CN116925421A - Thermal insulation foam material based on cellulose-muscovite-zinc oxide and preparation method thereof - Google Patents
Thermal insulation foam material based on cellulose-muscovite-zinc oxide and preparation method thereof Download PDFInfo
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- CN116925421A CN116925421A CN202310876637.6A CN202310876637A CN116925421A CN 116925421 A CN116925421 A CN 116925421A CN 202310876637 A CN202310876637 A CN 202310876637A CN 116925421 A CN116925421 A CN 116925421A
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- Prior art keywords
- cellulose
- zinc oxide
- muscovite
- foam material
- mass
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 67
- 239000000463 material Substances 0.000 title claims abstract description 54
- 239000002937 thermal insulation foam Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 87
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000007787 solid Substances 0.000 claims abstract description 83
- 229920002678 cellulose Polymers 0.000 claims abstract description 80
- 239000001913 cellulose Substances 0.000 claims abstract description 80
- 239000012153 distilled water Substances 0.000 claims abstract description 72
- 238000003756 stirring Methods 0.000 claims abstract description 60
- 239000007864 aqueous solution Substances 0.000 claims abstract description 58
- 238000005406 washing Methods 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 49
- 239000006261 foam material Substances 0.000 claims abstract description 47
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 42
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 42
- 239000000126 substance Substances 0.000 claims abstract description 41
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052627 muscovite Inorganic materials 0.000 claims abstract description 38
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001914 filtration Methods 0.000 claims abstract description 30
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 28
- GRTOGORTSDXSFK-XJTZBENFSA-N ajmalicine Chemical compound C1=CC=C2C(CCN3C[C@@H]4[C@H](C)OC=C([C@H]4C[C@H]33)C(=O)OC)=C3NC2=C1 GRTOGORTSDXSFK-XJTZBENFSA-N 0.000 claims abstract description 28
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 28
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 28
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 28
- KSVSZLXDULFGDQ-UHFFFAOYSA-M sodium;4-aminobenzenesulfonate Chemical compound [Na+].NC1=CC=C(S([O-])(=O)=O)C=C1 KSVSZLXDULFGDQ-UHFFFAOYSA-M 0.000 claims abstract description 28
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims abstract description 27
- 229960002218 sodium chlorite Drugs 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 238000004108 freeze drying Methods 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 230000005496 eutectics Effects 0.000 claims abstract description 19
- 239000002023 wood Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 78
- 239000011268 mixed slurry Substances 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 44
- 239000002002 slurry Substances 0.000 claims description 43
- 239000011259 mixed solution Substances 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 16
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 10
- 241000219000 Populus Species 0.000 claims description 8
- 241000121220 Tricholoma matsutake Species 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 240000008042 Zea mays Species 0.000 claims description 5
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 5
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 5
- 235000005822 corn Nutrition 0.000 claims description 5
- 239000002699 waste material Substances 0.000 claims description 5
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 3
- 235000019743 Choline chloride Nutrition 0.000 claims description 3
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 3
- 229960003178 choline chloride Drugs 0.000 claims description 3
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical compound O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 description 22
- 239000012895 dilution Substances 0.000 description 22
- 229920005610 lignin Polymers 0.000 description 22
- 239000006260 foam Substances 0.000 description 20
- 239000011148 porous material Substances 0.000 description 17
- 238000009413 insulation Methods 0.000 description 14
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 14
- 238000005266 casting Methods 0.000 description 12
- 239000004964 aerogel Substances 0.000 description 9
- 239000012774 insulation material Substances 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 239000002055 nanoplate Substances 0.000 description 4
- 239000002135 nanosheet Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
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- 230000000694 effects Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000012779 reinforcing material Substances 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 244000235858 Acetobacter xylinum Species 0.000 description 1
- 235000002837 Acetobacter xylinum Nutrition 0.000 description 1
- 229920002749 Bacterial cellulose Polymers 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000005016 bacterial cellulose Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011140 metalized polyester Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000008104 plant cellulose Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0033—Use of organic additives containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/052—Closed cells, i.e. more than 50% of the pores are closed
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
- C08J2301/12—Cellulose acetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Emergency Medicine (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention relates to the field of thermal management materials, in particular to a thermal insulation foam material based on cellulose-muscovite-zinc oxide and a preparation method thereof, wherein the preparation method comprises the following steps: adding powdery wood raw materials with cellulose content of more than 35% into a deep eutectic solvent, heating and stirring, filtering and washing to obtain a solid substance I, dispersing the solid substance I in sodium chlorite aqueous solution, adding acetic acid, heating and stirring, filtering and washing to obtain a solid substance II, dispersing the solid substance II in distilled water, performing cell disruption treatment, adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose, ball milling for 12-16 h, adding polyvinyl alcohol aqueous solution and glutaraldehyde, stirring uniformly, transferring into a mold, freeze-drying, and demolding to obtain the heat-insulating foam material.
