CN114874504A - Light and heat-insulating polysaccharide-based composite aerogel taking wood waste as raw material and preparation method thereof - Google Patents
Light and heat-insulating polysaccharide-based composite aerogel taking wood waste as raw material and preparation method thereof Download PDFInfo
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- CN114874504A CN114874504A CN202210409139.6A CN202210409139A CN114874504A CN 114874504 A CN114874504 A CN 114874504A CN 202210409139 A CN202210409139 A CN 202210409139A CN 114874504 A CN114874504 A CN 114874504A
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 47
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- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 claims description 4
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- 229960000892 attapulgite Drugs 0.000 claims description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 3
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- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 3
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 241000771208 Buchanania arborescens Species 0.000 description 1
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- 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
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- 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
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- 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
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- 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
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- 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
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/405—Impregnation with polymerisable compounds
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- 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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- 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
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2497/00—Characterised by the use of lignin-containing materials
- C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a light and heat-insulating polysaccharide-based composite aerogel taking wood waste as a raw material and a preparation method thereof. The method of the invention comprises the steps of respectively passing the wood waste through alkali liquor and H 2 O 2 Carrying out heat treatment on the solution to remove lignin and obtain wood cellulose; mixing the wood cellulose, the curdlan and the inorganic fillerHeating in water bath to obtain mixed gel; and then freezing the mixed gel, drying to remove water, and adopting an alkylation method to make the aerogel have hydrophobicity. The maximum compression modulus of the composite aerogel is not more than 3.84MPa, and the thermal conductivity can reach 32 multiplied by 10 ‑ 3 W/(m.K) is even lower. The hydrophobic contact angle of the aerogel is not less than 120 degrees. The high-performance and ultra-light nontoxic aerogel prepared by using the renewable wood waste can be applied to scenes such as food heat preservation, heat management of electronic products and the like. The composite aerogel prepared by the preparation method has important significance in the aspects of environmental protection and sustainable energy.
Description
Technical Field
The invention relates to materials used in the fields of heat insulation, heat exchange and heat storage, in particular to a light and low-heat-conductivity polysaccharide-based composite aerogel taking wood waste as a raw material and a preparation method thereof.
Background
With the continuous enhancement of social sustainable development and ecological environmental protection consciousness, the biomass material with light weight, high heat insulation and strong flame retardant property has important significance for modern society. The aerogel has the characteristics of light weight, high porosity and high specific surface area, and can be widely applied to scenes such as pollutant treatment, heat insulation and sound insulation, and the fields such as buildings, clothes, textiles and the like. Over the last decade, various aerogel materials have been developed in succession. Among them, silica aerogel, which is a typical inorganic aerogel, is a good thermal insulation material having ultra-low thermal conductivity due to its low density, high porosity and high specific surface area. However, silica aerogels have poor strength, limiting their further applications. Also, the silica aerogel is prepared by a process, usually supercritical CO 2 Drying, high energy consumption, low cost benefit and difficult realization of large-scale production.
In recent years, renewable biomass aerogels such as nano-cellulose aerogel, silk fibroin aerogel, starch aerogel, chitosan aerogel and konjac glucomannan aerogel have attracted more and more attention due to the characteristics of abundant raw material sources, low cost, environmental protection, sustainable application and the like. Curdlan, one of such biomass aerogels, is a polysaccharide product fermented by microorganisms, and is also a very abundant renewable biomass polymer on earth. Due to its high bioactivity and biodegradability, it can be used for biological medicine and food packaging. In addition, due to the characteristics of good mechanical strength, light weight and the like, the curdlan plays a key role in designing functional composite materials, particularly composite materials applied to heat management.
