CN115709055A - Wood cellulose-based carbon dioxide adsorption and desorption foam and preparation method thereof - Google Patents
Wood cellulose-based carbon dioxide adsorption and desorption foam and preparation method thereof Download PDFInfo
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 87
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000001913 cellulose Substances 0.000 title claims abstract description 55
- 229920002678 cellulose Polymers 0.000 title claims abstract description 55
- 239000006260 foam Substances 0.000 title claims abstract description 41
- 239000002023 wood Substances 0.000 title claims abstract description 39
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 37
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 37
- 238000003795 desorption Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 19
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 18
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000412 dendrimer Substances 0.000 claims abstract description 3
- 229920000736 dendritic polymer Polymers 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000004061 bleaching Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 240000007182 Ochroma pyramidale Species 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims 4
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 19
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 4
- 239000011147 inorganic material Substances 0.000 abstract description 4
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000003463 adsorbent Substances 0.000 description 9
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- 239000000126 substance Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000010382 chemical cross-linking Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013317 conjugated microporous polymer Substances 0.000 description 2
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- 238000012360 testing method Methods 0.000 description 2
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- 241000609240 Ambelania acida Species 0.000 description 1
- 240000006248 Broussonetia kazinoki Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
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- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
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- 229910021536 Zeolite Inorganic materials 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- -1 amine compound Chemical class 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
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- 239000003208 petroleum Substances 0.000 description 1
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- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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Images
Classifications
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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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention discloses wood cellulose-based carbon dioxide adsorption and desorption foam and a preparation method thereof, and belongs to the field of carbon dioxide adsorption and desorption materials. The invention aims to solve the technical problems of long time consumption, complex synthesis process and low repeated utilization rate of the conventional method for preparing the amino-based adsorption material by mainly using an inorganic material as a carrier. According to the invention, wood cellulose is used as a raw material, 3-glycidyl ether oxypropyl methyl diethoxy silane is used as a cross-linking agent, and dendrimer polyethylene imine is grafted to synthesize the carbon dioxide adsorption foam material, so that high carbon dioxide adsorption capacity at ambient temperature can be realized, and release can be controlled at ambient temperature. The adsorption and desorption foam provided by the invention is green and environment-friendly, and has high economic value and high material recycling rate.
Description
Technical Field
The invention belongs to the field of carbon dioxide adsorption and desorption materials, and particularly relates to wood cellulose-based carbon dioxide adsorption and desorption foam and a preparation method thereof.
Background
In the development process of times, fossil fuels play an important role in production and life of people. While burning fossil fuels brings economic benefits and life convenience to people, a large amount of carbon dioxide gas is brought in the burning process, and in the past decades, people have been dedicated to alleviating the problem by capturing carbon dioxide from main pollution sources such as coal, petroleum and gas power plants, and the current technical methods for capturing carbon dioxide mainly comprise physical adsorption and chemical adsorption, and a membrane separation process. The traditional carbon dioxide physical adsorption material comprises inorganic materials and organic materials, wherein the inorganic materials comprise zeolite molecular sieves, activated carbon, metal oxides and the like; organic materials such as Conjugated Microporous Polymers (CMP), covalent organic framework Compounds (COF), metal framework chemical compounds (MOF) and other porous materials have various technical problems in the current industrial production, such as complicated preparation process conditions which are difficult to regulate, difficult degradation in natural environment, high economic cost and the like. In the existing known chemical adsorption materials, an amine compound is used as one of ideal chemical adsorbents, a chemical reaction between amine and carbon dioxide is used as a leading path of chemical adsorption, and the conventional method for preparing the amine adsorption material mainly uses inorganic materials (such as nano-alumina, nano-silica and the like) as carriers, so that the preparation process is long in time consumption, the synthesis process is complex and the recycling rate is low.
Disclosure of Invention
In order to develop a natural renewable resource green carrier, namely delignified wood cellulose, the wood cellulose is used as an environmentally-friendly, renewable and degradable green material and has good machinery, and cross-linking functional groups are introduced through surface modification to prepare the carbon dioxide high-adsorption and desorption wood cellulose adsorption foam.