Description
Technical Field
The invention relates to the field of thermal management materials, in particular to a thermal insulation foam material based on cellulose-muscovite-zinc oxide and a preparation method thereof.
Background
The indoor temperature is 18-25 ℃, so people feel the most comfortable, various methods can be used for keeping the indoor temperature in the range, a large amount of energy is consumed for the operation every year, and the energy consumption can be reduced by selecting a high-energy-efficiency building enclosure structure (namely, the enclosure of each side of a building and a room, such as a door, a window, a wall and the like, which can effectively resist adverse environmental effects under the condition that little or no additional energy is supplied), and the energy consumption can be reduced by reducing the energy exchange (mainly by heat conduction, convection and emission) between the indoor and the outdoor, most of heat is blocked outside a building wall in summer, and the loss of the indoor energy to the external environment can be reduced in winter, so that the indoor comfort can be still maintained to a great extent under the condition that the energy consumption is reduced by people.
The building enclosure structure with high energy efficiency is generally made of high-heat-insulation materials, common heat-insulation materials are mainly divided into porous materials, heat-reflection materials and vacuum heat-insulation materials, and the heat conductivity coefficient of air or inert gas in pores of the porous materials is very low, so that the porous materials are mainly used for heat insulation by utilizing the pores of the porous materials, such as foam materials, fiber materials and the like; the heat reflecting material has high reflection coefficient, and can reflect heat, such as gold, silver, nickel, aluminum foil or metallized polyester, polyimide film and the like; the vacuum heat insulation material achieves the purpose of heat insulation by utilizing the vacuum barrier convection inside the material. Besides being used as a building enclosure structure, the heat insulation material can be widely applied to other scenes.
Along with the environmental protection concept becoming a focus of development, in recent years, environment-friendly heat insulation materials become a hot spot, in the development process, it is found that cellulose is a natural polymer material very suitable for preparing environment-friendly heat insulation materials, cellulose reserves are abundant, wide sources are provided, plant cellulose materials can be extracted from straws, cotton, wood and the like, bacterial cellulose can be extracted from acetobacter xylinum and the like, regenerated cellulose can be extracted from newspapers, cartons and the like, cellulose also has the advantages of low price, degradability, reproducibility, no toxicity, no harm, easiness in modification and the like, cellulose is utilized to develop the heat insulation material based on cellulose, namely cellulose-based aerogel, the cellulose-based aerogel is a solid material with a nano three-dimensional porous network structure, the pores of the cellulose-based aerogel are filled with a gaseous dispersion medium, the cellulose-based aerogel has the advantages of high porosity, low thermal conductivity, ultra-low density and the like, and the cellulose-based aerogel can be subjected to proper modification treatment, so that the cellulose-based aerogel can be endowed with the performances of adsorption, heat insulation, sound insulation, water resistance and the like, and is particularly suitable for being applied to the fields of energy storage, heat insulation, catalyst carrier, adsorbent, electromagnetic shielding and the like, aviation industry and the like. However, although the cellulose-based aerogel has good heat insulation performance, the cellulose-based aerogel is easy to break, has poor mechanical stability and is complex in preparation method.
Therefore, the existing cellulose-based heat insulation material also has the problems of poor mechanical stability and complex preparation method.
Disclosure of Invention
The present invention aims to overcome the drawbacks of the prior art and to provide a thermal insulation foam based on cellulose-muscovite-zinc oxide (hereinafter referred to simply as "thermal insulation foam") having a good thermal insulation performance and a good mechanical stability, and a simpler method for preparing the thermal insulation foam.
The technical scheme adopted for solving the technical problems is as follows: the invention provides a preparation method of a thermal insulation foam material based on cellulose-muscovite-zinc oxide, which comprises the following steps:
step 1: adding powdery wood raw materials with cellulose content of more than 35% into a deep eutectic solvent, wherein the volume mass ratio of the deep eutectic solvent to the powdery wood raw materials is 100: (1-1.5) mL/g, heating and stirring, adding distilled water, filtering and washing for multiple times to obtain a solid substance I;
step 2: dispersing the solid substance I obtained in the step 1 into 15-25 g/L sodium chlorite aqueous solution, adding acetic acid with the concentration of 99.5%, and the mass of the solid substance I: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g: (100-150) mL: (1-2) mL, heating and stirring, adding distilled water, filtering and washing for multiple times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 12-15 mg/mL, and carrying out cell disruption treatment on the aqueous dispersion liquid A for 60-180 min to obtain esterified cellulose slurry;
Step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is (120-180) mL:1 g/g (0.5-1.2) g/g (0.5-1) g/g (1.5-2) and ball milling for 12-16 h to obtain mixed slurry B;
step 4: adding 10wt% of polyvinyl alcohol aqueous solution and 95wt% of glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of (120-180) mL to (50-60) mL to (2-5) mL to obtain a mixed solution C, transferring the mixed solution C into a mold, freeze-drying the mixed solution C, and demolding to obtain the heat-insulating foam material based on cellulose-muscovite-zinc oxide.
