CN110482997A - A kind of preparation method of thermal insulation separation hot-bulb and thermal insulation separation hot-bulb obtained - Google Patents

A kind of preparation method of thermal insulation separation hot-bulb and thermal insulation separation hot-bulb obtained Download PDF

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CN110482997A
CN110482997A CN201910792590.9A CN201910792590A CN110482997A CN 110482997 A CN110482997 A CN 110482997A CN 201910792590 A CN201910792590 A CN 201910792590A CN 110482997 A CN110482997 A CN 110482997A
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thermal insulation
insulation separation
bulb
agent solution
separation hot
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CN110482997B (en
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张尚权
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Anhui Keang Nanotechnology Co Ltd
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    • 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
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    • 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
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    • 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
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    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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    • 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
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    • 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

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Abstract

The present invention discloses a kind of preparation method of thermal insulation separation hot-bulb, is related to heat preserving and insulating material technical field, comprising the following steps: (1) mixes adhesive with solvent, configure gluing agent solution;Curing agent is mixed with solvent, configures curing agent solution;(2) heat preserving and insulating material and gluing agent solution are mixed in a certain ratio uniformly, obtain prefabricated slurry;(3) curing agent solution is added dropwise in prefabricated slurry, obtains prefabricated slurry bead;(4) prefabricated slurry bead is dry, obtain thermal insulation separation hot-bulb.The present invention also provides the thermal insulation separation hot-bulbs as made from above-mentioned preparation method, the beneficial effects of the present invention are: insulation ball prepared by the present invention has light-weighted effect, with good fire-retardant and heat-proof quality, simultaneously, thermal insulation separation hot-bulb simple process of the invention, yield is big, is suitble to industrial production.