The method utilizes the characteristics of large specific surface area, abundant hydroxyl on the surface, high mechanical strength and the like of the delignified wood cellulose, carries out hydroxyl modification on the surface of the delignified wood cellulose by hydrolyzing the silicon-based glycidyl ether, and further carries out crosslinking with solid amine to prepare the wood cellulose-based carbon dioxide adsorption and desorption foam with high adsorption and desorption performances. The preparation process mainly solves the technical problems of complex synthesis process, poor adsorption and desorption performance at ambient temperature, low repeated utilization rate and the like of the existing carbon dioxide adsorbing material, and provides a new approach for the green and sustainable 'double-carbon' goal.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention aims to provide wood cellulose-based carbon dioxide adsorption and desorption foam, which is prepared by grafting dendrimer polyethyleneimine onto cellulose serving as a raw material through a cross-linking agent; the cross-linking agent is 3-glycidyl ether oxypropyl methyldiethoxysilane (GPTMS); the method specifically comprises the following steps:
step one, dispersing cellulose in deionized water to obtain a cellulose solution;
step two, adding a cross-linking agent into the cellulose solution, and magnetically stirring for at least 2 hours at room temperature;
step three, dropwise adding the polyethyleneimine water solution while stirring, and continuously stirring for at least 12 hours after the dropwise adding is finished;
and step four, rapidly freezing the mixture for 2 hours by using liquid nitrogen, and freeze-drying the mixture for at least 48 hours at the temperature of between 80 ℃ below zero and 50 ℃ below zero to obtain the carbon dioxide adsorption and desorption foam.
Further defined, the production raw material of the cellulose is derived from wood, cotton linter, wheat straw, rice straw, reed, hemp, mulberry bark, paper mulberry bark, bagasse and the like, and is preferably delignified lignocellulose; more preferably, it is prepared from balsa, which is obtained by dewaxing, delignification, bleaching and rinsing balsa.
Further limiting, delignification is carried out in a dark place, and bleaching is carried out by using 30wt% of hydrogen peroxide.
Further defined, the mass concentration of the cellulose solution is 0.5wt% to 1.0wt%.
Further defined, the mass ratio of the cross-linking agent to the cellulose is 1.
Further limiting, the dropping speed in the step three is 1 d/s-5 d/s.
Further, the mass ratio of polyethyleneimine to cellulose is 1 (1-2).
Further defined, the concentration of the polyethyleneimine solution is 1wt% to 5wt%.
The method adopts the delignified wood cellulose, is uniformly dispersed and stable in water, has a foam structure after freeze-drying, has large pore, large specific surface area, high mechanical strength, excellent regenerability, good biocompatibility, biodegradability and light texture. The surface of the wood cellulose is rich in a large number of hydroxyl groups, dendritic molecular polyethyleneimine is grafted on the surface through chemical reaction with silicon base, so that a carbon dioxide adsorption foam material is synthesized, the high adsorption capacity of carbon dioxide at ambient temperature can be realized, and the release can be controlled at the ambient temperature.
The method utilizes a large number of hydroxyl groups on the surface of the delignified wood cellulose as reaction sites, introduces the silicon-based glycidyl ether, generates a chemical condensation reaction with the delignified wood cellulose, and further generates a chemical crosslinking reaction with the silicon-based glycidyl ether through amino groups to form a cross network structure; the adsorption foam with large adsorption pore channel and higher mechanical strength is formed by utilizing the characteristics of large specific surface area and the like of the delignified wood cellulose; the amino groups on the surface of the adsorption foam provide sites required by chemical adsorption of the adsorption foam, so that the aim of simultaneously performing physical adsorption and chemical adsorption is fulfilled.
Compared with the prior art, the invention has the following beneficial effects:
the method utilizes the renewable green environment-friendly material which has large specific surface area and high mechanical strength of the delignified wood cellulose, realizes sustainable utilization of waste, and accords with the aim of double carbon;
the delignified wood cellulose freeze-drying is in a foam structure, and has the advantages of large pore, large specific surface area, high mechanical strength, excellent regenerability, good biocompatibility, biodegradability, light texture and the like;
the invention develops a novel, green and environment-friendly method for preparing adsorption foam by utilizing simple and convenient chemical crosslinking;
the invention also provides a technical method for high adsorption quantity and controllable release of carbon dioxide at ambient temperature.
For a better understanding of the nature and technical content of the present invention, reference should be made to the following detailed description of the invention and to the accompanying drawings, which are provided for purposes of illustration and description only and are not intended to be limiting.