Further, the preparation method of the deep eutectic solvent in the step 1 comprises the following steps: according to 1:1, weighing choline chloride and oxalic acid dihydrate according to the mass ratio, uniformly mixing, heating at 90 ℃ until the mixture is melted into transparent liquid, and mixing the transparent liquid with the following components: distilled water is 1:100 volume ratio of distilled water is weighed and added into transparent liquid, and the mixture is uniformly mixed.
Further, the powdery wood raw material with the cellulose content of more than 35% in the step 1 is one or a mixture of more than one of poplar powder, ba Sha Mufen, pine mushroom powder, lignocellulose waste and corn stalk powder.
Further, the heating temperature in the step 1 is 120-150 ℃, the stirring time is 60-90 min, and the filtering and the water washing are carried out for 3-5 times.
Further, the heating temperature in the step 2 is 90-110 ℃, the stirring time is 3-5 h, and the filtering and the water washing are carried out for 3-5 times.
Further, the power of the cell disruption treatment in the above step 2 is 800 to 1000W.
Further, the preparation method of the nano zinc oxide in the step 3 comprises the following steps: zinc nitrate hexahydrate is dissolved in distilled water to obtain a solution E with the concentration of 0.02mol/L, and the solution E is prepared according to the volume of the distilled water: the molar mass of the sodium hydroxide is 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times with water, washing for 3 times with ethanol, and vacuum drying for 12 hours at 60-80 ℃.
Further, the aqueous solution of polyvinyl alcohol in the step 4 is 10wt% of the aqueous solution of polyvinyl alcohol.
Further, the freeze-drying temperature in the step 4 is-55 to-65 ℃ and the time is 36 to 48 hours.
The invention provides a thermal insulation foam material based on cellulose-muscovite-zinc oxide, which is prepared by any one of the preparation methods of the thermal insulation foam material based on cellulose-muscovite-zinc oxide.
The beneficial effects of the invention are as follows: the heat insulation foam material provided by the invention has better heat insulation performance and better mechanical stability. The heat-insulating foam material can well shield ultraviolet light and reflect heat, the surface temperature can be reduced under illumination, and meanwhile, only few tiny holes are found on the surface of the heat-insulating foam material, so that the heat-insulating foam material has higher closed porosity, lower heat conductivity and more excellent heat-insulating performance. The heat-insulating foam material has a self-reinforced structure based on the entanglement of the esterified cellulose frames, the muscovite nano-sheets can be filled in the heat-insulating foam material to be used as a reinforcing material to effectively ensure the structural stability of a cross-linked framework, the polyvinyl alcohol can play a role in gluing in the interweaved frames, and under the combined action of the polyvinyl alcohol and the reinforcing material, the heat-insulating foam material has higher mechanical strength and higher tensile strength, and is rigid in fracture and has better mechanical stability.
In addition, the heat-insulating foam material has better acid and alkali resistance, heat resistance and water stability, and the heat-insulating foam material contains a polymer material, namely polyvinyl alcohol, wherein the polyvinyl alcohol can further fill pores in the heat-insulating foam material, and the polyvinyl alcohol can interact with esterified cellulose under the action of glutaraldehyde to reduce active group sites such as hydroxyl, carbonyl and the like on an esterified cellulose molecular chain, so that the structure of the heat-insulating foam material is effectively prevented from being damaged by water molecules.