As one of the plants growing faster in the world, wood is used to manufacture various furniture products. However, in the wood processing process, over million tons of wood waste are generated every year, and the biomass waste is a special resource and can be used for manufacturing other high value-added products. However, the existing biomass waste has low efficiency of rational utilization and unsatisfactory added value of products, and further development of more application fields is needed.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art and provide the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material and the preparation method thereof.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a light and heat-insulating polysaccharide-based composite aerogel taking wood waste as a raw material is prepared by taking the wood waste as a raw material, and comprises the following steps:
1) adding NaOH and NaHSO into wood waste 3 In the mixed solution of (1);
2) heating the mixed solution obtained in the step 1) to remove lignin in wood;
3) washing the product obtained after the lignin is removed in the step 2) with deionized water, and adding H with the mass percent concentration of not less than 30 wt% 2 O 2 In the solution, heating to obtain a solid product;
4) drying the solid product obtained in the step 3) in a forced air oven to obtain wood cellulose;
5) mixing the wood cellulose, polysaccharide carbohydrate and inorganic filler obtained in the step 4) with deionized water, and uniformly mixing on a stirring table to obtain a mixture;
6) heating the mixture obtained in the step 5) in a water bath to obtain mixture gel;
then placing the mixture gel in a freeze dryer for freezing treatment;
after freezing treatment, primary freeze drying is carried out to remove water;
then transferring the mixture gel subjected to freeze drying into a blast oven for secondary drying to obtain a primary product of the wood cellulose/polysaccharide-based composite aerogel;
7) putting the wood cellulose/polysaccharide-based composite aerogel obtained in the step 6) into a container filled with polysiloxane, integrally moving the container filled with reactants into a vacuum drier, and vacuumizing the vacuum drier;
and then putting the vacuum dryer of the container filled with the reactants into a blast oven, and continuing to react to obtain the wood cellulose/polysaccharide-based composite aerogel with the hydrophobic property.
Preferably, in the step 1), the wood waste is a mixture of wood chips of any one or more of balsa wood, pine wood and fir wood;
preferably, in the step 1), the concentration of the NaOH solution in the mixed solution is 0.5-6.5 mol/L, and the NaHSO in the mixed solution 3 The concentration of the solution is 0.1-2.5 mol/L.
Preferably, in the step 2), the heating temperature is 30-300 ℃, and the heating time is 2-24 hours. Further preferably, the heating temperature of the heating treatment is 80-100 ℃, and the heating time is 8-24 h.
Preferably, in the step 3), the deionized water washing method comprises soaking the product treated by the alkali liquor in deionized water for 15-60 min, and repeatedly soaking for 3-5 times;
preferably, in the step 3), the heating temperature is 50-200 ℃, and the heating time is 2-24 hours. Further preferably, the heating temperature of the heating treatment is 70-100 ℃, and the heating time is 4-12 h.
Preferably, in the step 4), the temperature of the blast oven is controlled to be 50-150 ℃ and the drying time is 2-48 h. Further preferably, the temperature of the blast air oven is 80-150 ℃, and the drying time is 12-48 h.
Preferably, in the step 5), the polysaccharide carbohydrate is at least one material selected from gelatin, curdlan, xanthan gum and konjac glucomannan;
preferably, in the step 5), the inorganic filler is at least one material selected from nano hydroxyapatite, montmorillonite and attapulgite;
preferably, in the step 5), the mass ratio of the wood cellulose to the polysaccharide carbohydrate is 1: 1-5;
preferably, in the step 5), the mass ratio of the wood cellulose to the inorganic filler is 3: 0 to 20;
preferably, in the step 5), the stirring rotation speed is controlled to be 500-.
Preferably, in the step 6), the water bath heating is carried out at the temperature of 50-200 ℃ for 15 min-2 h; further preferably, the temperature for heating in the water bath is 85-200 ℃;
preferably, in the step 6), the freezing temperature of the mixture gel is not higher than-18 ℃, and the freezing time is 4-48 h; further preferably, the mixture gel is frozen in a cold trap of a freeze dryer at the temperature of between 55 ℃ below zero and 18 ℃ below zero for 4 to 24 hours;
preferably, in the step 6), the freeze-drying time is controlled to be 6-64 h when the preliminary freeze-drying is carried out; further preferably, the freeze drying time is controlled to be 24-48 h;
preferably, in the step 6), when the second drying is performed, the drying temperature of the forced air oven is controlled to be 50-150 ℃, and the heating and drying time is 2-48 h. Further preferably, the heating and drying time is 24-48 h.
Preferably, in the step 7), the density of the prepared primary product of the wood cellulose/polysaccharide-based composite aerogel is not more than 48.7 × 10 -3 g/cm 3 。
Preferably, in the step 7), the polysiloxane is at least one of methyltrimethoxysilane, tetraethoxysilane and hexadecyltrimethoxysilane;
preferably, in the step 7), the temperature of the air-blast oven is 50-80 ℃, and the reaction time is 12-48 h.
