CN114373566A - Natural polymer conductive aerogel and preparation method thereof - Google Patents
Natural polymer conductive aerogel and preparation method thereof Download PDFInfo
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- CN114373566A CN114373566A CN202210055615.9A CN202210055615A CN114373566A CN 114373566 A CN114373566 A CN 114373566A CN 202210055615 A CN202210055615 A CN 202210055615A CN 114373566 A CN114373566 A CN 114373566A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 102
- 229920005615 natural polymer Polymers 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 67
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 67
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 67
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 67
- 239000011240 wet gel Substances 0.000 claims abstract description 66
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 22
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 22
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 22
- 229920002678 cellulose Polymers 0.000 claims abstract description 22
- 239000001913 cellulose Substances 0.000 claims abstract description 22
- 238000004108 freeze drying Methods 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 56
- 229920001046 Nanocellulose Polymers 0.000 claims description 46
- 239000002608 ionic liquid Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 21
- RVWUHFFPEOKYLB-UHFFFAOYSA-N 2,2,6,6-tetramethyl-1-oxidopiperidin-1-ium Chemical compound CC1(C)CCCC(C)(C)[NH+]1[O-] RVWUHFFPEOKYLB-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 19
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000007710 freezing Methods 0.000 claims description 10
- 230000008014 freezing Effects 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 235000019253 formic acid Nutrition 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 11
- 238000003763 carbonization Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 24
- 239000011148 porous material Substances 0.000 description 10
- 229920001661 Chitosan Polymers 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Polymers (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a natural polymer conductive aerogel and a preparation method thereof, and relates to the technical field of conductive aerogels. When the natural polymer conductive aerogel is prepared, firstly, the modified nano-cellulose is prepared into wet gel, then the wet gel and ammonium bicarbonate are subjected to freeze drying together to prepare the aerogel, and finally, the natural polymer conductive aerogel is prepared by a carbonization process under the atmosphere of mixed gas of nitrogen and hydrogen; the modified nano-cellulose wet gel is formed by wrapping microcrystalline cellulose by long chains of alpha, omega-dihydroxy dimethyl siloxane oligomers and has a three-dimensional network structure; the natural polymer conductive aerogel prepared by the invention has good toughness and stronger adsorption capacity.
Description
Technical Field
The invention relates to the technical field of conductive aerogel, in particular to natural polymer conductive aerogel and a preparation method thereof.
Background
Carbon aerogels are novel porous carbon materials, and are found in 1989 by Pekala et al as nanoscale porous amorphous materials, which are obtained by high-temperature carbonization of aerogels. After the organic aerogel with low density, low thermal conductivity and a network structure is carbonized at high temperature, the obtained aerogel not only keeps the porous network structure of the organic aerogel, but also has excellent conductivity.
CN201610605988 discloses a modified chitosan/nanocellulose composite aerogel, a preparation method and an application thereof, wherein the chitosan is modified with sulfur to obtain modified chitosan, and then the modified chitosan is compounded with nanocellulose to prepare the sulfur-containing modified chitosan/nanocellulose composite porous aerogel; although the adsorption effect is good, the prepared product has no conductivity and poor toughness.
And the conductive aerogel prepared after natural polymer aerogel is carbonized, although the porosity is taught, the pores are often large, and even if electrostatic adsorption is utilized, the adsorption effect of the natural polymer aerogel cannot be completely developed. In order to improve the adsorption efficiency, the natural polymer conductive aerogel with high toughness and strong adsorption capacity is researched and prepared.
Disclosure of Invention
The invention aims to provide a natural polymer conductive aerogel and a preparation method thereof, so as to solve the problems in the background technology.
A preparation method of natural polymer conductive aerogel sequentially comprises the following steps: preparing modified nano cellulose wet gel, preparing aerogel, and preparing natural high-molecular conductive aerogel; the preparation method is characterized in that the preparation of the modified nano-cellulose wet gel comprises the steps of putting pretreated microcrystalline cellulose into ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide, and then adding alpha, omega-dihydroxy dimethyl siloxane oligomer for reaction to prepare the modified nano-cellulose wet gel.
Preferably, the preparation process of the aerogel comprises the steps of adding an ammonium bicarbonate solution into the wet modified nano-cellulose gel treated by acetone, sealing, heating to 40-50 ℃, reacting, and carrying out freeze drying and low-temperature vacuum drying treatment to obtain the aerogel.