The preparation method of the heat-insulating foam material is simple, and firstly, esterified cellulose is extracted from powdery wood raw materials with cellulose content of more than 35% by adopting one-step solvent encapsulation treatment and chlorination process to prepare esterified cellulose slurry; secondly, converting zinc salt into nano zinc oxide clusters by using a water bath stirring method; adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethylcellulose into esterified cellulose slurry for ball milling treatment, further finishing fibrillation of cellulose through ball milling, further opening the structures of large fibers and coarse fibers, providing rich hydrogen bond binding sites for the construction of cellulose fibril crosslinked frames, simultaneously introducing muscovite powder with excellent mechanical stability and heat resistance, realizing in-situ stripping of muscovite nano-sheets in the ball milling process, loading zinc oxide nano-particles into an interweaving layer, solving the problem of uneven dispersion caused by direct mutual combination, greatly absorbing the energy of ultraviolet wave bands, and improving the heat insulation performance of foam wiping materials; and finally, adding a polymer and a cross-linking agent into the mixture slurry, and performing freeze drying treatment to form the heat-insulating foam material. The preparation method involves conventional steps, is simple and easy to operate, uses the wood raw materials with low price, does not involve any toxic solvent for the treatment of the wood raw materials, and is environment-friendly and pollution-free in the whole preparation process. Therefore, the preparation method is simple and easy to operate, low in cost, pollution-free and suitable for industrial mass production.
Drawings
FIG. 1 is a macroscopic photograph of the insulating foam prepared in example 1;
FIG. 2 is a photomicrograph of an optical microscope of the insulating foam material prepared in example 1;
FIG. 3 is a TEM image of muscovite nanoplatelets in example 1;
FIG. 4 is an SEM image of nano-zinc oxide clusters prepared in example 1;
FIG. 5 is a graph showing the mechanical properties of the insulating foam prepared in example 2;
FIG. 6 is a graph showing the acid and alkali resistance of the insulating foam prepared in example 2;
FIG. 7 is a graph showing the thermal insulation performance test of the thermal insulation foam material prepared in example 2;
FIG. 8 is a graph showing the heat stability test of the insulating foam material prepared in example 3;
FIG. 9 is a graph showing the ultraviolet-visible-near infrared light absorption and reflection performance of the insulating foam material prepared in example 4.
Detailed Description
The invention will be further described with reference to the drawings and the specific embodiments.
The particle size of the powdery wood raw material having a cellulose content of 35% or more used in each of the following examples was 100 mesh.
The preparation method of the deep eutectic solvent used in the following examples is as follows: according to 1:1, weighing choline chloride and oxalic acid dihydrate according to the mass ratio, uniformly mixing, heating at 90 ℃ until the mixture is melted into transparent liquid, and mixing the transparent liquid with the following components: distilled water is 1:100 volume ratio of distilled water is weighed and added into transparent liquid, and the mixture is uniformly mixed.
The concentration of acetic acid used in the following examples was 99.5% and the mass fraction of glutaraldehyde was 95% by weight.
The aqueous polyvinyl alcohol solutions used in the following examples were prepared by: the solid polyvinyl alcohol having a molecular weight of 145000 was dispersed in water at 95℃and dissolved to prepare a 10wt% aqueous polyvinyl alcohol solution.
In the following examples, KH20A type desk-top high-speed centrifuge was used as the apparatus for centrifugation, DZF-6050 type vacuum drying oven was used as the apparatus for cell disruption treatment, QM-3SP04 type planetary ball mill was used as the apparatus for ball milling, and SCIENTZ-10N/A type freeze dryer was used as the apparatus for freeze drying.
[ example 1 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by distilled water, washing for 3 times by ethanol, and finally drying in vacuum for 12 hours at 60 ℃ to obtain nano zinc oxide clusters, wherein a large amount of zinc oxide nano particles are agglomerated after being generated in a solvent to form the nano zinc oxide clusters with relatively uniform shape and size as shown in figure 4.
(2) Preparation of insulating foam
Step 1: adding 1g of poplar powder into 100mL of deep eutectic solvent, continuously stirring at 120 ℃ for 60min to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 3 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:100mL:1mL, continuously heating and stirring for 5h at 90 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 3 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 12mg/mL, and carrying out cell disruption treatment for 60min at the power of 800W to obtain esterified cellulose slurry;
step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 120mL:1 g/0.5 g, ball milling for 12h to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
Step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of 120mL to 50mL to 2mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at the temperature of minus 60 ℃ for 36 hours, and demoulding to obtain the heat-insulating foam material.
As shown in FIG. 1, the heat-insulating foam material after demolding from the mold still keeps the original structure, no collapse occurs, no obvious pore holes and other defect structures are observed on the surface of the heat-insulating foam material, and the heat-insulating foam material has the advantage of expanding preparation on the aspect of macroscopic scale, and can be prepared into various shapes meeting the use requirement by compression molding.