Description

A kind of preparation method of thermal insulation separation hot-bulb and thermal insulation separation hot-bulb obtained
Technical field
The present invention relates to heat preserving and insulating material technical fields, and in particular to a kind of preparation method of thermal insulation separation hot-bulb and is made Thermal insulation separation hot-bulb.
Background technique
Current energy environment issues it is increasingly serious, to the effective use of the energy, more stringent requirements are proposed.In thermal insulation separation More environmentally protective efficient thermal insulation material is developed in hot field, and reducing energy loss has important strategic importance.
Light heat insulation material is a kind of light-weighted heat preserving and insulating material, and thermal insulation separation hot-bulb is with light-weighted insulation Spherical thermal insulation material made of material can be widely applied to a variety of filling field of thermal insulation.Patent CN201810463443.2 is public It has opened a kind of composite aerogel microballoon and preparation method thereof: having removed the graphite oxide ultrasound of preparation to obtain graphene oxide first Solution adds Ca2+、PO4 3-And Zn2+Solution, Ca2+With PO4 3-Molar ratio 1.17~2.17, hydroxyapatite and oxidation stone Black alkene mass ratio is 1:0.1~1:10, adds ammonium hydroxide, stirring forms composite dispersion liquid, is connect finally by spraying, cooling bath It receives, sieving, be freeze-dried and obtain composite aerogel microballoon, this method program is complex.Invent CN201810438091.5 Disclose a kind of nano-porous alumina aeroge ceramic bead and preparation method thereof: it is molten that SS01 configures the aluminium containing polyvinyl alcohol Glue;SS02 prepares oil ammonia column solution;SS03 balling-up;SS04 aging, supercritical drying;SS05 heat treatment.This method wants equipment Ask higher.
To sum up, material and the method for preparing environmental type thermal insulation separation hot-bulb at present are still relatively limited.Therefore, it still needs A kind of simply and easily method is wanted to prepare thermal insulation separation hot-bulb.
Summary of the invention
Present invention solves the technical problem that one of be that the preparation method of existing thermal insulation separation hot-bulb is complicated, a kind of guarantor is provided The preparation method of warm heat insulating ball.
The present invention adopts the following technical solutions solves above-mentioned technical problem:
The present invention provides a kind of preparation method of thermal insulation separation hot-bulb, comprising the following steps:
(1) it configures gluing agent solution: adhesive is mixed with solvent, obtain gluing agent solution;
(2) it configures curing agent solution: curing agent is mixed with solvent, obtain curing agent solution;
(3) heat preserving and insulating material and gluing agent solution are mixed in a certain ratio uniformly, obtain prefabricated slurry;
(4) prefabricated slurry is added dropwise curing agent solution, is spherical shape when prefabricated slurry drips, into curing agent solution, It is solidified into spherical shape, is swum in curing agent solution, prefabricated slurry bead is obtained;
(5) prefabricated slurry bead is dry, obtain thermal insulation separation hot-bulb.
Preferably, it is 0.05-50wt% that the adhesive, which accounts for the mass percent of solvent,;The curing agent accounts for the matter of solvent Amount percentage is 0.05-50wt%.
Preferably, the heat preserving and insulating material includes aerosil, SiO 2 hollow microsphere, polyimides gas Gel, carbonization silica aerogel, boron nitride aeroge, Silica Nanotube, Sic nanotube, one in boron nitride nano-tube Kind is a variety of.
Preferably, the adhesive includes waterglass, gypsum, polyvinyl acetate, cellulose esters, polyvinyl alcohol, crosses chlorine Ethylene, polyisobutene, polyacrylate, a-cyanoacrylate, Pioloform, polyvinyl acetal, epoxy resin, phenolic resin, ureaformaldehyde tree Rouge, melamine-formaldehyde resin, organic siliconresin, acrylic resin, polyimides, polybenzimidazoles, phenolic aldehyde-polyvinyl alcohol contracting Aldehyde, phenolic aldehyde-epoxy resin, natural rubber, rosin, gelatin, cellulose, amylan, neoprene, butadiene-styrene rubber, butyl rubber, Buna, isoprene rubber, polysulfide rubber, polyurethane rubber, chlorosulfonated polyethylene, silicon rubber, phenolic aldehyde-nitrile rubber, phenolic aldehyde-chlorine One of fourth glue, phenolic resin-polyurethane adhesive, epoxy resin-nitrile rubber, epoxy resin-polysulfide rubber are a variety of.
Preferably, the curing agent includes one of acid anhydrides, resol type phenol resin, amino resins, dicyandiamide, hydrazides Or it is a variety of.
The solvent includes deionized water, C1-6One of alkanol, hexamethylene, octadecylene, oleic acid are a variety of.
It preferably, is 0.25-5 drop per second by the rate of addition that curing agent solution is added dropwise in the prefabricated slurry.
Preferably, the drying means in the step (4) is steam drying, constant pressure and dry, freeze-drying, one in flash distillation Kind is a variety of.
Preferably, the diameter of the prefabricated slurry bead is 1-10mm.
Preferably, the drying temperature is -50~150 DEG C, and the drying time is 1-72h.
Present invention solves the technical problem that two be to provide a kind of thermal insulation separation hot-bulb as made from above-mentioned preparation method.
The beneficial effects of the present invention are:
(1) present invention has by the way that thermal insulation separation hot-bulb is made in heat preserving and insulating material, adhesive, curing agent mixed-forming Lightweight has good fire-retardant, heat-proof quality;
(2) thermal insulation separation hot-bulb preparation process flow provided by the invention is simple, without rinsing, high temperature etc. when preparing the material It operates, the secondary pollutions such as waste water, exhaust gas, with good economic efficiency and environmental benefit will not be generated in preparation process.
Detailed description of the invention
Fig. 1 is the picture of the thermal insulation separation hot-bulb prepared in the embodiment of the present invention 1;
Fig. 2 is the picture that the thermal insulation separation hot-bulb prepared in the embodiment of the present invention 1 is swum on the water surface.
Fig. 3 is the thermal coefficient of thermal insulation separation hot-bulb prepared in the embodiment of the present invention 1 and prepares in comparative example 1 of the present invention The thermal coefficient of thermal insulation separation hot-bulb contrasts figure.
Specific embodiment
The present invention is described in further details below with reference to Figure of description and embodiment.
Test material and reagent as used in the following examples etc., unless otherwise specified, commercially obtain.