Preferably, the preparation of the natural polymer conductive aerogel comprises the following steps: and placing the aerogel in a tubular furnace, replacing the air in the furnace with a mixed gas of hydrogen and nitrogen, and sintering at high temperature to obtain the natural polymer conductive aerogel.
Preferably, the preparation method of the natural polymer conductive aerogel comprises the following specific steps:
(1) placing the pretreated microcrystalline cellulose in an ionic liquid with the mass 20-30 times that of the microcrystalline cellulose, uniformly stirring until the microcrystalline cellulose is dissolved, adding alpha and omega-dihydroxydimethylsiloxane oligomers with the mass 0.3-0.5 time that of the microcrystalline cellulose, and stirring at room temperature and 150-300 rpm for 24-28 hours to prepare modified nano-cellulose wet gel;
(2) adding an ammonium bicarbonate solution which is 0.15-0.3 time of the mass of the modified nanocellulose wet gel and 10-25% of the mass of the modified nanocellulose wet gel into the acetone-treated modified nanocellulose wet gel, sealing, heating to 40-50 ℃, reacting for 30-50 min, transferring to a freeze dryer, and immediately carrying out freeze drying and low-temperature vacuum drying treatment to prepare aerogel;
(3) placing the aerogel in a tubular furnace, and replacing the air in the furnace with a mixed gas of hydrogen and nitrogen, wherein the mass ratio of the nitrogen to the hydrogen is 0.5: 1-1: 1, heating to 800-1000 ℃ at a speed of 4-5 ℃/min, preserving heat for 2-3 h, and cooling to room temperature to obtain the natural polymer conductive aerogel.
Preferably, in the step (1): the process for pretreating the microcrystalline cellulose comprises the following steps: dispersing microcrystalline cellulose in a formic acid solution with the mass fraction of 3-5% being 50-60 times of the mass of the microcrystalline cellulose, performing ultrasonic treatment at 20 ℃ and 50-60 kHz for 3-5 h, adding distilled water with the mass being 100-200 times of the mass of the microcrystalline cellulose, and performing rapid filtration by using filter paper under a vacuum condition to obtain the pretreated microcrystalline cellulose.
Preferably, in the step (1): in the ionic liquid, the mass ratio of the imidazole ionic liquid to the 2,2,6, 6-tetramethyl piperidine oxide is 10: 0.05-10: 0.15.
preferably, in the step (1): the preparation method of the alpha, omega-dihydroxy dimethyl siloxane oligomer comprises the following steps: octamethylcyclotetrasiloxane, acetic anhydride and aluminum oxide in a mass ratio of 5: 1: 0.08-5: 1.5: 0.1, mixing, placing in a three-neck flask, heating to 120 ℃, carrying out reflux reaction for 8-10 h, cooling to 50 ℃, carrying out suction filtration, washing the filtrate for 3-5 times by using a mixed solution of sodium chloride and ammonium bicarbonate with the mass fraction of 10%, placing in the three-neck flask after washing, adding deionized water with the mass of 2-3 times that of octamethylcyclotetrasiloxane, reacting for 3-4 h at 70 ℃, cooling to room temperature, washing for 3-5 times by using the deionized water, separating liquid, and carrying out reduced pressure distillation to obtain the alpha, omega-dihydroxydimethylsiloxane oligomer.
Preferably, in the step (2): the process of treating the modified nanocellulose wet gel by acetone comprises the following steps: and immersing the modified nano-cellulose wet gel in acetone, replacing the acetone once every 24 hours and three times to obtain the acetone-treated modified nano-cellulose wet gel.
Preferably, in the step (2): during freeze drying, the freezing temperature is-48 to-52 ℃, the freezing time is 12 to 15 hours, and during low-temperature vacuum drying treatment, the pressure is 1Pa, and the drying time is 48 hours.
Preferably, the natural polymer conductive aerogel prepared by the preparation method of the natural polymer conductive aerogel comprises the following raw materials in percentage by weight: 20-30 parts of modified nano cellulose wet gel and 3-9 parts of ammonium bicarbonate solution; the modified nano-cellulose wet gel is prepared by dissolving microcrystalline cellulose in ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide, and adding alpha, omega-dihydroxy dimethyl siloxane oligomer after dissolving; the ionic liquid is imidazole ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide; the mass fraction of the ammonium bicarbonate solution is 10-25%.