Preferably, in the step 7), the contact angle of the prepared lignocellulose/polysaccharide-based composite aerogel is not less than 116 °. It is further preferable that the contact angle is not less than 121 °.
The invention discloses a light and heat-insulating polysaccharide-based composite aerogel, which is prepared by using the preparation method of the light and heat-insulating polysaccharide-based composite aerogel.
Preferably, the lightweight and heat-insulating polysaccharide-based composite aerogel takes polysaccharide carbohydrate as a structural framework and wood cellulose as a reinforcing phase, has a cellular porous microstructure, has the thermal conductivity of not higher than 0.032W/(m.K), and has the maximum compression modulus of not higher than 3.84 MPa. Further preferably, the polysaccharide-based composite aerogel has a thermal conductivity of not higher than 0.0301W/(m.K) and a maximum compressive modulus of not higher than 0.5593 MPa.
The method for extracting the cellulose from the wood waste as the reinforcing phase in the composite material is a current advanced resource recycling method, and the strength and the toughness of the composite material can be effectively improved by introducing the wood cellulose into a soft aerogel matrix. The composite aerogel prepared by the method is prepared by taking curdlan as a structural frame, taking wood cellulose as a reinforcing phase to be dispersed in the structural frame, adding an inorganic filler into the composite material to improve the thermal and mechanical properties of the composite aerogel, and reducing the thermal conductivity of the composite aerogel to 30.1 multiplied by 10 -3 W/(m.K), even lower, the maximum compression modulus is not more than 1.65MPa, and the preparation method has great application potential in the aspects of solving the problems of food heat insulation and heat preservation and modern electronic product heat management.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method extracts the wood cellulose by treating the wood powder treated as waste, takes polysaccharide carbohydrate as an adhesive matrix, and adds inorganic filler to improve the mechanical property and the thermal stability of the wood cellulose; (ii) a
2. Compared with other reinforced phase materials, the wood cellulose has a flexible and porous supporting structure, and the prepared composite aerogel has lower thermal conductivity, excellent mechanical properties such as strength and toughness and good hydrophobic property, so that the composite aerogel has wide application potential in the field of thermal management;
3. the composite material prepared by the method also has the advantages of low cost, light weight, environmental friendliness, no toxicity and simple preparation process.
Drawings
Fig. 1 is a structural morphology diagram of a wood fiber/curdlan aerogel prepared in example 1 of the present invention.
Fig. 2 is a microstructure topography of the wood fiber/curdlan @ hydroxyapatite composite aerogel prepared in example 2 of the present invention.
Fig. 3 is a contact angle diagram of the wood fiber/curdlan @ hydroxyapatite composite aerogel prepared in example 2 of the present invention.
FIG. 4 is a numerical graph showing the change in surface color after heat treatment of aerogels prepared in examples 1 and 2 of the present invention.
Fig. 5 is a thermogravimetric plot of aerogels prepared in examples 1 and 2 of the present invention.
Fig. 6 is a graph of mechanical properties of aerogels prepared in examples 1 and 2 of the present invention.
Fig. 7 is a flowchart of a method for preparing a polysaccharide-based composite aerogel according to preferred embodiment 2 of the present invention.
Detailed Description
The invention is further illustrated below with reference to the accompanying drawings and the following embodiments. The invention relates to a light and heat-insulating polysaccharide-based composite aerogel taking wood waste as a raw material and a preparation method thereof, and the specific scheme is as follows: firstly, sequentially treating light wood powder with alkali liquor and aqueous hydrogen peroxide for 4-24 hours to obtain wood cellulose, then uniformly mixing the wood cellulose, polysaccharide carbohydrate and inorganic filler by stirring, and heating to obtain mixed gel. And freezing the obtained gel, then putting the gel into a freeze dryer for drying for 24-48h to obtain aerogel, and then putting the aerogel into a blast oven for heat treatment for 8-24 h. And finally, putting the aerogel and a glass bottle filled with polysiloxane into a vacuum drier together, permeating the polysiloxane into the aerogel by utilizing gas phase transfer, and then putting the aerogel into a blast air oven for continuous reaction to obtain the composite aerogel with hydrophobic performance.