As shown in fig. 2, from a microscopic view, only few tiny holes are found on the surface of the heat insulation foam material, because the heat insulation foam material is a bionic structure similar to that of building construction, esterified cellulose frames are interwoven with each other to construct a main body of the heat insulation foam material, and white mica nano-sheets, micro-nano-level cellulose and nano zinc oxide generated by in-situ stripping are jointly combined in the cellulose frames to construct an interweaved structure. Under the action of glutaraldehyde, the polyvinyl alcohol can further strengthen the frame of the heat-insulating foam material through the adhesive action, so that the frame has higher mechanical strength, and meanwhile, the polyvinyl alcohol can also fill redundant pores of the heat-insulating foam material, so that the pores in the frame are eliminated to a great extent, and therefore, the heat-insulating foam material has higher closed porosity, and under the condition that the porosity is the same, the smaller the pore size is, the smaller the heat conductivity is; the more the interconnected pores, the higher the heat conductivity, the higher the closed pore ratio, the lower the heat conductivity, because after the foam material absorbs moisture and is wetted, the moisture (including water vapor) exists in the pores, at this time, the diffusion of the steam and the movement of water molecules in the pores play a main role in heat transfer, and the heat conductivity of the water is about 20 times greater than that of the air, so that the effective heat conductivity of the foam material is obviously improved, if the water in the pores is frozen, the heat conductivity of the ice is greater, and the heat conductivity of the material is increased more. The insulating foam material has lower heat conductivity, more excellent heat insulating performance and higher mechanical stability.
As shown in fig. 3, after ball milling, the muscovite powder is peeled off to form a few-layer nano-plate with transverse dimensions distributed on the micrometer scale, the muscovite nano-plate is helpful to strengthen the mechanical strength of the frame of the heat insulation foam material and further endow the heat insulation foam material with higher mechanical stability, and the muscovite nano-plate is used as a heat insulation and high temperature resistant material and can also promote the heat insulation performance of the heat insulation foam material.
[ example 2 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally drying in vacuum at 80 ℃ for 12 hours to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.5g of poplar powder into 100mL of deep eutectic solvent, continuously stirring at 150 ℃ for 90min to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 5 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:150mL:2mL, continuously heating and stirring for 3h at 110 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 5 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 13mg/mL, and carrying out cell disruption treatment for 180min at the power of 1000W to obtain esterified cellulose slurry;
Step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 180mL:1g to 1.2g to 1g to 2g, ball milling for 16 hours to ensure that the components are mixed more uniformly, obtaining mixed slurry B after finishing, and transferring the mixed slurry B into a clean container;
step 4: adding polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of 180mL to 60mL to 5mL to obtain a mixed solution C, casting the mixed solution C into a mould, freeze-drying the mixed solution C at the temperature of minus 60 ℃ for 48 hours, and demoulding to obtain the heat-insulating foam material.
Comparative example 1
Casting the esterified cellulose slurry obtained in the step 2 in the example 2 into a mould, freeze-drying at the temperature of minus 60 ℃ for 48 hours, and demoulding to obtain a comparative sample, namely esterified cellulose foam.
As shown in fig. 5, the soft esterified cellulose foam is converted into a rigid structural material with high mechanical strength based on the inter-entangled self-reinforcing structure of the cellulose frame, the filling of the muscovite nano-sheets to the insulating foam material at a microscopic scale, and the adhesive action of polyvinyl alcohol in the interlaced frame. The thermal insulation foam material prepared in example 2 was tested for tensile properties, and the maximum load bearing capacity reached 17.8N, and exhibited rigid cracking, and the thermal insulation foam material had higher strength, longer service life, and great difference from the conventional cellulose-based aerogel foam material.
As shown in fig. 6, the heat insulation foam material prepared in example 2 was immersed in a strong alkali solution having ph=14 and a strong acid solution having ph=1, respectively, and the mass loss was measured, and the mass loss of the heat insulation foam material after immersing in the strong acid and strong alkali solutions for 120min was less than 0.8%, and the mass remaining was greater than 99.2%, and the heat insulation foam material had excellent acid and alkali resistance.
As shown in FIG. 7, the heat resistance of the heat insulation foam material prepared in example 2 was significantly better than that of the esterified cellulose foam prepared in comparative example 1, and the optical power density was 100mW/cm 2 The surface temperature of the insulating foam material showed a significant decrease of 70.5% compared to the esterified cellulose foam, indicating that the introduction of the functional filler greatly improved the thermal insulation properties and the insulating effect of the insulating foam material.