Preferably, the modified nano-cellulose wet gel is prepared by dissolving microcrystalline cellulose in ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide, and adding alpha, omega-dihydroxydimethylsiloxane oligomer after dissolving; the ionic liquid is imidazole ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide; the mass fraction of the ammonium bicarbonate solution is 10-25%.
Compared with the prior art, the invention has the following beneficial effects:
when the natural polymer conductive aerogel is prepared, the modified nano-cellulose is firstly prepared into wet gel, then the wet gel is dried to prepare the aerogel, and finally the carbonization process is carried out to prepare the natural polymer conductive aerogel;
dissolving microcrystalline cellulose in ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide, adding alpha, omega-dihydroxy dimethyl siloxane oligomer after dissolving, and modifying nano cellulose wet gel; the 2,2,6, 6-tetramethylpiperidine oxide oxidizes hydroxyl on the surface of the nanocellulose into carboxyl, so that the dissolution of a crystallization area of the microcrystalline cellulose is improved, and simultaneously, under the catalysis of the 2,2,6, 6-tetramethylpiperidine oxide, the residual hydroxyl and the generated carboxyl of the microcrystalline cellulose are crosslinked with alpha, omega-dihydroxydimethylsiloxane oligomer to form a modified nanocellulose wet gel with a long chain wrapping and three-dimensional network structure, so that the strength of the modified nanocellulose wet gel is increased, and the toughness of the conductive aerogel is enhanced;
when drying, adding ammonium bicarbonate into the modified nano-cellulose wet gel, sealing and heating, and then freeze-drying; decomposing ammonium bicarbonate to generate ammonia gas, water and carbon dioxide during heating, sealing to enable the gas to be left in the modified nanocellulose wet gel, enabling the ammonia gas to react with hydroxyl and carboxyl to aminate the modified nanocellulose wet gel to form a bridge in the wet gel, and performing freeze drying, thermal expansion and cold contraction to enable pores in the aerogel to be dispersed by the bridge, then performing contraction, so that the pores are reduced, the porosity is increased, and the adsorption capacity is enhanced; when carrying out the carbonization technology at last, regard as the protective gas with nitrogen gas and hydrogen, on the one hand for aerogel supplyes ammonia and continue the reaction, on the other hand adsorbs the carbon dioxide who produces and gets rid of from the aerogel, prevents that the carbon dioxide that produces from influencing the adsorptivity of electrically conductive aerogel during the drying.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are given to illustrate the method for testing each index of the natural polymer conductive aerogel prepared in the examples and comparative examples as follows:
toughness: the elastic modulus of the natural polymer conductive aerogel prepared in the embodiment and the comparative example is detected by a static method;
adsorptivity: the natural polymer conductive aerogel prepared in the examples and the comparative examples is subjected to surface, area and pore size tests by using an adsorption instrument.
Example 1
A natural polymer conductive aerogel mainly comprises the following components in parts by weight:
20 parts of modified nano-cellulose wet gel and 3 parts of ammonium bicarbonate solution.
A preparation method of natural polymer conductive aerogel comprises the following steps:
(1) dispersing microcrystalline cellulose in a formic acid solution with the mass fraction of 5 percent 50 times that of the microcrystalline cellulose, performing ultrasonic treatment at 20 ℃ and 50kHz for 3h, adding distilled water with the mass of 100 times that of the microcrystalline cellulose, and performing rapid filtration by using filter paper under a vacuum condition to obtain pretreated microcrystalline cellulose; the mass ratio of 1,2, 4-triazole ionic liquid to 2,2,6, 6-tetramethylpiperidine oxide is 10: 0.05 mixing to prepare ionic liquid; octamethylcyclotetrasiloxane, acetic anhydride and aluminum oxide in a mass ratio of 5: 1: 0.08 of the mixture is placed in a three-neck flask, the mixture is heated to 120 ℃ and is subjected to reflux reaction for 8 hours, the mixture is cooled to 50 ℃ and then is subjected to suction filtration, the filtrate is washed for 3 times by using a mixed solution of sodium chloride and sodium bicarbonate with the mass fraction of 10%, the washed filtrate is placed in the three-neck flask, deionized water with the mass of 2 times that of octamethylcyclotetrasiloxane is added, the mixture is reacted for 3 hours at 70 ℃, the temperature is cooled to room temperature, the washed filtrate is washed for 3 times by using the deionized water, liquid separation is carried out, and reduced pressure distillation is carried out, so that alpha, omega-dihydroxydimethylsiloxane oligomer is prepared; placing the pretreated microcrystalline cellulose in ionic liquid with the mass 20 times that of the microcrystalline cellulose, uniformly stirring until the microcrystalline cellulose is dissolved, adding alpha and omega-dihydroxydimethylsiloxane oligomers with the mass 0.3 time that of the microcrystalline cellulose, and stirring at room temperature and 150rpm for 28 hours to prepare modified nano-cellulose wet gel;
