2
- 229920005570 flexible polymer Polymers 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a method for composite modification of aerogel, which comprises the steps of adding 30-50 parts of deionized water into a reaction kettle, sequentially adding 0.5-1.5 parts of emulsifying agent, 5-8 parts of methyl acrylate, 10-15 parts of butyl acrylate and 1-3 parts of functional monomer, and stirring at a high speed to obtain a pre-emulsion; dissolving 0.1-0.5 part of initiator in a small amount of deionized water, and adding 2-4 parts of vinyl siloxane to prepare an initiator solution; adding half of the initiator solution into the pre-emulsion, stirring and heating to 80-100 ℃ to start reaction, and cooling and stopping reaction after blue light begins to appear in the emulsion; adding 20-30 parts of aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 90-120 ℃ for continuous reaction, continuously preserving heat for 80-100 ℃ for reaction for 1-3 hours after the initiator is dropwise added, and naturally cooling to room temperature to obtain aerogel modified emulsion; placing the aerogel modified emulsion into a vacuum box, heating and drying at 60-80 ℃ for 5-8h; and crushing and sieving the dried product to obtain the composite modified aerogel. The method takes siloxane as a medium to perform condensation reaction with hydroxyl groups on the surface of the aerogel, and realizes surface wrapping modification of the aerogel powder by an acrylic resin in-situ polymerization technology. Due to the protection of the surface flexible polymer, the modified aerogel reduces particle breakage caused by external force dispersion when in use, simultaneously endows the aerogel with rich functional groups on the surface, can chemically react with matrix resin, and improves the strength of the aerogel material.
Description
The invention relates to the technical field of aerogel, in particular to a composite modification method of aerogel.
Background
The aerogel is used as a super heat insulation material and has great application prospect in the fields of heat preservation, fire prevention, sound insulation and the like. The aerogel belongs to a porous material, has relatively poor mechanical properties, is extremely easy to crack and pulverize in use, and needs to use an adhesive in the application process so as to ensure certain mechanical properties, but the particle size of the adhesive is much smaller than the pore diameter of the aerogel, so that the pores of the aerogel are extremely easy to be filled, the aerogel loses the characteristics of the porous material, and the performances of heat insulation, heat preservation and the like of the aerogel can be greatly reduced.
In order to exert the pore structure characteristics of aerogel materials, a method of adding a small amount or dispersing at a low speed is mostly adopted in the preparation of aerogel materials at present. The small amount of addition can ensure that the aerogels cannot be mutually extruded, so that the crushing and failure of materials are avoided, but the addition amount is limited in the mode; the low-speed dispersion can also avoid the damage of the aerogel structure, but the processing mode is extremely easy to cause uneven material dispersion, thereby causing unstable overall performance of the composite material.
In order to solve the problems, the invention provides a method for composite modification of aerogel, namely, in-situ polymerization of silicone condensation modified flexible acrylic resin is realized on the surface of aerogel powder by in-situ polymerization and surface modification grafting technology. The modified aerogel powder is free from particle breakage caused by external force dispersion when in use due to the double modification protection of the surface, and meanwhile, the aerogel has rich surface functional groups, can be subjected to chemical reaction with other components, and improves the bonding strength between aerogel particles.
Disclosure of Invention
In order to achieve the above purpose, the present invention provides the following technical solutions:
the aerogel composite modification method is characterized by comprising the following components in percentage by weight: 5-8 parts of methyl acrylate, 10-15 parts of butyl acrylate, 1-3 parts of functional monomer, 0.5-1.5 parts of emulsifier, 2-4 parts of vinyl siloxane, 20-30 parts of aerogel, 0.1-0.5 part of initiator and 30-50 parts of deionized water.
Further, the specific steps are as follows: (1) Adding deionized water into a reaction kettle, sequentially adding an emulsifier, methyl acrylate, butyl acrylate and a functional monomer, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving an initiator in deionized water, and adding vinyl siloxane to prepare an initiator solution;
(3) Adding half of the initiator solution into the pre-emulsion, stirring and heating to 80-100 ℃ to start reaction, and cooling and stopping reaction after blue light begins to appear in the emulsion;
(4) Adding aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the residual initiator solution, heating to 90-120 ℃ for continuous reaction, continuously preserving heat for 80-100 ℃ for reaction for 1-3 hours after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 60-80 ℃ for 5-8h;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
The functional monomer is one or more of acrylic acid, methacrylic acid, hydroxyethyl acrylate and acrylamide;
the emulsifier is one or more of sodium dodecyl sulfate, ammonium dodecyl sulfonate and sodium acrylamide isopropyl sulfonate;
the vinyl siloxane is one of divinyl tetramethyl disiloxane, vinyl triethoxysilane and vinyl trimethoxysilane;
the initiator is one of ammonium persulfate, potassium persulfate and sodium persulfate;
the aerogel is one of silicon oxide aerogel powder, aluminum oxide aerogel powder, titanium oxide aerogel powder and polyimide aerogel powder.