[ example 3 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally drying in vacuum at 70 ℃ for 12 hours to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.3g of poplar powder into 100mL of deep eutectic solvent, continuously stirring at 130 ℃ for 75min to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 4 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:130mL:1.5mL, continuously heating and stirring for 4h at 110 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 4 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 14mg/mL, and carrying out cell disruption treatment for 150min at 900W power to obtain esterified cellulose slurry;
step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 150mL:1g to 1g, 0.8g to 1.5g, ball milling for 16 hours to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
Step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with a volume ratio of 150mL to 55mL to 3mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at-60 ℃ for 40h, and demoulding to obtain the heat-insulating foam material.
As shown in FIG. 8, the heat-resistant stability test was conducted on the heat-insulating foam material prepared in example 3, and irradiation with solar light was simulated by using a xenon lamp at an optical power density of 100mW/cm 3 Under conditions of (about 1 solar energy) irradiation for 180 minutes, the final surface temperature of the insulating foam reached 35.6 ℃ and under continued irradiation, the final thermal mass loss was less than 0.9%, mainly due to the almost complete loss of water in the mixed slurry B after sublimation during freeze-drying, resulting in a dense integrated structure of the components. Meanwhile, zinc oxide and the in-situ generated muscovite nano-plate also participate in the cross-linked framework structure of esterified cellulose, so that the heat-insulating foam material has excellent mechanical stability and heat resistance.
[ example 4 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally drying in vacuum at 80 ℃ for 12 hours to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.2g of poplar powder into 100mL of deep eutectic solvent, continuously stirring at 120 ℃ for 60min to fully dissolve lignin, adding distilled water for dilution, filtering and washing 3 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:150mL:1.5mL, continuously heating and stirring for 3h at 110 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 5 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 15mg/mL, and carrying out cell disruption treatment for 180min at the power of 1000W to obtain esterified cellulose slurry;
Step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 150mL:1 g/1.2 g/0.8 g/1.5 g, ball milling for 16h to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with a volume ratio of 150mL to 60mL to 4mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at the temperature of minus 60 ℃ for 48 hours, and demoulding to obtain the heat-insulating foam material.
As shown in fig. 9, the reflectance of the thermal insulation foam material prepared in example 4 is drastically reduced in the wavelength range of 200 to 380nm, because the nano zinc oxide has absorption and scattering effects on ultraviolet light, so that the nano zinc oxide can well shield ultraviolet light; in the wavelength range of visible light (380-780 nm) -near infrared (780-1500 nm), the heat insulation foam material has higher reflectivity which can reach 97.5-99.8%, which shows that the heat insulation foam material has obvious effect on heat reflection, and the heat insulation foam material has excellent heat insulation performance.
[ example 5 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally vacuum drying for 12 hours at 60 ℃ to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.25g of bar Sha Mufen into 100mL of deep eutectic solvent, continuously stirring at 135 ℃ for 75min to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 4 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into 15g/L sodium chlorite aqueous solution and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:125mL:1mL, continuously heating and stirring for 4h at 100 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 4 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 15mg/mL, and carrying out cell disruption treatment for 120min at the power of 1000W to obtain esterified cellulose slurry;
Step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 120mL:1 g/0.85 g/0.75 g, ball milling for 14h to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of 120mL to 60mL to 4mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at the temperature of minus 55 ℃ for 42h, and demoulding to obtain the heat-insulating foam material.
[ example 6 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally drying in vacuum at 75 ℃ for 12 hours to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.25g of pine mushroom powder into 100mL of deep eutectic solvent, continuously stirring at 140 ℃ for 80min to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 5 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 25g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:120mL:2mL, continuously heating and stirring for 5h at 95 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 3 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 13mg/mL, and carrying out cell disruption treatment for 100min at 900W power to obtain esterified cellulose slurry;
step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 120mL:1 g/0.8 g/0.6 g/1.8 g, ball milling for 13h to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
Step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of 120mL to 50mL to 2mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at the temperature of-65 ℃ for 36h, and demoulding to obtain the heat-insulating foam material.
[ example 7 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally vacuum drying for 12 hours at 60 ℃ to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1g of lignocellulose waste into 100mL of deep eutectic solvent, continuously stirring at 120 ℃ for 60min to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 3 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:100mL:1mL, continuously heating and stirring for 5h at 90 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 3 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 12mg/mL, and carrying out cell disruption treatment for 60min at the power of 800W to obtain esterified cellulose slurry;
Step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 120mL:1 g/0.5 g, ball milling for 12h to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of 120mL to 50mL to 2mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at the temperature of minus 60 ℃ for 36 hours, and demoulding to obtain the heat-insulating foam material.