(2) immersing the modified nanocellulose wet gel in acetone, replacing the acetone once every 24 hours and three times to obtain the acetone-treated modified nanocellulose wet gel; adding an ammonium bicarbonate solution with the mass fraction of 10 percent, which is 0.15 times of the mass of the modified nanocellulose wet gel, into the acetone-treated modified nanocellulose wet gel, sealing, heating to 40 ℃, reacting for 30min, transferring to a freeze dryer, and immediately performing freeze drying and low-temperature vacuum drying, wherein during freeze drying, the freezing temperature is-48 ℃, the freezing time is 12 hours, during low-temperature vacuum drying, the pressure is 1Pa, and the drying time is 48 hours to prepare the aerogel;
(3) mixing nitrogen and hydrogen in a mass ratio of 0.5: 1 mixing to prepare mixed gas; and (3) placing the aerogel in a tubular furnace, replacing the air in the furnace with mixed gas, heating to 800-1000 ℃ at a speed of 4 ℃/min, preserving the heat for 2 hours, and cooling to room temperature to obtain the natural polymer conductive aerogel.
Example 2
A natural polymer conductive aerogel mainly comprises the following components in parts by weight:
25 parts of modified nano-cellulose wet gel and 5 parts of ammonium bicarbonate solution.
A preparation method of natural polymer conductive aerogel comprises the following steps:
(1) dispersing microcrystalline cellulose in a formic acid solution with mass fraction of 4% and mass which is 55 times of that of the microcrystalline cellulose, performing ultrasonic treatment at 20 ℃ and 55kHz for 4h, adding distilled water with mass which is 150 times of that of the microcrystalline cellulose, and rapidly filtering by using filter paper under a vacuum condition to obtain pretreated microcrystalline cellulose; the mass ratio of 1,2, 4-triazole ionic liquid to 2,2,6, 6-tetramethylpiperidine oxide is 10: 0.1 mixing to prepare ionic liquid; octamethylcyclotetrasiloxane, acetic anhydride and aluminum oxide in a mass ratio of 5: 1: 0.09, mixing and placing the mixture in a three-neck flask, heating the mixture to 120 ℃, carrying out reflux reaction for 9 hours, cooling the mixture to 50 ℃, carrying out suction filtration, washing the filtrate for 4 times by using a mixed solution of sodium chloride and sodium bicarbonate with the mass fraction of 10%, placing the washed filtrate in the three-neck flask, adding deionized water with the mass of 3 times that of octamethylcyclotetrasiloxane, reacting for 4 hours at 70 ℃, cooling the mixture to room temperature, washing the mixture for 4 times by using the deionized water, separating liquid, and carrying out reduced pressure distillation to prepare alpha, omega-dihydroxydimethylsiloxane oligomer; placing the pretreated microcrystalline cellulose in ionic liquid with the mass 25 times that of the microcrystalline cellulose, uniformly stirring until the microcrystalline cellulose is dissolved, adding alpha and omega-dihydroxydimethylsiloxane oligomers with the mass 0.4 times that of the microcrystalline cellulose, and stirring at room temperature and 200rpm for 26 hours to prepare modified nano-cellulose wet gel;
(2) immersing the modified nanocellulose wet gel in acetone, replacing the acetone once every 24 hours and three times to obtain the acetone-treated modified nanocellulose wet gel; adding an ammonium bicarbonate solution with the mass fraction of 15 percent which is 0.2 times that of the modified nanocellulose wet gel into the acetone-treated modified nanocellulose wet gel, sealing, heating to 45 ℃, reacting for 40min, transferring to a freeze dryer, and immediately performing freeze drying and low-temperature vacuum drying treatment, wherein the freezing temperature is-50 ℃, the freezing time is 14h, the pressure is 1Pa and the drying time is 48h during freeze drying, so as to prepare the aerogel;
(3) mixing nitrogen and hydrogen in a mass ratio of 0.8: 1 mixing to prepare mixed gas; placing the aerogel in a tubular furnace, replacing the air in the furnace with mixed gas, heating to 9000 ℃ at the speed of 4.5 ℃/min, preserving the heat for 2.5h, and cooling to room temperature to obtain the natural polymer conductive aerogel.