Due to the adoption of the technical scheme, the invention has the following characteristics:
1. the invention takes the siloxane as a medium to perform condensation reaction with the hydroxyl on the surface of the aerogel, and realizes the surface wrapping modification of the aerogel powder by an acrylic resin in-situ polymerization technology. Due to the protection of the surface flexible polymer, the particle breakage caused by external force dispersion is reduced when the modified aerogel is used, meanwhile, the abundant functional groups on the surface of the aerogel are endowed, and the modified aerogel can be subjected to chemical reaction with matrix resin to improve the strength of the aerogel material;
2. according to the invention, the aerogel is wrapped and modified in an in-situ emulsion polymerization mode, the process is environment-friendly, the modification of the aerogel on the molecular size is realized, the particle size and appearance of the finished product are not greatly different from those of a common aerogel product, and the problem that the heat insulation performance of the aerogel is reduced due to the blockage of the aerogel holes is greatly reduced.
Detailed Description
The following detailed description of the technical solutions in the embodiments of the present invention will make it apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
(1) Adding 40 parts of deionized water into a reaction kettle, and sequentially adding 1 part of sodium dodecyl sulfate, 6 parts of methyl acrylate, 10 parts of butyl acrylate and 1 part of acrylic acid, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving 0.2 part of ammonium persulfate in 10 parts of deionized water, and adding 2 parts of divinyl tetramethyl disiloxane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 80 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 30 parts of silica aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 90 ℃ for continuous reaction, continuously preserving heat for 3 hours at 80 ℃ after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 80 ℃ for 5 hours;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
Examples
(1) Adding 38 parts of deionized water into a reaction kettle, and sequentially adding 1 part of ammonium dodecyl sulfate, 8 parts of methyl acrylate, 12 parts of butyl acrylate and 3 parts of methacrylic acid, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving 0.5 part of sodium persulfate in 12 parts of deionized water, and adding 4 parts of vinyl triethoxysilane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 100 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 22 parts of alumina aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 120 ℃ for continuous reaction, continuously preserving heat for 100 ℃ for reaction for 3 hours after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 70 ℃ for 7h;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
Examples
(1) Adding 35 parts of deionized water into a reaction kettle, and sequentially adding 1.5 parts of sodium acrylamide isopropyl sulfonate, 8 parts of methyl acrylate, 15 parts of butyl acrylate and 1 part of hydroxyethyl acrylate, and stirring at a high speed to fully pre-emulsify the materials to obtain a pre-emulsion;
(2) Dissolving 0.5 part of sodium persulfate in 15 parts of deionized water, and adding 3 parts of vinyl triethoxysilane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 90 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 21 parts of polyimide aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 90 ℃ for continuous reaction, continuously preserving heat for reaction for 1h at 80 ℃ after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 80 ℃ for 8 hours;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
(1) Adding 40 parts of deionized water into a reaction kettle, and sequentially adding 1.5 parts of sodium dodecyl sulfate, 5 parts of methyl acrylate, 15 parts of butyl acrylate and 3 parts of acrylamide, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving 0.5 part of ammonium persulfate in 10 parts of deionized water, and adding 3 parts of divinyl tetramethyl disiloxane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 80 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 22 parts of silicon oxide aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 120 ℃ for continuous reaction, continuously preserving heat for 3 hours at 100 ℃ after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 80 ℃ for 8 hours;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
Example 5
(1) Adding 38 parts of deionized water into a reaction kettle, and sequentially adding 0.5 part of sodium dodecyl sulfate, 8 parts of methyl acrylate, 15 parts of butyl acrylate and 1 part of acrylic acid, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving 0.5 part of ammonium persulfate in 10 parts of deionized water, and adding 2 parts of divinyl tetramethyl disiloxane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 80 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 25 parts of titanium oxide aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 100 ℃ for continuous reaction, continuously preserving heat for 90 ℃ for reaction for 2 hours after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 70 ℃ for 7h;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
Examples
