CN110482997B - Preparation method of heat preservation and insulation ball and prepared heat preservation and insulation ball - Google Patents

Preparation method of heat preservation and insulation ball and prepared heat preservation and insulation ball Download PDF

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CN110482997B
CN110482997B CN201910792590.9A CN201910792590A CN110482997B CN 110482997 B CN110482997 B CN 110482997B CN 201910792590 A CN201910792590 A CN 201910792590A CN 110482997 B CN110482997 B CN 110482997B
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heat
curing agent
rubber
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prefabricated slurry
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CN110482997A (en
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张尚权
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Anhui Keang Nano Technology Co ltd
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    • 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
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/10Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/20Polyamides
    • 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
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/14Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
    • 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
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • C04B28/26Silicates of the alkali metals
    • 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
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/08Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
    • 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
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/08Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
    • C04B38/085Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances of micro- or nanosize
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • 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
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The invention discloses a preparation method of a heat preservation and insulation ball, relating to the technical field of heat preservation and insulation materials and comprising the following steps: (1) mixing an adhesive with a solvent to prepare an adhesive solution; mixing a curing agent with a solvent to prepare a curing agent solution; (2) uniformly mixing a heat-insulating material and an adhesive solution according to a certain proportion to obtain prefabricated slurry; (3) dropwise adding the prefabricated slurry into a curing agent solution to obtain prefabricated slurry balls; (4) and drying the prefabricated slurry pellets to obtain the heat-insulating balls. The invention also provides the heat preservation and insulation ball prepared by the preparation method, and the heat preservation and insulation ball has the beneficial effects that: the heat-insulating ball prepared by the invention has the advantages of light weight effect, good flame retardant and heat-insulating properties, simple process, high yield and suitability for industrial production.