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
example one
In this embodiment, a method for preparing a light and heat-insulating polysaccharide-based composite aerogel by using wood waste as a raw material includes the following steps:
1) putting the balsawood scraps as raw materials into a beaker, and then adding NaOH solution and NaHSO into the beaker 3 A solution is prepared, the concentration of NaOH solution in the mixed solution is 2.5mol/L, and NaHSO in the mixed solution 3 The concentration of the solution is 0.5mol/L, and the solution is uniformly mixed;
2) placing the beaker in the step 1) in an oil bath, and heating at 90 ℃ for 12h to remove lignin in the balsawood powder;
3) filtering the product solution obtained after the lignin is removed in the step 2), and soaking and washing the obtained product by using deionized water; after repeating the washing three times, the obtained wood flour was charged into a beaker, and then H was added to the beaker in a concentration of 30 wt.% in terms of mass percentage 2 O 2 Putting the beaker into a 70 ℃ water bath kettle, and heating for 6 hours; filtering the solution, washing the obtained product with deionized water until the pH value of the washing liquid is 7 to obtain a solid product;
4) putting the solid product obtained in the step 3) into a forced air oven at 80 ℃ for drying for 24 hours to obtain wood cellulose;
5) mixing the wood cellulose obtained in the step 4) with a curdlan aqueous solution with the mass percentage concentration of 3 wt.%, mixing the wood cellulose and the curdlan according to the mass ratio of 3:5, and uniformly mixing on a stirring table to obtain a mixture;
6) uniformly stirring the mixture solution obtained in the step 5), and putting the mixture solution into a water bath kettle at 85 ℃ for water bath heating for 15min to obtain mixed gel;
then placing the mixture gel in a cold trap of a freeze dryer, and freezing for 24h at-55 ℃;
after freezing treatment, primary freeze drying is carried out for 48 hours to remove water;
then transferring the mixture gel subjected to freeze drying into a 50 ℃ blast oven for secondary drying for 24 hours to obtain a primary product of the wood cellulose/polysaccharide-based composite aerogel, and marking as WFs/Cm;
7) putting the wood cellulose/polysaccharide-based composite aerogel obtained in the step 6) into a container filled with methyltrimethoxysilane, integrally moving the container filled with the reactant into a vacuum drier, and vacuumizing the vacuum drier;
and then putting the vacuum dryer of the container filled with the reactants into a blast oven at 80 ℃, and continuing to react for 24 hours to obtain the wood cellulose/polysaccharide-based composite aerogel with the hydrophobic property.
Experimental test analysis:
in this example, the density of the composite aerogel WFs/Cm prepared in step 6) is 4.97X 10 -3 g/cm 3 In this embodiment, the composite aerogel WFs/Cm prepared in step 6) has a cellular porous microstructure, and the internal microstructure thereof is shown in fig. 1. The contact angle is 0 DEG, and the hydrophilic coating has hydrophilicity. In this embodiment, the color change of the aerogel after the thermal treatment at different temperatures of the composite aerogel WFs/Cm prepared in step 6) is shown in FIG. 4. In the embodiment, the thermal conductivity of the composite aerogel WFs/Cm prepared in the step 6) is 30.1 multiplied by 10 -3 W/(m.K) is lower than the thermal conductivity of 0.032-0.048W/(m.K) of the thermal insulation aerogel obtained by the patent publication No. CN 110789191A. In the embodiment, the mass residue rate of the composite aerogel WFs/Cm prepared in the step 6) after the heat treatment at 700 ℃ is 26.5 percent, which is shown in a thermogravimetric experimental curve of FIG. 5. The compression modulus of the composite aerogel WFs/Cm prepared in the step 6) of the embodiment is 0.1366MPa, see FIG. 6.
In this example, the contact angle of the composite aerogel with hydrophobic property finally prepared in step 7) is 116 °.