[ example 8 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally drying in vacuum at 80 ℃ for 12 hours to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.5g of corn stalk powder into 100mL of deep eutectic solvent, continuously stirring at 150 ℃ for 90min to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 5 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:150mL:2mL, continuously heating and stirring for 3h at 110 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 5 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 13mg/mL, and carrying out cell disruption treatment for 180min at the power of 1000W to obtain esterified cellulose slurry;
step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 180mL:1g to 1.2g to 1g to 2g, ball milling for 16 hours to ensure that the components are mixed more uniformly, obtaining mixed slurry B after finishing, and transferring the mixed slurry B into a clean container;
Step 4: adding polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of 180mL to 60mL to 5mL to obtain a mixed solution C, casting the mixed solution C into a mould, freeze-drying the mixed solution C at the temperature of minus 60 ℃ for 48 hours, and demoulding to obtain the heat-insulating foam material.
[ example 9 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally drying in vacuum at 70 ℃ for 12 hours to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.3g of a mixture of poplar powder, babbitt Sha Mufen, pine mushroom powder, lignocellulose waste and corn stalk powder into 100mL of deep eutectic solvent, continuously stirring for 75min at 130 ℃ to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 4 times to obtain a solid substance I;
Step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:130mL:1.5mL, continuously heating and stirring for 4h at 110 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 4 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 14mg/mL, and carrying out cell disruption treatment for 150min at 900W power to obtain esterified cellulose slurry;
step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 150mL:1g to 1g, 0.8g to 1.5g, ball milling for 16 hours to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with a volume ratio of 150mL to 55mL to 3mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at-60 ℃ for 40h, and demoulding to obtain the heat-insulating foam material.
[ example 10 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally drying in vacuum at 80 ℃ for 12 hours to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.2g of poplar powder, ba Sha Mufen and pine mushroom powder into 100mL of deep eutectic solvent, continuously stirring at 120 ℃ for 60min to fully dissolve lignin, adding distilled water for dilution, filtering and washing 3 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into a sodium chlorite aqueous solution with the concentration of 20g/L and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:150mL:1.5mL, continuously heating and stirring for 3h at 110 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 5 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 15mg/mL, and carrying out cell disruption treatment for 180min at the power of 1000W to obtain esterified cellulose slurry;
Step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 150mL:1 g/1.2 g/0.8 g/1.5 g, ball milling for 16h to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with a volume ratio of 150mL to 60mL to 4mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at the temperature of-65 ℃ for 48 hours, and demoulding to obtain the heat-insulating foam material.
[ example 11 ]
(1) Preparation of nano zinc oxide clusters
Zinc nitrate hexahydrate is dissolved in distilled water to prepare a solution E with the concentration of 0.02mol/L, and the solution E comprises the following components in percentage by volume: the amount of sodium hydroxide material was 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times by using distilled water, washing for 3 times by using ethanol, and finally vacuum drying for 12 hours at 60 ℃ to obtain nano zinc oxide clusters;
(2) Preparation of insulating foam
Step 1: adding 1.25g of pine mushroom powder, lignocellulose waste and corn stalk powder into 100mL of deep eutectic solvent, continuously stirring for 75min at 135 ℃ to fully dissolve lignin, adding distilled water for dilution, filtering and washing for 4 times to obtain a solid substance I;
step 2: dispersing all solid substance I obtained in the step 1 into 15g/L sodium chlorite aqueous solution and adding acetic acid, wherein the mass of the solid substance I is as follows: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g:125mL:1mL, continuously heating and stirring for 4h at 100 ℃, fully dissolving residual lignin, adding distilled water for dilution after the completion, filtering and washing for 4 times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 15mg/mL, and carrying out cell disruption treatment for 120min at the power of 1000W to obtain esterified cellulose slurry;
step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is 120mL:1 g/0.85 g/0.75 g, ball milling for 14h to obtain mixed slurry B, and transferring the mixed slurry B into a clean container;
Step 4: adding a polyvinyl alcohol aqueous solution and glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of 120mL to 60mL to 4mL to obtain a mixed solution C, casting the mixed solution C in a mould, freeze-drying the mixed solution C at the temperature of minus 55 ℃ for 42h, and demoulding to obtain the heat-insulating foam material.