Drawings
FIG. 1 is a graph showing the regeneration performance test of adsorption foams DLW-GPTMS-PEI-1eq and DLW-GPTMS-PEI-2 eq;
FIG. 2 is a DLW-GPTMS-PEI-1eq adsorption rate curve of the adsorption foam;
FIG. 3 is a DLW-GPTMS-PEI-2eq adsorption rate curve of the adsorption foam;
FIG. 4 is a DLW-GPTMS-PEI-1eq desorption rate curve for adsorption foam;
FIG. 5 is a DLW-GPTMS-PEI-2eq desorption rate curve for adsorption foam;
FIG. 6 is a Fourier infrared absorption spectrum of DLW, DLW-GPTMS-PEI-1eq, DLW-GPTMS-PEI-2 eq;
FIG. 7a is a scanning electron micrograph of the adsorbent DLW-GPTMS-PEI-1 eq;
FIG. 7b is a scanning electron micrograph of the adsorbent DLW-GPTMS-PEI-2eq.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1: the preparation method of the wood cellulose-based carbon dioxide adsorption and desorption foam in the embodiment comprises the following steps:
A. carrying out dewaxing, delignification, bleaching, rinsing and other treatments on the balsawood to obtain wood cellulose;
B. uniformly dispersing 50 mg of wood cellulose in 10 ml of deionized water at ambient temperature to ensure that the concentration of the wood cellulose dispersion liquid is 0.5wt%;
C. weighing 50 mg of 3-glycidyl ether oxypropyl methyldiethoxysilane (GPTMS), and stirring for 2 hours at room temperature on a magnetic stirrer to ensure that the 3-glycidyl ether oxypropyl methyldiethoxysilane is completely crosslinked with wood cellulose;
D. weighing 50 mg of polyethyleneimine, and dissolving the polyethyleneimine in 5 ml of deionized water to ensure that the concentration of the polyethyleneimine solution is 1wt%;
E. dropping the polyethyleneimine water solution into the C at a speed of one drop per second, and continuously stirring the reaction on a magnetic stirrer for 12 hours;
F. and immediately transferring the reacted reaction solution into a beaker, quickly freezing the reaction solution for 2 hours by using liquid nitrogen, and freeze-drying the reaction solution for 48 hours by using a freeze dryer at the temperature of-80 ℃ to obtain the wood cellulose-based carbon dioxide adsorbing material, and bagging the wood cellulose-based carbon dioxide adsorbing material for later use, wherein the packed wood cellulose-based carbon dioxide adsorbing material is named as DLW-GPTMS-PEI-1eq.
Example 2: the preparation method of the wood cellulose-based carbon dioxide adsorption and desorption foam comprises the following steps:
A. carrying out dewaxing, delignification, bleaching, rinsing and other treatments on the balsa wood to obtain wood cellulose;
B. uniformly dispersing 50 mg of wood cellulose in 10 ml of deionized water at ambient temperature to ensure that the concentration of the wood cellulose dispersion liquid is 0.5wt%;
C. weighing 50 mg of 3-glycidyl ether oxypropyl methyldiethoxysilane (GPTMS), and stirring for 2 hours at room temperature on a magnetic stirrer to ensure that the 3-glycidyl ether oxypropyl methyldiethoxysilane is completely crosslinked with wood cellulose;
D. weighing 100 mg of polyethyleneimine, and dissolving the polyethyleneimine in 10 ml of deionized water to ensure that the concentration of the polyethyleneimine solution is 1wt%;
E. dripping the polyethyleneimine water solution into the C at the speed of one drop per second, and continuously stirring the reaction on a magnetic stirrer for 12 hours;
F. and immediately transferring the reacted reaction solution into a beaker, quickly freezing the reaction solution for 2 hours by using liquid nitrogen, and freeze-drying the reaction solution for 48 hours by using a freeze dryer at the temperature of minus 80 ℃ to obtain the wood cellulose-based carbon dioxide adsorption material, and bagging the wood cellulose-based carbon dioxide adsorption material for later use, wherein the wood cellulose-based carbon dioxide adsorption material is named as DLW-GPTMS-PEI-2eq.
The carbon dioxide adsorption test was performed on wood cellulose based adsorption foam by the following method:
A. placing the prepared adsorption foam in a vacuum oven at 90 ℃, carrying out heat treatment for 24 hours, removing moisture and other impurities, and activating material pore channels;
B. hermetically transferring and weighing the mixture, and recording the weight of the mixture after the mixture is cooled to room temperature;
C. putting the material into an adsorption bottle, opening an air valve, starting a diaphragm pump to enable the gas in the adsorption bottle to fully flow, and recording the time;
D. after 24 hours of adsorption, the air valve and the pump are closed, and the material is taken out, sealed and weighed.
The regeneration performance test graphs of the adsorption foam DLW-GPTMS-PEI-1eq and DLW-GPTMS-PEI-2eq are shown in figure 1; as can be seen from FIG. 1, at ambient temperature, as the cycle adsorption and desorption test period increases, the adsorption foam DLW-GPTMS-PEI-1eq is substantially maintained at an adsorption amount of above 5 mmol/g, with the highest adsorption amount being up to 5.81 mmol/g; the adsorption foam DLW-GPTMS-PEI-2eq is basically kept above the adsorption capacity of 5.5 mmol/g, wherein the highest adsorption capacity can reach 8.01 mmol/g.
