CN116554723A - Aerogel composite powder and preparation method thereof - Google Patents

Aerogel composite powder and preparation method thereof Download PDF

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Publication number
CN116554723A
CN116554723A CN202210982044.3A CN202210982044A CN116554723A CN 116554723 A CN116554723 A CN 116554723A CN 202210982044 A CN202210982044 A CN 202210982044A CN 116554723 A CN116554723 A CN 116554723A
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aerogel
composite powder
parts
pressure
aerogel composite
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Inventor
喻学锋
康翼鸿
何睿
陈海平
向振涛
兰洁
王晓琴
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Wuhan Zhongke Advanced Material Technology Co Ltd
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Wuhan Zhongke Advanced Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • C04B40/0042Powdery mixtures
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • C08K7/26Silicon- containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention provides aerogel composite powder, which consists of the following raw materials: aerogel, polymer resin and withstand voltage hollow nanospheres, the aerogel composite powder inlayer is aerogel and silica hollow nanospheres, and the silica hollow nanospheres are filled in the aerogel hole. The silica hollow nano-spheres are used for filling the aerogel holes, so that the support of the silica on the aerogel holes can be realized, and the aerogel holes are prevented from collapsing due to various reasons in the use process of the aerogel; the high molecular resin is used for wrapping the aerogel and the silica hollow nano microsphere, so that the mechanical strength of the aerogel can be enhanced; the silica hollow nano-microsphere is combined with the aerogel, so that the negative influence of other materials on the overall heat insulation performance of the composite material when the aerogel is compounded with other materials can be reduced, and the better heat insulation performance of the aerogel composite powder is maintained.