Claims (10)
1. A method for preparing a cellulose-muscovite-zinc oxide-based heat insulation foam material, which is characterized by comprising the following steps:
step 1: adding powdery wood raw materials with cellulose content of more than 35% into a deep eutectic solvent, wherein the volume mass ratio of the deep eutectic solvent to the powdery wood raw materials is 100: (1-1.5) mL/g, heating and stirring, adding distilled water, filtering and washing for multiple times to obtain a solid substance I;
step 2: dispersing the solid substance I obtained in the step 1 into 15-25 g/L sodium chlorite aqueous solution, adding acetic acid with the concentration of 99.5%, and the mass of the solid substance I: volume of sodium chlorite aqueous solution: the volume of acetic acid was 1g: (100-150) mL: (1-2) mL, heating and stirring, adding distilled water, filtering and washing for multiple times to obtain a solid substance II, dispersing the solid substance II in distilled water to prepare an aqueous dispersion liquid A with the concentration of 12-15 mg/mL, and carrying out cell disruption treatment on the aqueous dispersion liquid A for 60-180 min to obtain esterified cellulose slurry;
Step 3: adding muscovite powder, nano zinc oxide, sodium sulfanilate and sodium carboxymethyl cellulose into the esterified cellulose slurry obtained in the step 2, wherein the volume of the esterified cellulose slurry is as follows: mass of the muscovite powder: the mass of the nano zinc oxide: mass of sodium sulfanilate: the mass of the sodium carboxymethyl cellulose is (120-180) mL:1 g/g (0.5-1.2) g/g (0.5-1) g/g (1.5-2) and ball milling for 12-16 h to obtain mixed slurry B;
step 4: adding 10wt% of polyvinyl alcohol aqueous solution and 95wt% of glutaraldehyde into the mixed slurry B obtained in the step 3, uniformly stirring the mixed slurry B, the polyvinyl alcohol aqueous solution and the glutaraldehyde with the volume ratio of (120-180) mL to (50-60) mL to (2-5) mL to obtain a mixed solution C, transferring the mixed solution C into a mold, freeze-drying the mixed solution C, and demolding to obtain the heat-insulating foam material based on cellulose-muscovite-zinc oxide.
2. The method for preparing a cellulose-muscovite-zinc oxide-based thermal insulation foam material according to claim 1, wherein the method for preparing the deep eutectic solvent in the step 1 comprises the following steps: according to 1:1, weighing choline chloride and oxalic acid dihydrate according to the mass ratio, uniformly mixing, heating at 90 ℃ until the mixture is melted into transparent liquid, and mixing the transparent liquid with the following components: distilled water is 1:100 volume ratio of distilled water is weighed and added into transparent liquid, and the mixture is uniformly mixed.
3. The method for preparing the heat-insulating foam material based on cellulose, muscovite and zinc oxide according to claim 1, wherein the powdery wood raw material with the cellulose content of more than 35% in the step 1 is one or a mixture of a plurality of poplar powder, ba Sha Mufen, pine mushroom powder, lignocellulose waste and corn stalk powder.
4. The method for preparing a heat insulation foam material based on cellulose-muscovite-zinc oxide according to claim 1, wherein the heating temperature in the step 1 is 120-150 ℃, the stirring time is 60-90 min, and the heat insulation foam material is filtered and washed 3-5 times.
5. The method for preparing a heat insulation foam material based on cellulose-muscovite-zinc oxide according to claim 1, wherein the heating temperature in the step 2 is 90-110 ℃, the stirring time is 3-5 h, and the heat insulation foam material is filtered and washed 3-5 times.
6. The method for preparing a cellulose-muscovite-zinc oxide-based thermal insulation foam according to claim 1, wherein the power of the cell disruption treatment in the step 2 is 800 to 1000W.
7. The method for preparing the thermal insulation foam material based on cellulose-muscovite-zinc oxide according to claim 1, wherein the method for preparing the nano zinc oxide in the step 3 comprises the following steps: zinc nitrate hexahydrate is dissolved in distilled water to obtain a solution E with the concentration of 0.02mol/L, and the solution E is prepared according to the volume of the distilled water: the molar mass of the sodium hydroxide is 1L: adding sodium hydroxide solid into the solution E according to the proportion of 0.002mol, uniformly mixing, stirring for 5 hours at 95 ℃, centrifuging for 5 minutes at the rotating speed of 8000r/min, washing for 3 times with water, washing for 3 times with ethanol, and vacuum drying for 12 hours at 60-80 ℃.
8. The method for preparing the heat insulation foam material based on cellulose-muscovite-zinc oxide according to claim 1, wherein the polyvinyl alcohol aqueous solution in the step 4 is 10wt% of the polyvinyl alcohol aqueous solution.
9. The method for preparing a heat insulating foam material based on cellulose-muscovite-zinc oxide according to claim 1, wherein the freeze-drying temperature in the step 4 is-55 to-65 ℃ for 36 to 48 hours.
10. A thermal insulation foam based on cellulose-muscovite-zinc oxide, characterized in that it is produced by a method for producing a thermal insulation foam based on cellulose-muscovite-zinc oxide as claimed in any one of claims 1 to 9.
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