Example two
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, as shown in fig. 7, a method for preparing a lightweight, heat-insulating polysaccharide-based composite aerogel using wood waste as a raw material includes the following steps:
1) the step is the same as the first embodiment;
2) the step is the same as the first embodiment;
3) the step is the same as the first embodiment;
4) the step is the same as the first embodiment;
5) mixing the wood cellulose obtained in the step 4) with a curdlan aqueous solution with the mass percentage concentration of 3 wt.%, mixing the wood cellulose with the curdlan according to the mass ratio of 3:5, adding nano-hydroxyapatite to enable the mass percentage of the nano-hydroxyapatite in the mixed solution to be 20 wt.%, magnetically stirring the mixture on a stirring table for 4 hours, and uniformly mixing the mixture to obtain a mixture;
6) uniformly stirring the mixture solution obtained in the step 5), and putting the mixture solution into a water bath kettle at 85 ℃ for water bath heating for 15min to obtain mixed gel;
then placing the mixture gel in a cold trap of a freeze dryer, and freezing for 24h at-55 ℃;
after freezing treatment, primary freeze drying is carried out for 48 hours to remove water;
then transferring the mixture gel subjected to freeze drying into a 50 ℃ blast oven for secondary drying for 24 hours to obtain a primary product of the wood cellulose/polysaccharide-based composite aerogel, and marking as HAP @ WFs/Cm;
7) putting the wood cellulose/polysaccharide-based composite aerogel HAP @ WFs/Cm obtained in the step 6) into a container filled with methyltrimethoxysilane, moving the container filled with the reactant into a vacuum drier as a whole, and vacuumizing the vacuum drier;
and then putting the vacuum dryer of the container filled with the reactants into a blast oven at 80 ℃, and continuing to react for 24 hours to obtain the wood cellulose/polysaccharide-based composite aerogel with the hydrophobic property.
Experimental test analysis:
in the embodiment, the density of the HAP @ WFs/Cm of the composite aerogel prepared in the step 6) is 22.9 multiplied by 10 -3 g/cm 3 In this example, the composite aerogel HAP @ WFs/Cm prepared in step 6) has a honeycomb-like porous microstructure, and the internal microstructure thereof is shown in fig. 2. In the embodiment, the contact angle of the HAP @ WFs/Cm of the composite aerogel prepared in the step 6) is 0 °, and the composite aerogel has hydrophilicity, as shown in fig. 3a and 3 c. In this example, the surface color of the aerogel after the composite aerogel HAP @ WFs/Cm prepared in step 6) is heat-treated at different temperatures is shown in FIG. 4. In the embodiment, the thermal conductivity of the composite aerogel HAP @ WFs/Cm prepared in the step 6) is 30.1 multiplied by 10 -3 W/(m.K) is lower than the thermal conductivity of 0.032-0.048W/(m.K) of the thermal insulation aerogel obtained by the patent publication No. CN 110789191A. In this example, the mass residue of the composite aerogel HAP @ WFs/Cm prepared in step 6) after heat treatment at 700 ℃ is 49.7%, as shown in FIG. 5 of a thermogravimetric experimental curve. In the embodiment, the HAP @ WFs/Cm of the composite aerogel prepared in the step 6) is 0.5596MPa, as shown in FIG. 6.
In this example, the contact angle of the composite aerogel with hydrophobic property finally prepared in step 7) is 128 °, and the test results are shown in fig. 3b and fig. 3 d.
EXAMPLE III
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a method for preparing a lightweight, heat-insulating polysaccharide-based composite aerogel using wood waste as a raw material includes the following steps:
1) putting the balsawood scraps as raw materials into a beaker, and then adding NaOH solution and NaHSO into the beaker 3 A solution is prepared, the concentration of NaOH solution in the mixed solution is 6.5mol/L, and NaHSO in the mixed solution 3 The concentration of the solution is 2.5mol/L, and the solution is uniformly mixed;
2) placing the beaker in the step 1) in an oil bath pot, and heating at 100 ℃ for 24 hours to remove lignin in the balsawood powder;
3) filtering the product solution obtained after the lignin is removed in the step 2), and soaking and washing the obtained product by using deionized water; after repeating the washing three times, the obtained wood flour was charged into a beaker, and then H was added to the beaker in a concentration of 30 wt.% in terms of mass percentage 2 O 2 Water solution, placing the beaker in a water bath kettle at 100 ℃ and heating for 12 hours; filtering the solution, washing the obtained product with deionized water until the pH value of the washing liquid is 7 to obtain a solid product;
4) putting the solid product obtained in the step 3) into a forced air oven at 150 ℃ for drying for 12 hours to obtain wood cellulose;
5) mixing the wood cellulose obtained in the step 4) with a curdlan aqueous solution with the mass percentage concentration of 3 wt.%, mixing the wood cellulose with the curdlan according to the mass ratio of 1:1, adding nano-hydroxyapatite to enable the mass percentage of the nano-hydroxyapatite in the mixed solution to be 60 wt.%, magnetically stirring the mixture on a stirring table for 4 hours, and uniformly mixing the mixture to obtain a mixture;
6) uniformly stirring the mixture solution obtained in the step 5), and heating the mixture solution in an oil bath kettle at the temperature of 200 ℃ for 2 hours to obtain mixed gel;
then placing the mixture gel in a cold trap of a freeze dryer, and freezing for 48h at-18 ℃;
after freezing treatment, primary freeze drying is carried out for 24 hours to remove water;
then transferring the mixture gel subjected to freeze drying into a 50 ℃ blast oven for secondary drying for 48 hours to obtain a primary product of the wood cellulose/polysaccharide-based composite aerogel;
7) putting the wood cellulose/polysaccharide-based composite aerogel obtained in the step 6) into a container filled with methyltrimethoxysilane, integrally moving the container filled with the reactant into a vacuum drier, and vacuumizing the vacuum drier;
and then putting the vacuum dryer of the container filled with the reactants into a 50 ℃ blast oven, and continuing to react for 48 hours to obtain the wood cellulose/polysaccharide-based composite aerogel with the hydrophobic property.