Description

Aerogel composite powder and preparation method thereof
Technical Field
The invention belongs to the technical field of chemical materials, and particularly relates to aerogel composite powder and a preparation method thereof.
Background
The gel has a three-dimensional network structure with nanometer holes, is a solid material which takes gaseous substances as continuous dispersion media, has the special properties of low density, high porosity and specific surface area, high surface activity, low heat conductivity, high transmittance, high adsorption rate and the like, and can be widely applied to the fields of heat insulation coating, heat insulation composite materials and the like, and has very wide application prospect.
Although aerogel has a plurality of excellent characteristics in the fields of heat insulation coating, heat insulation composite material and the like, the heat conductivity coefficient is as low as 0.01W/(m.K), but the characteristics of unique porous network structure, low density and the like lead to poor mechanical properties of the aerogel, and limit the application of the aerogel. In addition, when the aerogel is mixed with water and a non-low surface organic solvent to prepare a coating, the holes collapse after the aerogel is infiltrated. When the aerogel pores are destroyed to a large extent, the thermal conductivity is much more than 0.07W/(m·k), which results in that the thermal insulation properties of the aerogel cannot be exerted. In addition, because of its light weight, it is difficult to disperse when mixed with other substances, and uneven dispersion can lead to uneven local properties of the prepared material, and the service life can be affected. Therefore, there is a need to develop aerogel materials that have high mechanical strength, good collapse resistance and easy dispersion.
Disclosure of Invention
The invention aims to provide a preparation method of aerogel composite powder. The method has the advantages of simple materials and process and good collapse resistance, and the prepared aerogel material composite board has high mechanical strength and low heat conductivity coefficient, and is beneficial to the application of the aerogel.
In order to achieve the above object, the technical scheme of the invention is as follows:
an aerogel composite powder is composed of the following raw materials: aerogel, polymer resin and withstand voltage hollow nanometer microballon, aerogel composite powder includes inlayer and skin, and the inlayer constitutes aerogel and withstand voltage hollow nanometer microballon, and withstand voltage hollow nanometer microballon fills in the aerogel hole, and the skin is the polymer resin coating.
The polymer resin coating layer contains pressure-resistant hollow nano microspheres.
The aerogel composite powder comprises the following components in parts by weight: 60-80 parts of aerogel, 5-15 parts of high polymer resin and 15-25 parts of pressure-resistant hollow nano microspheres.
The aerogel is silica aerogel with epoxy groups.
The high polymer resin is epoxy high polymer resin, and the molecular weight is 5000-100000.
The pressure-resistant hollow nanospheres are pressure-resistant silicon dioxide hollow nanospheres and one or more of pressure-resistant glass hollow nanospheres are mixed.
The preparation method of the aerogel composite powder provided by the invention comprises the following steps:
step one, adding pressure-resistant hollow nano microspheres into aerogel, and uniformly dispersing;
secondly, ball milling is carried out by a ball mill under the condition of pressurization;
step three, adding the high molecular epoxy resin into the mixture in the step two, and uniformly stirring at a low speed;
and step four, drying and crushing the mixture in the step three into micron-sized small particles, and thus obtaining the aerogel composite powder.
The aerogel in the first step is silica aerogel with epoxy groups, and the preparation method comprises the following steps:
1) Taking 90 parts of hydrophobic silica aerogel powder, and spraying 10 parts of epoxy silane coupling agent in the high-speed stirring process;
2) Mixing for a period of time at 80 ℃ to obtain the silica aerogel with epoxy groups.
The pore diameter of the hydrophobic aerogel in the first step is larger than the particle diameter of the pressure-resistant hollow nano microsphere.
The aperture of the hydrophobic aerogel is larger than the particle size of the pressure-resistant hollow nano microsphere and is in the range of 10-30nm.
The pressure in the second step is 1-5MPa;
the rotating speed of the ball mill is 70% -85% of the critical rotating speed; the speed of low-speed stirring in the third step is 300-600r/min.
The epoxy silane coupling agent is selected from one or two of gamma- (2, 3-glycidoxy) propyl trimethoxy silane and gamma- (2, 3-glycidoxy) propyl triethoxy silane.
The hydrophobic silica aerogel in the step 1) is one or more hydrophobically modified silica aerogels selected from hexamethyldisilazane, tetramethyl chlorosilane, alkyl silane, methoxytrimethyl silane and hexamethyldisiloxane;
the aerogel composite powder prepared by the invention can be used in the fields of paint, coating, composite material preparation and the like or in a system containing resin.
The invention has the following beneficial effects:
(1) The hollow silica nano-spheres are used for filling the aerogel holes, so that the mechanical property of the aerogel can be enhanced, meanwhile, the hollow nano-spheres can play a supporting role on the silica aerogel holes, the hole collapse of the aerogel in various application scenes in the use process can be improved to a great extent, and the heat insulation property of the aerogel can be better exerted;
(2) The aerogel and the silica hollow nano-microspheres are wrapped by using the high polymer resin, so that the hollow nano-microspheres can be locked in the aerogel holes, and meanwhile, the hollow microspheres which do not enter the aerogel holes can be dispersed in the high polymer resin, so that the mechanical strength of the aerogel powder can be enhanced;
(3) In addition, the weight of the aerogel is increased by the high polymer resin and the hollow microspheres, so that the aerogel is easy to disperse when being mixed with other components, and the problem of nonuniform material performance caused by nonuniform mixing when the aerogel is used for preparing materials is solved;