The adsorption foam DLW-GPTMS-PEI-1eq adsorption rate curve is shown in figure 2; as can be seen from FIG. 2, at ambient temperature, the adsorption of carbon dioxide can be promoted due to the fact that the adsorption foam has the pore channels, the adsorption process is dominated by chemical adsorption and physical adsorption at the same time, the pore channels are filled with carbon dioxide gas along with the prolonging of the adsorption time, the DLW-GPTMS-PEI-1eq adsorption rate is gradually reduced and tends to be flat, and further the adsorption balance is achieved.
The adsorption foam DLW-GPTMS-PEI-2eq adsorption rate curve is shown in figure 3; as can be seen from fig. 3, at ambient temperature, the adsorption foam DLW-GPTMS-PEI-2eq having the same volume as the adsorption foam DLW-GPTMS-PEI-1eq has more amino groups, the initial adsorption is faster, the pore channels are filled with carbon dioxide gas, and the decrease gradually becomes gentle as the adsorption time is prolonged, so that the adsorption balance is achieved.
The desorption rate curve of the adsorption foam DLW-GPTMS-PEI-1eq is shown in figure 4; as can be seen from FIG. 4, the desorption rate of the adsorption foam DLW-GPTMS-PEI-1eq at ambient temperature is balanced after 6 hours and reaches 51% at ambient temperature along with the increase of the desorption time.
The adsorption foam DLW-GPTMS-PEI-2eq desorption rate curve is shown in figure 5; as can be seen from FIG. 5, the desorption rate of the adsorption foam DLW-GPTMS-PEI-2eq at the ambient temperature is balanced after 6 hours and reaches 19 percent at the ambient temperature along with the increase of the desorption time.
A Fourier infrared absorption spectrogram of the wood cellulose DLW, the adsorbent DLW-GPTMS-PEI-1eq and the adsorbent DLW-GPTMS-PEI-2eq is shown in figure 6; as can be seen from FIG. 6, in comparison with DLW, DLW-GPTMS-PEI-1eq of the adsorbent and DLW-GPTMS-PEI-2eq, the infrared absorption peak at 1570cm-1 of the adsorbent is attributed to the N-H bond bending vibration peak, the infrared absorption peak at 1466cm-1 is attributed to the C-N bond stretching vibration peak, the infrared absorption peaks at 2936cm-1 and 2869cm-1 are attributed to the N-H stretching vibration peak, the infrared absorption peak at 3412cm-1 is attributed to the O-H stretching vibration peak, and the infrared absorption peak at 908cm-1 is attributed to the characteristic peak of the epoxy group.
The scanning electron microscope picture of the adsorbent DLW-GPTMS-PEI-1eq is shown in FIG. 7 a; FIG. 7b shows a scanning electron microscope image of the DLW-GPTMS-PEI-2eq adsorbent, and it can be seen from FIG. 7 that the adsorption foam has large pore channels formed by crossing fiber filaments and large specific surface area, thereby providing a basis for physical adsorption.
Claims (10)
1. The wood cellulose-based carbon dioxide adsorption and desorption foam is characterized in that cellulose is used as a raw material, and dendrimer polyethyleneimine is grafted through a cross-linking agent; the cross-linking agent is 3-glycidyl ether oxypropyl methyldiethoxysilane (GPTMS).
2. The carbon dioxide adsorption and desorption foam according to claim 1, wherein the cellulose is delignified lignocellulose.
3. The method for producing carbon dioxide adsorption and desorption foam according to claim 1 or 2, which comprises the steps of:
step one, dispersing cellulose in deionized water to obtain a cellulose solution;
step two, adding a cross-linking agent into the cellulose solution, and magnetically stirring for at least 2 hours at room temperature;
step three, dropwise adding the polyethyleneimine aqueous solution while stirring, and continuously stirring for at least 12 hours after dropwise adding;
and step four, rapidly freezing the mixture for 2 hours by using liquid nitrogen, and freeze-drying the mixture for at least 48 hours at the temperature of between 80 ℃ below zero and 50 ℃ below zero to obtain the carbon dioxide adsorption and desorption foam.
4. The method according to claim 3, wherein the cellulose in the first step is obtained by dewaxing, delignification, bleaching and rinsing of balsa wood.
5. The preparation method according to claim 4, wherein the delignification is carried out in the absence of light and bleaching is carried out with 30wt% hydrogen peroxide.
6. The method according to claim 3, wherein the cellulose solution has a mass concentration of 0.5 to 1.0wt%.
7. The production method according to claim 3, wherein the mass ratio of the crosslinking agent to the cellulose is 1.
8. The production method according to claim 3, wherein the dropping rate is 1d/s to 5d/s.
9. The method according to claim 3, wherein the mass ratio of the polyethyleneimine to the cellulose is 1 (1-2).
10. The method according to claim 3, wherein the concentration of the polyethyleneimine solution is 1wt% to 5wt%.
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