In the examples where no specific technique or condition is specified, can according to the literature in the art described technology or Condition is carried out according to product description.
Embodiment 1
The preparation method of thermal insulation separation hot-bulb
(1) 0.5g waterglass is mixed with 10mL distilled water, configures gluing agent solution;
(2) 0.25g acetic anhydride is mixed with 50mL distilled water, configures curing agent solution;
(3) 5g SiO 2 hollow microsphere is poured into configured gluing agent solution and stirs 15min and be uniformly mixed, stirred Mixing speed is 900r/min, obtains prefabricated slurry;
(4) curing agent solution is added dropwise in prefabricated slurry, rate of addition is 1 drop per second, and prefabricated slurry drips Shi Weiqiu Shape is solidified into spherical shape into curing agent solution, swim in curing agent solution, obtains prefabricated slurry bead, obtains pre- slurrying Expect bead;
(5) prefabricated slurry bead is dry in 60 DEG C of thermostatic drying chamber, obtain thermal insulation separation hot-bulb.
Experimental result: figure one is thermal insulation separation hot-bulb material object photo provided in this embodiment.This is measured using penetron The density of thermal insulation separation hot-bulb obtained is 0.6g/cm in embodiment3, measuring thermal coefficient using heat conduction coefficient tester is 0.03W/m·K.Figure two is that above-mentioned thermal insulation separation hot-bulb swims in the photo in kind on the water surface.
Embodiment 2
The preparation method of thermal insulation separation hot-bulb
(1) 0.5g polyvinyl alcohol is mixed with 50mL hexamethylene, configures gluing agent solution;
(2) 0.15g amino resins is mixed with 50mL ethyl alcohol, configures curing agent solution;
(3) 8g polyimide aerogels are poured into configured gluing agent solution and stirs 30min and be uniformly mixed, stir Speed is 1200r/min, obtains prefabricated slurry;
(4) curing agent solution is added dropwise in prefabricated slurry, rate of addition is 2 drop per second, and prefabricated slurry drips Shi Weiqiu Shape is solidified into spherical shape into curing agent solution, swim in curing agent solution, obtains prefabricated slurry bead, obtains pre- slurrying Expect bead;
(5) prefabricated slurry bead is dry in 80 DEG C of thermostatic drying chamber, obtain thermal insulation separation hot-bulb.
Identification identical with above-described embodiment 1 and detection and analysis are carried out to resulting sample, determine insulation obtained The density of ball is 0.5g/cm3, thermal coefficient 0.025W/mK.
Embodiment 3
The preparation method of thermal insulation separation hot-bulb
(1) 0.1g polyimides is mixed with 20mL distilled water, configures gluing agent solution;
(2) 0.15g tertiary amine is mixed with 50mL ethyl alcohol, configures curing agent solution;
(3) 2g aerosil is poured into configured gluing agent solution and stirs 30min and be uniformly mixed, obtained Prefabricated slurry agitation speed is 2000r/min;
(4) curing agent solution is added dropwise in prefabricated slurry, rate of addition is 1 drop per second, and prefabricated slurry drips Shi Weiqiu Shape is solidified into spherical shape into curing agent solution, swim in curing agent solution, obtains prefabricated slurry bead, obtains pre- slurrying Expect bead;
(5) prefabricated slurry bead is dry in 60 DEG C of thermostatic drying chamber, obtain thermal insulation separation hot-bulb.
Identification identical with above-described embodiment 1 and detection and analysis are carried out to resulting sample, determine insulation obtained The density of ball is 0.65g/cm3, thermal coefficient 0.02W/mK.
Comparative example 1
(1) 0.5g waterglass is mixed with 10mL distilled water, configures gluing agent solution;
(2) 0.25g acetic anhydride is mixed with 50mL distilled water, configures curing agent solution;
(3) 5g silica solid microsphere is poured into configured gluing agent solution and stirs 15min and be uniformly mixed, stirred Mixing speed is 900r/min, obtains prefabricated slurry;
(4) curing agent solution is added dropwise in prefabricated slurry, rate of addition is 1 drop per second, obtains prefabricated slurry bead;
(5) prefabricated slurry bead is dry in 60 DEG C of thermostatic drying chamber, obtain thermal insulation separation hot-bulb.
Experimental result: being 1.8g/ using the density that penetron measures thermal insulation separation hot-bulb obtained in the present embodiment cm3, surveying thermal coefficient using heat conduction coefficient tester is 0.56W/mK, and thermal insulation separation hot-bulb density obtained is larger.Comparison knot Fruit is as shown in Figure 3.
Comparative example 2
(1) 0.5g polyvinyl alcohol is mixed with 50mL hexamethylene, configures gluing agent solution;
(2) 0.15g amino resins is mixed with 50mL ethyl alcohol, configures curing agent solution;
(3) 8g polyimide powder particle is poured into configured gluing agent solution and stirs 30min and be uniformly mixed, stirred Mixing speed is 1200r/min, obtains prefabricated slurry;
(4) curing agent solution is added dropwise in prefabricated slurry, rate of addition is 2 drop per second, and prefabricated slurry drips Shi Weiqiu Shape is solidified into spherical shape into curing agent solution, swim in curing agent solution, obtains prefabricated slurry bead;
(5) prefabricated slurry bead is dry in 80 DEG C of thermostatic drying chamber, obtain thermal insulation separation hot-bulb.
Identification identical with above-mentioned comparative example 1 and detection and analysis are carried out to resulting sample, determine insulation obtained The density of ball is 1.25g/cm3, thermal coefficient 0.5W/mK, thermal insulation separation hot-bulb density obtained is larger.
Comparative example 3
(1) 0.1g polyimides is mixed with 20mL distilled water, configures gluing agent solution;
(2) 0.15g tertiary amine is mixed with 50mL ethyl alcohol, configures curing agent solution;
(3) 2g SiO 2 powder particle is poured into configured gluing agent solution and stirs 30min and be uniformly mixed, obtained It is 2000r/min to prefabricated slurry agitation speed;
(4) curing agent solution is added dropwise in prefabricated slurry, rate of addition is 1 drop per second, and prefabricated slurry drips Shi Weiqiu Shape is solidified into spherical shape into curing agent solution, swim in curing agent solution, obtains prefabricated slurry bead, obtains pre- slurrying Expect bead;
(5) prefabricated slurry bead is dry in 60 DEG C of thermostatic drying chamber, obtain thermal insulation separation hot-bulb.
Identification identical with above-mentioned comparative example 1 and detection and analysis are carried out to resulting sample, determine insulation obtained The density of ball is 1.75g/cm3, thermal coefficient 0.6W/mK, thermal insulation separation hot-bulb density obtained is larger.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment, It is within the scope of the invention with present inventive concept without the various process programs of substantial differences.