Example 3
A natural polymer conductive aerogel mainly comprises the following components in parts by weight:
30 parts of modified nano-cellulose wet gel and 6 parts of ammonium bicarbonate solution.
A preparation method of natural polymer conductive aerogel comprises the following steps:
(1) dispersing microcrystalline cellulose in a formic acid solution with the mass fraction of 5 percent being 60 times of the mass of the microcrystalline cellulose, carrying out ultrasonic treatment at 20 ℃ and 60kHz for 5 hours, adding distilled water with the mass being 200 times of the mass of the microcrystalline cellulose, and rapidly filtering by using filter paper under a vacuum condition to obtain pretreated microcrystalline cellulose; mixing 1, 3-dimethyl-3-imidazole hexafluorophosphate ionic liquid and 2,2,6, 6-tetramethyl piperidine oxide according to the mass ratio of 10: 0.15 mixing to prepare ionic liquid; octamethylcyclotetrasiloxane, acetic anhydride and aluminum oxide in a mass ratio of 5: 1.5: 0.1, mixing and placing in a three-neck flask, heating to 120 ℃, carrying out reflux reaction for 10 hours, cooling to 50 ℃, carrying out suction filtration, washing the filtrate for 5 times by using a mixed solution of sodium chloride and sodium bicarbonate with the mass fraction of 10%, placing in the three-neck flask after washing, adding deionized water with the mass of 3 times that of octamethylcyclotetrasiloxane, reacting for 4 hours at 70 ℃, cooling to room temperature, washing for 5 times by using the deionized water, separating liquid, and carrying out reduced pressure distillation to obtain alpha, omega-dihydroxydimethylsiloxane oligomer; placing the pretreated microcrystalline cellulose in ionic liquid with the mass 30 times that of the microcrystalline cellulose, uniformly stirring until the microcrystalline cellulose is dissolved, adding alpha and omega-dihydroxydimethylsiloxane oligomers with the mass 0.5 time that of the microcrystalline cellulose, and stirring at room temperature and 300rpm for 24 hours to prepare modified nano-cellulose wet gel;
(2) immersing the modified nanocellulose wet gel in acetone, replacing the acetone once every 24 hours and three times to obtain the acetone-treated modified nanocellulose wet gel; adding an ammonium bicarbonate solution with the mass fraction of 25 percent, which is 0.3 time of the mass of the modified nanocellulose wet gel, into the acetone-treated modified nanocellulose wet gel, sealing, heating to 50 ℃, reacting for 50min, transferring to a freeze dryer, and immediately performing freeze drying and low-temperature vacuum drying, wherein during freeze drying, the freezing temperature is-52 ℃, the freezing time is 15 hours, during low-temperature vacuum drying, the pressure is 1Pa, and the drying time is 48 hours to prepare the aerogel;
(3) mixing nitrogen and hydrogen in a mass ratio of 1: 1 mixing to prepare mixed gas; placing the aerogel in a tubular furnace, replacing the air in the furnace with mixed gas, heating to 1000 ℃ at the speed of 5 ℃/min, preserving heat for 3h, and cooling to room temperature to obtain the natural polymer conductive aerogel.
Comparative example 1
The formulation of comparative example 1 was the same as that of example 2. The natural polymer conductive aerogel and the preparation method thereof are only different from the embodiment 2 in the step (1), and the step (1) is modified as follows: dispersing microcrystalline cellulose in a formic acid solution with mass fraction of 4% and mass which is 55 times of that of the microcrystalline cellulose, performing ultrasonic treatment at 20 ℃ and 55kHz for 4h, adding distilled water with mass which is 150 times of that of the microcrystalline cellulose, and rapidly filtering by using filter paper under a vacuum condition to obtain pretreated microcrystalline cellulose; the mass ratio of the imidazole ionic liquid to the 2,2,6, 6-tetramethyl piperidine oxide is 10: 0.1 mixing to prepare ionic liquid; and (3) placing the pretreated microcrystalline cellulose in ionic liquid with the mass of 25 times that of the microcrystalline cellulose, uniformly stirring until the microcrystalline cellulose is dissolved, and stirring at room temperature and 200rpm for 26 hours to prepare the modified nano cellulose wet gel. The rest of the procedure was the same as in example 2.