Description

Preparation method of heat preservation and insulation ball and prepared heat preservation and insulation ball
Technical Field
The invention relates to the technical field of heat preservation and insulation materials, in particular to a preparation method of a heat preservation and insulation ball and the prepared heat preservation and insulation ball.
Background
The increasing environmental problem of energy sources at present puts higher demands on the effective utilization of the energy sources. In the field of heat preservation and heat insulation, more green, environment-friendly and efficient heat preservation materials are developed, and the energy loss is reduced, so that the method has important strategic significance.
The light heat-insulating material is a light heat-insulating material, and the heat-insulating ball is a spherical heat-insulating material made of the light heat-insulating material, and can be widely applied to various filling heat-insulating fields. Patent CN201810463443.2 discloses a composite aerogel microsphere and its preparation method: firstly, ultrasonically stripping prepared graphite oxide to obtain a graphene oxide solution, and then adding Ca2+、PO4 3-And Zn2+Solution, Ca2+And PO4 3-The molar ratio of the hydroxyapatite to the graphene oxide is 1: 0.1-1: 10, adding ammonia water, stirring to form a composite dispersion liquid, and finally, carrying outSpraying, cooling bath receiving, sieving, and freeze-drying to obtain the composite aerogel microspheres, wherein the process is complicated. The invention CN201810438091.5 discloses a nano porous alumina aerogel ceramic pellet and a preparation method thereof: SS01 is prepared into aluminum sol containing polyvinyl alcohol; preparing an oil ammonia column solution by SS 02; SS03 balling; aging with SS04, and supercritical drying; SS05 heat treatment. The method has high requirements on equipment.
In summary, the materials and methods for preparing the green environment-friendly heat-insulating ball are still limited. Therefore, a simple and convenient method for preparing the heat-insulating ball is still needed.
Disclosure of Invention
The invention solves the technical problem that the existing preparation method of the heat-insulation ball is complex, and provides the preparation method of the heat-insulation ball.
The invention adopts the following technical scheme to solve the technical problems:
the invention provides a preparation method of a heat preservation and insulation ball, which comprises the following steps:
(1) preparing an adhesive solution: mixing an adhesive with a solvent to obtain an adhesive solution;
(2) preparing a curing agent solution: mixing a curing agent with a solvent to obtain a curing agent solution;
(3) uniformly mixing a heat-insulating material and an adhesive solution according to a certain proportion to obtain prefabricated slurry;
(4) dropwise adding the prefabricated slurry into a curing agent solution, wherein the prefabricated slurry is spherical when dropping, enters the curing agent solution, is cured into spheres, and floats in the curing agent solution to obtain prefabricated slurry balls;
(5) and drying the prefabricated slurry pellets to obtain the heat-insulating balls.
Preferably, the adhesive accounts for 0.05 to 50 wt% of the solvent; the mass percentage of the curing agent in the solvent is 0.05-50 wt%.
Preferably, the heat preservation and insulation material comprises one or more of silica aerogel, silica hollow microspheres, polyimide aerogel, silicon carbide aerogel, boron nitride aerogel, silica nanotubes, silicon carbide nanotubes and boron nitride nanotubes.
Preferably, the adhesive comprises water glass, gypsum, polyvinyl acetate, cellulose ester, polyvinyl alcohol, perchloroethylene, polyisobutylene, polyacrylate, alpha-cyanoacrylate, polyvinyl acetal, epoxy resin, phenolic resin, urea-formaldehyde resin, melamine-formaldehyde resin, organic silicon resin, acrylic resin, polyimide, polybenzimidazole, phenolic-polyvinyl acetal, phenolic-epoxy resin, one or more of natural rubber, rosin, gelatin, cellulose, starch glue, chloroprene rubber, styrene-butadiene rubber, butyl rubber, sodium butadiene rubber, isoprene rubber, polysulfide rubber, polyurethane rubber, chlorosulfonated polyethylene, silicone rubber, phenol-butadiene rubber, phenol-chloroprene rubber, phenol resin-polyurethane rubber, epoxy resin-nitrile rubber and epoxy resin-polysulfide rubber.
Preferably, the curing agent comprises one or more of acid anhydride, resol type phenolic resin, amino resin, dicyandiamide and hydrazide.
The solvent comprises deionized water and C1-6One or more of alkanol, cyclohexane, octadecene and oleic acid.
Preferably, the pre-slurry is added dropwise to the curing agent solution at a dropping rate of 0.25 to 5 drops per second.
Preferably, the drying method in the step (4) is one or more of steam drying, atmospheric drying, freeze drying and flash evaporation.
Preferably, the diameter of the pre-slurry pellets is 1-10 mm.
Preferably, the drying temperature is-50 to 150 ℃, and the drying time is 1 to 72 hours.
The second technical problem to be solved by the invention is to provide the heat-preservation and heat-insulation ball prepared by the preparation method.
The invention has the beneficial effects that:
(1) the heat-insulating ball is prepared by mixing and molding the heat-insulating material, the adhesive and the curing agent, and has light weight, good flame retardance and heat-insulating property;
(2) the preparation process of the heat-insulating ball provided by the invention is simple, operations such as rinsing and high temperature are not needed when the material is prepared, secondary pollution such as waste water and waste gas is not generated in the preparation process, and the heat-insulating ball has good economic benefit and environmental protection benefit.
Drawings
FIG. 1 is a photograph of a heat-insulating ball prepared in example 1 of the present invention;
FIG. 2 is a photograph showing the heat insulating ball prepared in example 1 of the present invention floating on the water surface.
Fig. 3 is a graph comparing the thermal conductivity of the thermal insulation balls prepared in example 1 of the present invention with that of the thermal insulation balls prepared in comparative example 1 of the present invention.
Detailed Description
The invention will be described in further detail below with reference to the drawings and examples of the specification.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
Preparation method of heat-preservation and heat-insulation ball
(1) Mixing 0.5g of water glass with 10mL of distilled water to prepare an adhesive solution;
(2) mixing 0.25g of acetic anhydride with 50mL of distilled water to prepare a curing agent solution;
(3) pouring 5g of silicon dioxide hollow microspheres into the prepared adhesive solution, stirring for 15min, and uniformly mixing at the stirring speed of 900r/min to obtain prefabricated slurry;