Experimental test analysis:
this example shows that the density of the composite aerogel prepared in step 6) is 48.7 × 10 -3 g/cm 3 In this embodiment, the composite aerogel prepared in step 6) has a cellular and porous microstructure. In this embodiment, the contact angle of the composite aerogel prepared in step 6) is 0 °, and the composite aerogel has hydrophilicity. The thermal conductivity of the composite aerogel prepared in the step 6) of the present example was 32 × 10 -3 W/(m.K), not higher than the thermal conductivity of the thermal insulation aerogel obtained by the patent publication No. CN 110789191A by 0.032-0.048W/(m.K). In this example, the mass residue rate of the composite aerogel prepared in step 6) after the heat treatment at 700 ℃ is 52.5%. The compression modulus of the composite aerogel prepared in the step 6) of the embodiment is 3.84 MPa.
In this example, the contact angle of the composite aerogel with hydrophobic property finally prepared in step 7) is 121 °.
Example four
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a method for preparing a light and heat-insulating polysaccharide-based composite aerogel using wood waste as raw material,
in the step 1), the wood waste is a mixture of wood chips of any one or more of balsa wood, pine wood and fir wood;
in the step 5), the polysaccharide carbohydrate adopts at least one material of gelatin, curdlan, xanthan gum and konjac glucomannan;
in the step 5), the inorganic filler is at least one material selected from nano hydroxyapatite, montmorillonite and attapulgite;
in the step 7), the polysiloxane is at least one of methyltrimethoxysilane, tetraethoxysilane and hexadecyltrimethoxysilane.
The preparation method of the gel polysaccharide-based composite aerogel has the advantages of being low in cost, light in weight, non-toxic, excellent in heat insulation performance, good in thermal stability, simple in preparation process and the like.
In summary, the gel polysaccharide based composite aerogel and the preparation method thereof of the present invention use wood waste as a raw material, and the composite aerogel has the characteristics of ultra-light weight and ultra-low thermal conductivity. In the above embodiment of the present invention, the wood waste is respectively treated with alkali solution and H 2 O 2 Carrying out heat treatment on the solution to remove lignin and hemicellulose in the wood to obtain the required wood cellulose; uniformly mixing the wood cellulose, the curdlan and the inorganic filler, and then heating in a water bath to obtain mixed gel; the mixed gel is then frozen and then placed in a freeze dryer to remove water and the aerogel is rendered hydrophobic by alkylation. The maximum compression modulus of the composite aerogel obtained by the invention is not more than 3.84MPa, and the thermal conductivity can be as low as 32 multiplied by 10 -3 W/(m.K), even lower. The hydrophobic contact angle of the aerogel is not less than 120 degrees. The high-performance and ultra-light nontoxic aerogel prepared by using the renewable wood waste can be applied to scenes such as food heat preservation, heat management of electronic products and the like. The composite aerogel prepared by the preparation method of the embodiment of the invention has important significance in the aspects of environmental protection and sustainable energy.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.