(1) Adding 32 parts of deionized water into a reaction kettle, and sequentially adding 1.5 parts of ammonium dodecyl sulfate, 8 parts of methyl acrylate, 15 parts of butyl acrylate and 3 parts of hydroxyethyl acrylate, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving 0.5 part of potassium persulfate in 6 parts of deionized water, and adding 4 parts of divinyl tetramethyl disiloxane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 100 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 30 parts of silica aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 120 ℃ for continuous reaction, continuously preserving heat for 3 hours at 100 ℃ after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 80 ℃ for 8 hours;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
Examples
(1) Adding 35 parts of deionized water into a reaction kettle, and sequentially adding 1.5 parts of sodium dodecyl sulfate, 8 parts of methyl acrylate, 15 parts of butyl acrylate and 1 part of acrylic acid, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving 0.5 part of sodium persulfate in 15 parts of deionized water, and adding 3 parts of vinyl triethoxysilane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 90 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 21 parts of polyimide aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 90 ℃ for continuous reaction, continuously preserving heat for reaction for 1h at 80 ℃ after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 80 ℃ for 8 hours;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
Examples
(1) Adding 40 parts of deionized water into a reaction kettle, and sequentially adding 1.5 parts of sodium dodecyl sulfate, 5 parts of methyl acrylate, 15 parts of butyl acrylate and 3 parts of acrylic acid, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving 0.5 part of ammonium persulfate in 10 parts of deionized water, and adding 3 parts of divinyl tetramethyl disiloxane to prepare an initiator solution;
(3) Half of the initiator solution is added into the pre-emulsion, the mixture is stirred and heated to 80 ℃ to start the reaction, and the emulsion is cooled to stop the reaction after blue light begins to appear;
(4) Adding 22 parts of alumina aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the rest initiator solution, heating to 120 ℃ for continuous reaction, continuously preserving heat for 100 ℃ for reaction for 3 hours after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the emulsion into a vacuum box, heating and drying at 80 ℃ for 8 hours;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
Claims (7)
1. The aerogel composite modification method is characterized by comprising the following components in parts by weight: 5-8 parts of methyl acrylate, 10-15 parts of butyl acrylate, 1-3 parts of functional monomer, 0.5-1.5 parts of emulsifier, 2-4 parts of vinyl siloxane, 20-30 parts of aerogel, 0.1-0.5 part of initiator and 30-50 parts of deionized water.
2. A method for composite modification of aerogel comprises the following specific steps:
(1) Adding deionized water into a reaction kettle, sequentially adding an emulsifier, methyl acrylate, butyl acrylate and a functional monomer, and stirring at a high speed to fully pre-emulsify the mixture to obtain a pre-emulsion;
(2) Dissolving an initiator in deionized water, and adding vinyl siloxane to prepare an initiator solution;
(3) Adding half of the initiator solution into the pre-emulsion, stirring and heating to 80-100 ℃ to start reaction, and cooling and stopping reaction after blue light begins to appear in the emulsion;
(4) Adding aerogel powder into a reaction kettle, fully dispersing, then beginning to dropwise add the residual initiator solution, heating to 90-120 ℃ for continuous reaction, continuously preserving heat for 80-100 ℃ for reaction for 1-3 hours after the initiator dropwise addition is completed, and naturally cooling to room temperature to obtain aerogel modified emulsion;
(5) Placing the aerogel modified emulsion into a vacuum box, heating and drying at 60-80 ℃ for 5-8h;
(6) And crushing and sieving the dried product to obtain modified aerogel powder.
3. The method of claim 1, wherein the functional monomer is one or more of acrylic acid, methacrylic acid, hydroxyethyl acrylate, and acrylamide.
4. The method of claim 1, wherein the emulsifier is one or more of sodium dodecyl sulfate, ammonium dodecyl sulfonate, and sodium acrylamide isopropyl sulfonate.
5. The method of claim 1, wherein the vinyl siloxane is one of divinyl tetramethyl disiloxane, vinyl triethoxysilane, vinyl trimethoxysilane.
6. The method of claim 1, wherein the initiator is one of ammonium persulfate, potassium persulfate, and sodium persulfate.
7. The method of claim 1, wherein the aerogel is one of silica aerogel powder, alumina aerogel powder, titania aerogel powder, and polyimide aerogel powder.
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| CN202310386597.7A CN116396450A (en) | 2023-04-12 | 2023-04-12 | Aerogel composite modification method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117384557A (en) * | 2023-11-01 | 2024-01-12 | 南雄市沃太化工有限公司 | Low-temperature-resistant polyacrylate pressure-sensitive adhesive and preparation method thereof |
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2023
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117384557A (en) * | 2023-11-01 | 2024-01-12 | 南雄市沃太化工有限公司 | Low-temperature-resistant polyacrylate pressure-sensitive adhesive and preparation method thereof |
| CN117384557B (en) * | 2023-11-01 | 2024-04-09 | 南雄市沃太化工有限公司 | Low-temperature-resistant polyacrylate pressure-sensitive adhesive and preparation method thereof |
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