(4) dropwise adding the prefabricated slurry into a curing agent solution at a dropping speed of 1 drop per second, wherein the prefabricated slurry is spherical when dropping, enters the curing agent solution, is solidified into a sphere, and floats in the curing agent solution to obtain prefabricated slurry balls, so as to obtain prefabricated slurry balls;
(5) and (3) drying the prefabricated slurry balls in a constant-temperature drying box at 60 ℃ to obtain the heat-preservation and heat-insulation balls.
The experimental results are as follows: the first picture is a photograph of the heat preservation and insulation ball provided by the embodiment. The density of the thermal insulation ball prepared in the embodiment measured by a density measuring instrument is 0.6g/cm3The thermal conductivity was measured to be 0.03W/m.K by a thermal conductivity tester. And the second picture is a photo of the object of the heat-preservation and heat-insulation ball floating on the water surface.
Example 2
Preparation method of heat-preservation and heat-insulation ball
(1) Mixing 0.5g of polyvinyl alcohol with 50mL of cyclohexane to prepare an adhesive solution;
(2) mixing 0.15g of amino resin with 50mL of ethanol to prepare a curing agent solution;
(3) pouring 8g of polyimide aerogel into the prepared adhesive solution, stirring for 30min, and uniformly mixing at the stirring speed of 1200r/min to obtain prefabricated slurry;
(4) dropwise adding the prefabricated slurry into a curing agent solution at a dropping speed of 2 drops per second, wherein the prefabricated slurry is spherical when dropping, enters the curing agent solution, is solidified into a sphere, and floats in the curing agent solution to obtain prefabricated slurry balls, so as to obtain prefabricated slurry balls;
(5) and (3) drying the prefabricated slurry balls in a constant-temperature drying box at 80 ℃ to obtain the heat-preservation and heat-insulation balls.
The same identification and detection analyses as in example 1 above were carried out on the obtained sample to confirm that the density of the produced thermal insulating ball was 0.5g/cm3The thermal conductivity was 0.025W/mK.
Example 3
Preparation method of heat-preservation and heat-insulation ball
(1) Mixing 0.1g of polyimide with 20mL of distilled water to prepare an adhesive solution;
(2) mixing 0.15g of tertiary amine with 50mL of ethanol to prepare a curing agent solution;
(3) 2g of silicon dioxide aerogel is poured into the prepared adhesive solution and stirred for 30min to be uniformly mixed, and the stirring speed of the obtained prefabricated slurry is 2000 r/min;
(4) dropwise adding the prefabricated slurry into a curing agent solution at a dropping speed of 1 drop per second, wherein the prefabricated slurry is spherical when dropping, enters the curing agent solution, is solidified into a sphere, and floats in the curing agent solution to obtain prefabricated slurry balls, so as to obtain prefabricated slurry balls;
(5) and (3) drying the prefabricated slurry balls in a constant-temperature drying box at 60 ℃ to obtain the heat-preservation and heat-insulation balls.
The same identification and detection analyses as in example 1 above were carried out on the obtained sample to confirm that the density of the produced thermal insulating ball was 0.65g/cm3The thermal conductivity was 0.02W/mK.
Comparative example 1
(1) Mixing 0.5g of water glass with 10mL of distilled water to prepare an adhesive solution;
(2) mixing 0.25g of acetic anhydride with 50mL of distilled water to prepare a curing agent solution;
(3) pouring 5g of silicon dioxide solid microspheres into the prepared adhesive solution, stirring for 15min, and uniformly mixing at the stirring speed of 900r/min to obtain prefabricated slurry;
(4) dropwise adding the prefabricated slurry into a curing agent solution at the dropping speed of 1 drop per second to obtain prefabricated slurry balls;
(5) and (3) drying the prefabricated slurry balls in a constant-temperature drying box at 60 ℃ to obtain the heat-preservation and heat-insulation balls.
The experimental results are as follows: the density of the thermal insulation ball prepared in the embodiment measured by a density measuring instrument is 1.8g/cm3The heat conductivity coefficient measured by a heat conductivity coefficient tester is 0.56W/m.K, and the prepared heat-insulating ball has higher density. The comparative results are shown in FIG. 3.
Comparative example 2
(1) Mixing 0.5g of polyvinyl alcohol with 50mL of cyclohexane to prepare an adhesive solution;
(2) mixing 0.15g of amino resin with 50mL of ethanol to prepare a curing agent solution;
(3) pouring 8g of polyimide powder particles into the prepared adhesive solution, stirring for 30min, and uniformly mixing at the stirring speed of 1200r/min to obtain prefabricated slurry;
(4) dropwise adding the prefabricated slurry into a curing agent solution at a dropping speed of 2 drops per second, wherein the prefabricated slurry is spherical when dropping, enters the curing agent solution, is solidified into a sphere, and floats in the curing agent solution to obtain a prefabricated slurry ball;
(5) and (3) drying the prefabricated slurry balls in a constant-temperature drying box at 80 ℃ to obtain the heat-preservation and heat-insulation balls.
The same identification and detection analyses as in comparative example 1 above were carried out on the obtained sample to confirm that the density of the produced thermal insulating ball was 1.25g/cm3The heat conductivity coefficient is 0.5W/m.K, and the prepared heat preservation and insulation ball has higher density.
Comparative example 3
(1) Mixing 0.1g of polyimide with 20mL of distilled water to prepare an adhesive solution;
(2) mixing 0.15g of tertiary amine with 50mL of ethanol to prepare a curing agent solution;
(3) 2g of silicon dioxide powder particles are poured into the prepared adhesive solution and stirred for 30min to be uniformly mixed, and the stirring speed of the obtained prefabricated slurry is 2000 r/min;
(4) dropwise adding the prefabricated slurry into a curing agent solution at a dropping speed of 1 drop per second, wherein the prefabricated slurry is spherical when dropping, enters the curing agent solution, is solidified into a sphere, and floats in the curing agent solution to obtain prefabricated slurry balls, so as to obtain prefabricated slurry balls;
(5) and (3) drying the prefabricated slurry balls in a constant-temperature drying box at 60 ℃ to obtain the heat-preservation and heat-insulation balls.
The same identification and detection analyses as in comparative example 1 above were carried out on the obtained sample to confirm that the density of the produced thermal insulating ball was 1.75g/cm3The heat conductivity coefficient is 0.6W/m.K, and the prepared heat preservation and insulation ball has higher density.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and various process schemes having no substantial difference from the concept of the present invention are within the protection scope of the present invention.