Claims (10)

1. a kind of preparation method of thermal insulation separation hot-bulb, it is characterised in that: the following steps are included:
(1) it configures gluing agent solution: adhesive is mixed with solvent, obtain gluing agent solution;
(2) it configures curing agent solution: curing agent is mixed with solvent, obtain curing agent solution;
(3) heat preserving and insulating material and gluing agent solution are mixed in a certain ratio uniformly, obtain prefabricated slurry;
(4) curing agent solution is added dropwise in prefabricated slurry, is spherical shape when prefabricated slurry drips, it is into curing agent solution, i.e., solid Chemical conversion is spherical, swims in curing agent solution, obtains prefabricated slurry bead;
(5) prefabricated slurry bead is dry, obtain thermal insulation separation hot-bulb.
2. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: the adhesive accounts for the matter of solvent Amount percentage is 0.05-50wt%;The mass percent that the curing agent accounts for solvent is 0.05-50wt%.
3. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: the heat preserving and insulating material includes Aerosil, SiO 2 hollow microsphere, polyimide aerogels, carbonization silica aerogel, boron nitride aeroge, dioxy One of SiClx nanotube, Sic nanotube, boron nitride nano-tube are a variety of.
4. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: the adhesive includes water glass Glass, gypsum, polyvinyl acetate, cellulose esters, polyvinyl alcohol, Vinylidene Chloride, polyisobutene, polyacrylate, alpha-cyano third Olefin(e) acid ester, Pioloform, polyvinyl acetal, epoxy resin, phenolic resin, Lauxite, melamine-formaldehyde resin, organic siliconresin, third It is olefin(e) acid resin, polyimides, polybenzimidazoles, phenolic aldehyde-Pioloform, polyvinyl acetal, phenolic aldehyde-epoxy resin, natural rubber, rosin, bright Glue, cellulose, amylan, neoprene, butadiene-styrene rubber, butyl rubber, buna, isoprene rubber, polysulfide rubber, polyurethane Rubber, chlorosulfonated polyethylene, silicon rubber, phenolic aldehyde-nitrile rubber, phenolic aldehyde-neoprene, phenolic resin-polyurethane adhesive, epoxy resin- One of nitrile rubber, epoxy resin-polysulfide rubber are a variety of.
5. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: the curing agent include acid anhydrides, One of resol type phenol resin, amino resins, dicyandiamide, hydrazides are a variety of.
6. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: the solvent includes deionization Water, C1-6One of alkanol, hexamethylene, octadecylene, oleic acid are a variety of.
7. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: add the prefabricated slurry dropwise The rate of addition for entering curing agent solution is 0.25~5 drop per second.
8. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: the drying in the step (4) Method is one of steam drying, constant pressure and dry, freeze-drying, flash distillation or a variety of.
9. the preparation method of thermal insulation separation hot-bulb according to claim 1, it is characterised in that: the prefabricated slurry bead it is straight Diameter is 1-10mm.
10. thermal insulation separation hot-bulb made from the preparation method using thermal insulation separation hot-bulb of any of claims 1-9.
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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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
CN113119615A (en) * 2019-12-31 2021-07-16 昊佰电子科技(上海)有限公司 Non-sand-hole printing method for semitransparent material
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
CN117466569A (en) * 2023-12-28 2024-01-30 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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CN113119615A (en) * 2019-12-31 2021-07-16 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
CN117466569A (en) * 2023-12-28 2024-01-30 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
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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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

Pledgee: Dingyuan county development industry guidance fund management center (L.P.)

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