Claims (10)
1. A preparation method of a light and heat-insulating polysaccharide-based composite aerogel taking wood waste as a raw material is characterized by comprising the following steps:
1) waste wood materialAdding NaOH and NaHSO 3 In the mixed solution of (1);
2) heating the mixed solution obtained in the step 1) to remove lignin in wood;
3) washing the product obtained after the lignin is removed in the step 2) with deionized water, and adding H with the mass percent concentration of not less than 30 wt% 2 O 2 In the solution, heating to obtain a solid product;
4) drying the solid product obtained in the step 3) in a forced air oven to obtain wood cellulose;
5) mixing the wood cellulose, polysaccharide carbohydrate and inorganic filler obtained in the step 4) with deionized water, and uniformly mixing on a stirring table to obtain a mixture;
6) heating the mixture obtained in the step 5) in a water bath to obtain mixture gel;
then placing the mixture gel in a freeze dryer for freezing treatment;
after freezing treatment, primary freeze drying is carried out to remove water;
then transferring the mixture gel subjected to freeze drying into a blast oven for secondary drying to obtain a primary product of the wood cellulose/polysaccharide-based composite aerogel;
7) putting the wood cellulose/polysaccharide-based composite aerogel obtained in the step 6) into a container filled with polysiloxane, integrally moving the container filled with reactants into a vacuum drier, and vacuumizing the vacuum drier;
and then putting the vacuum dryer of the container filled with the reactants into a blast oven, and continuing to react to obtain the wood cellulose/polysaccharide-based composite aerogel with the hydrophobic property.
2. The method for preparing the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material according to claim 1, is characterized in that: in the step 1), the wood waste is a mixture of wood chips of any one or more of balsa wood, pine wood and fir wood;
or in the step 1), the concentration of NaOH solution in the mixed solution is 0.5-6.5 mol/L, and NaHSO in the mixed solution 3 The concentration of the solution is 0.1-2.5 mol/L.
3. The method for preparing the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material according to claim 1, is characterized in that: in the step 2), the heating temperature is 30-300 ℃, and the heating time is 2-24 hours.
4. The method for preparing the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material according to claim 1, is characterized in that: in the step 3), the deionized water washing method comprises soaking the product treated by the alkali liquor in deionized water for 15-60 min, and repeatedly soaking for 3-5 times;
or, in the step 3), the heating temperature is 50-200 ℃, and the heating time is 2-24 hours.
5. The method for preparing the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material according to claim 1, is characterized in that: in the step 4), when drying is carried out, the temperature of the oven is 50-150 ℃, and the drying time is 2-48 h.
6. The method for preparing the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material according to claim 1, is characterized in that: in the step 5), the polysaccharide carbohydrate adopts at least one material of gelatin, curdlan, xanthan gum and konjac glucomannan;
or, in the step 5), the inorganic filler is at least one material selected from nano hydroxyapatite, montmorillonite and attapulgite;
or, in the step 5), the mass ratio of the wood cellulose to the polysaccharide carbohydrate is 1: 1-5;
or, in the step 5), the mass ratio of the wood cellulose to the inorganic filler is 3: 0 to 20.
7. The method for preparing the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material according to claim 1, is characterized in that: in the step 6), the water bath heating is carried out at the temperature of 50-200 ℃ for 15 min-2 h;
or, in the step 6), the freezing temperature is not higher than-18 ℃, and the freezing time is 4-48 h;
or, in the step 6), when the preliminary freeze drying is carried out, the freeze drying time is controlled to be 6-64 h;
or, in the step 6), when the second drying is performed, the drying temperature of the blast oven is controlled to be 50-150 ℃, and the heating and drying time is 2-48 h.
8. The method for preparing the light and heat-insulating polysaccharide-based composite aerogel taking wood waste as the raw material according to claim 1, is characterized in that: in the step 7), the polysiloxane adopts at least one of methyltrimethoxysilane, tetraethoxysilane and hexadecyltrimethoxysilane;
or in the step 7), the temperature of the air-blast oven is 50-80 ℃, and the reaction time is 12-48 h.
9. The light and heat-insulating polysaccharide-based composite aerogel is characterized in that: the preparation method of the light and heat-insulating polysaccharide-based composite aerogel taking the wood waste as the raw material according to claim 1 is utilized to prepare the aerogel.
10. The lightweight, thermally insulating polysaccharide-based composite aerogel of claim 9, wherein: polysaccharide carbohydrate is used as a structural framework, wood cellulose is used as a reinforcing phase, and the composite material has a honeycomb porous microstructure, the thermal conductivity of the composite material is not higher than 0.032W/(m.K), and the maximum compression modulus of the composite material is not higher than 3.84 MPa.
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