Claims (7)

1. A preparation method of a heat preservation and insulation ball is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing an adhesive solution: mixing an adhesive with a solvent to obtain an adhesive solution; the adhesive comprises water glass, gypsum, polyvinyl acetate, cellulose ester, polyvinyl alcohol, perchloroethylene, polyisobutylene, polyacrylate, alpha-cyanoacrylate, polyvinyl acetal, epoxy resin, phenolic resin, urea-formaldehyde resin, melamine-formaldehyde resin, organic silicon resin, acrylic resin, polyimide, polybenzimidazole, phenolic-polyvinyl acetal and phenolic-epoxy resin, one or more of natural rubber, rosin, gelatin, cellulose, starch glue, chloroprene rubber, styrene-butadiene rubber, butyl rubber, sodium butadiene rubber, isoprene rubber, polysulfide rubber, polyurethane rubber, chlorosulfonated polyethylene, silicone rubber, phenol-butadiene rubber, phenol-chloroprene rubber, phenol resin-polyurethane rubber, epoxy resin-nitrile rubber, and epoxy resin-polysulfide rubber;
(2) preparing a curing agent solution: mixing a curing agent with a solvent to obtain a curing agent solution; the curing agent comprises one or more of acid anhydride, resol type phenolic resin, amino resin, dicyandiamide and hydrazide;
(3) uniformly mixing a heat-insulating material and an adhesive solution according to a certain proportion to obtain prefabricated slurry; the heat-insulating material comprises one or more of silicon dioxide aerogel, silicon dioxide hollow microspheres, polyimide aerogel, silicon carbide aerogel, boron nitride aerogel, silicon dioxide nanotubes, silicon carbide nanotubes and boron nitride nanotubes;
(4) dropwise adding the prefabricated slurry into a curing agent solution, wherein the prefabricated slurry is spherical when dropping, enters the curing agent solution, is cured into spheres, and floats in the curing agent solution to obtain prefabricated slurry balls;
(5) and drying the prefabricated slurry pellets to obtain the heat-insulating balls.
2. The preparation method of the heat-preservation and heat-insulation ball according to claim 1, characterized in that: the adhesive accounts for 0.05 to 50 weight percent of the solvent; the mass percentage of the curing agent in the solvent is 0.05-50 wt%.
3. The method of claim 1The preparation method of the heat preservation and insulation ball is characterized by comprising the following steps: the solvent comprises deionized water and C1-6One or more of alkanol, cyclohexane, octadecene and oleic acid.
4. The preparation method of the heat-preservation and heat-insulation ball according to claim 1, characterized in that: and dropwise adding the prefabricated slurry into the curing agent solution at a dropping speed of 0.25-5 drops per second.
5. The preparation method of the heat-preservation and heat-insulation ball according to claim 1, characterized in that: the drying method in the step (4) is one or more of steam drying, normal pressure drying, freeze drying and flash evaporation.
6. The preparation method of the heat-preservation and heat-insulation ball according to claim 1, characterized in that: the diameter of the prefabricated slurry small ball is 1-10 mm.
7. The heat-insulating ball prepared by the preparation method of the heat-insulating ball according to any one of claims 1 to 6.
CN201910792590.9A 2019-08-26 2019-08-26 Preparation method of heat preservation and insulation ball and prepared heat preservation and insulation ball Active CN110482997B (en)

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CN113119615B (en) * 2019-12-31 2023-02-03 昊佰电子科技(上海)有限公司 Non-sand-hole printing method for semitransparent material
CN111410438A (en) * 2020-04-27 2020-07-14 东莞市嘉镁光学电子有限公司 Wear-resisting vehicle-mounted glass outer screen
CN113637285A (en) * 2021-07-30 2021-11-12 万华建筑科技有限公司 Aerogel modified inorganic fiber adhesive and preparation process thereof
CN117466569B (en) * 2023-12-28 2024-04-12 北京玻钢院复合材料有限公司 Honeycomb structure reinforced aerogel-phenolic resin matrix composite material and preparation method thereof

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CN106672984A (en) * 2016-11-18 2017-05-17 陕西盛迈石油有限公司 Method for preparing millimeter hydrophobic SiO2 aerogel spheres through dripping method
CN108585798A (en) * 2018-05-09 2018-09-28 安徽中航名坤新材料科技有限公司 A kind of nano-porous alumina aeroge ceramic bead and preparation method thereof
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Denomination of invention: The invention relates to a preparation method of thermal insulation ball and the prepared thermal insulation ball

Effective date of registration: 20220308

Granted publication date: 20211022

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