(4) The polymer resin is coated on the surface of the aerogel, so that the damage of the aerogel caused by infiltration of the solvent into the aerogel holes in a system in which the solvent exists can be reduced; in addition, due to the existence of the high polymer resin, the aerogel composite heat insulation powder can be well mutually dissolved with the resin when being applied in a system containing the resin, and the stability of a target material is well improved;
(5) The silica hollow nano-microsphere with the particle size smaller than that of the aerogel holes is combined with the aerogel, and a small amount of high-molecular resin is used, so that the thermal conductivity of the hollow nano-microsphere is also small, the thermal conductivity of the prepared aerogel composite powder is changed slightly, and the excellent heat insulation performance of the aerogel can be still maintained.
Detailed Description
The technical scheme of the present invention will be clearly and completely described in the following in connection with examples.
Example 1
(1) Preparation of hydrophobic aerogel with epoxy groups:
taking 90 parts of hexamethyldisiloxane modified silica aerogel powder, wherein the pore diameter is 50nm, the heat conductivity coefficient is 0.013 w/(m.k), and 10 parts of epoxy silane coupling agent are sprayed in the high-speed stirring process; mixing at 80 ℃ for 60min to obtain the aerogel with epoxy groups.
(2) Preparing aerogel composite powder:
adding 25 parts of silica hollow nano microspheres (with the particle size of 30 nm) into 60 parts of aerogel, and stirring for 30min; then ball milling is carried out for 30min by a ball mill at 70% of the critical rotation speed of the ball mill under the pressure of 3 Mpa; adding 15 parts of high molecular epoxy resin, stirring at low speed for 30min, and drying at 100 ℃ for 1h; and finally, crushing the dried mixture into micron-sized particles in a grinding ball mode, and thus obtaining the aerogel composite powder.
Example 2
(1) Preparation of hydrophobic aerogel with epoxy groups:
taking 90 parts of hexamethyldisiloxane modified silica aerogel powder, wherein the pore diameter is 50nm, the heat conductivity coefficient is 0.013 w/(m.k), and 10 parts of epoxy silane coupling agent are sprayed in the high-speed stirring process; mixing at 80 ℃ for 60min to obtain the aerogel with epoxy groups.
(2) Preparing aerogel composite powder:
adding 25 parts of silica hollow nano microspheres (particle size of 30 nm) into 80 parts of aerogel, and stirring for 30min; then ball milling is carried out for 30min by a ball mill at 70% of the critical rotation speed of the ball mill under the pressure of 3 Mpa; adding 15 parts of high molecular epoxy resin, stirring at low speed for 30min, and drying at 100 ℃ for 1h; and finally, crushing the dried mixture into micron-sized particles in a grinding ball mode, and thus obtaining the aerogel composite powder.
Example 3
(1) Preparation of hydrophobic aerogel with epoxy groups:
taking 90 parts of hexamethyldisiloxane modified silica aerogel powder, wherein the pore diameter is 60nm, the heat conductivity coefficient is 0.013 w/(m.k), and 10 parts of epoxy silane coupling agent are sprayed in the high-speed stirring process; mixing at 80 ℃ for 60min to obtain the aerogel with epoxy groups.
(2) Preparing aerogel composite powder:
adding 25 parts of silica hollow nano microspheres (particle size of 30 nm) into 80 parts of aerogel, and stirring for 30min; then ball milling is carried out for 30min by a ball mill at 70% of the critical rotation speed of the ball mill under the pressure of 3 Mpa; adding 15 parts of high molecular epoxy resin, stirring at low speed for 30min, and drying at 100 ℃ for 1h; and finally, crushing the dried mixture into micron-sized particles in a grinding ball mode, and thus obtaining the aerogel composite powder.
Example 4
(1) Preparation of hydrophobic aerogel with epoxy groups:
taking 90 parts of hexamethyldisiloxane modified silica aerogel powder, wherein the pore diameter is 60nm, the heat conductivity coefficient is 0.013 w/(m.k), and 10 parts of epoxy silane coupling agent are sprayed in the high-speed stirring process; mixing at 80 ℃ for 60min to obtain the aerogel with epoxy groups.
(2) Preparing aerogel composite powder:
adding 15 parts of silica hollow nano microspheres (with the particle size of 30 nm) into 80 parts of aerogel, and stirring for 30min; then ball milling is carried out for 30min by a ball mill at 70% of the critical rotation speed of the ball mill under the pressure of 3 Mpa; adding 15 parts of high molecular epoxy resin, stirring at low speed for 30min, and drying at 100 ℃ for 1h; and finally, crushing the dried mixture into micron-sized particles in a grinding ball mode, and thus obtaining the aerogel composite powder.
Example 5
(1) Preparation of hydrophobic aerogel with epoxy groups:
taking 90 parts of hexamethyldisiloxane modified silica aerogel powder, wherein the pore diameter is 60nm, the heat conductivity coefficient is 0.013 w/(m.k), and 10 parts of epoxy silane coupling agent are sprayed in the high-speed stirring process; mixing at 80 ℃ for 60min to obtain the aerogel with epoxy groups.
(2) Preparing aerogel composite powder:
adding 15 parts of silica hollow nano microspheres (with the particle size of 30 nm) into 80 parts of aerogel, and stirring for 30min; then ball milling is carried out for 30min by a ball mill at 70% of the critical rotation speed of the ball mill under the pressure of 3 Mpa; adding 5 parts of high molecular epoxy resin, stirring at low speed for 30min, and drying at 100deg.C for 1 hr; and finally, crushing the dried mixture into micron-sized particles in a grinding ball mode, and thus obtaining the aerogel composite powder.
Comparative example 1
Taking 80 parts of aerogel (pore 50 nm), 25 parts of silica hollow nano-microspheres (particle size 50 nm) and 10 parts of high polymer epoxy resin, stirring for 1h, and drying at 100 ℃ for 1h; and then crushing the dried mixture into micron-sized particles in a grinding ball mode, and obtaining the aerogel composite powder.
Comparative example 2
80 parts of aerogel with the heat conductivity coefficient of 0.013 w/(m.k) and 25 parts of hollow nano-microspheres are mixed.
The products prepared in examples and comparative examples were tested and the test results are shown in the following table:
from the data in the table, the aerogel prepared by the method has better heat insulation performance and can improve collapse of aerogel holes caused by solvent infiltration.

Claims (10)

1. The aerogel composite powder is characterized by being prepared from the following raw materials: aerogel, polymer resin and withstand voltage hollow nanometer microballon, aerogel composite powder includes inlayer and skin, and the inlayer constitutes aerogel and withstand voltage hollow nanometer microballon, and withstand voltage hollow nanometer microballon fills in the aerogel hole, and the skin is the polymer resin coating.
2. The aerogel composite powder of claim 1, wherein the aerogel composite powder is prepared from the following raw materials in parts by weight: 60-80 parts of aerogel, 5-15 parts of high polymer resin and 15-25 parts of pressure-resistant hollow nano microspheres.
3. The aerogel composite powder of any of claims 1-2, wherein the aerogel is an epoxy-containing silica aerogel.
4. The aerogel composite powder according to any one of claims 1 to 2, wherein the polymer resin is an epoxy-based polymer resin having a molecular weight of 5000 to 100000.
5. The aerogel composite powder according to claim 1, wherein the pressure-resistant hollow nanospheres are one or more of pressure-resistant silica hollow nanospheres and pressure-resistant glass hollow nanospheres.
6. The preparation method of the aerogel composite powder is characterized by comprising the following steps:
step one, adding pressure-resistant hollow nano microspheres into aerogel, and uniformly dispersing;
secondly, ball milling is carried out by a ball mill under the condition of pressurization;
step three, adding the high molecular epoxy resin into the mixture in the step two, and uniformly stirring at a low speed;
and step four, drying and crushing the mixture in the step three into micron-sized small particles, and thus obtaining the aerogel composite powder.
7. The method for preparing aerogel composite powder according to claim 6, wherein the aerogel in the first step is silica aerogel with epoxy groups, and the method comprises the following steps:
1) Taking 90 parts of hydrophobic silica aerogel powder, and spraying 10 parts of epoxy silane coupling agent in the high-speed stirring process;
2) Mixing for a period of time at 80 ℃ to obtain the silica aerogel with epoxy groups.
8. The method of claim 6, wherein the pore size of the hydrophobic aerogel in the first step is larger than the particle size of the pressure-resistant hollow nano-microspheres.
9. The method for preparing aerogel composite powder according to claim 8, wherein the pore size of the hydrophobic aerogel is 10-30nm larger than the particle size of the pressure-resistant hollow nano-microspheres.
10. The method for preparing aerogel composite powder according to claim 6, wherein the pressure in the second step is 1-5MPa; the rotating speed of the ball mill is 70% -85% of the critical rotating speed; the speed of low-speed stirring in the third step is 300-600r/min.
CN202210982044.3A 2022-08-16 2022-08-16 Aerogel composite powder and preparation method thereof Pending CN116554723A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117177453A (en) * 2023-09-25 2023-12-05 深圳彩粒威科技有限公司 5G wave-transparent substrate and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100036104A (en) * 2008-09-29 2010-04-07 제일모직주식회사 Polymer-coated aerogels, method for preparing thereof and insulative resin compositions using the same
CN104496403A (en) * 2014-12-23 2015-04-08 南京唯才新能源科技有限公司 Reinforced aerogel composite material and preparation method thereof
CN107266938A (en) * 2016-04-08 2017-10-20 南京唯才新能源科技有限公司 A kind of enhanced aerogel powder and preparation method thereof
CN112010628A (en) * 2020-09-14 2020-12-01 成都硕屋科技有限公司 Silicon dioxide aerogel composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100036104A (en) * 2008-09-29 2010-04-07 제일모직주식회사 Polymer-coated aerogels, method for preparing thereof and insulative resin compositions using the same
CN104496403A (en) * 2014-12-23 2015-04-08 南京唯才新能源科技有限公司 Reinforced aerogel composite material and preparation method thereof
CN107266938A (en) * 2016-04-08 2017-10-20 南京唯才新能源科技有限公司 A kind of enhanced aerogel powder and preparation method thereof
CN112010628A (en) * 2020-09-14 2020-12-01 成都硕屋科技有限公司 Silicon dioxide aerogel composite material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117177453A (en) * 2023-09-25 2023-12-05 深圳彩粒威科技有限公司 5G wave-transparent substrate and preparation method thereof

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