Comparative example 2
Comparative example 2 was formulated in the same manner as in example 2. The natural polymer conductive aerogel and the preparation method thereof are only different from the embodiment 2 in the step (1), and the step (1) is modified as follows: dispersing microcrystalline cellulose in a formic acid solution with mass fraction of 4% and mass which is 55 times of that of the microcrystalline cellulose, performing ultrasonic treatment at 20 ℃ and 55kHz for 4h, adding distilled water with mass which is 150 times of that of the microcrystalline cellulose, and rapidly filtering by using filter paper under a vacuum condition to obtain pretreated microcrystalline cellulose; octamethylcyclotetrasiloxane, acetic anhydride and aluminum oxide in a mass ratio of 5: 1: 0.09, mixing and placing the mixture in a three-neck flask, heating the mixture to 120 ℃, carrying out reflux reaction for 9 hours, cooling the mixture to 50 ℃, carrying out suction filtration, washing the filtrate for 4 times by using a mixed solution of sodium chloride and sodium bicarbonate with the mass fraction of 10%, placing the washed filtrate in the three-neck flask, adding deionized water with the mass of 3 times that of octamethylcyclotetrasiloxane, reacting for 4 hours at 70 ℃, cooling the mixture to room temperature, washing the mixture for 4 times by using the deionized water, separating liquid, and carrying out reduced pressure distillation to prepare alpha, omega-dihydroxydimethylsiloxane oligomer; placing the pretreated microcrystalline cellulose in ionic liquid with the mass 25 times that of the microcrystalline cellulose, uniformly stirring until the microcrystalline cellulose is dissolved, adding alpha and omega-dihydroxydimethylsiloxane oligomers with the mass 0.4 times that of the microcrystalline cellulose, and stirring at room temperature and 200rpm for 26 hours to prepare the modified nanocellulose wet gel. The rest of the procedure was the same as in example 2.
Comparative example 3
The formulation of comparative example 3 was the same as that of example 2. The natural polymer conductive aerogel and the preparation method thereof are only different from the embodiment 2 in the step (2), and the step (2) is modified as follows: immersing the modified nanocellulose wet gel in acetone, replacing the acetone once every 24 hours and three times to obtain the acetone-treated modified nanocellulose wet gel; sealing the acetone-treated modified nanocellulose wet gel, heating to 45 ℃, reacting for 40min, transferring to a freeze dryer, and immediately performing freeze drying and low-temperature vacuum drying at-50 ℃ for 14h, under 1Pa for 48h, to obtain the aerogel. The rest of the procedure was the same as in example 2.
Comparative example 4
Comparative example 4 was formulated as in example 2. The natural polymer conductive aerogel and the preparation method thereof are different from the embodiment 2 only in the difference of the step (3), and the step (3) is modified as follows: and (3) placing the aerogel in a tubular furnace, replacing the air in the furnace with nitrogen, heating to 800-1000 ℃ at a speed of 4-5 ℃/min, preserving the heat for 2-3 h, and cooling to room temperature to obtain the natural polymer conductive aerogel. The rest of the procedure was the same as in example 2.
Comparative example 5
Comparative example 5 is the sulfur-containing modified chitosan aerogel prepared in example 1 of CN 201610605988.
Examples of effects
Table 1 below shows the results of performance analysis of rubber materials prepared using the natural polymer conductive aerogels of examples 1 and 2 and comparative examples 1,2, 3, and 4 according to the present invention.
TABLE 1
| Impact toughness (kJ/m)2) | Specific surface area (m)2/g) | Average pore diameter (nm) | |
| Example 1 | 6.0 | 372 | 5.08 |
| Example 2 | 6.1 | 365 | 5.13 |
| Example 3 | 5.9 | 369 | 5.02 |
| Comparative example 1 | 4.2 | 310 | 6.52 |
| Comparative example 2 | 4.9 | 327 | 6.34 |
| Comparative example 3 | 5.8 | 361 | 7.10 |
| Comparative example 4 | 5.7 | 319 | 6.49 |
| Comparative example 5 | 4.3 | 360 | 5.16 |
Compared with the experimental data of the comparative example and the example in table 1, it can be clearly found that the natural polymer conductive aerogels prepared in examples 1 and 2 have good impact toughness, large specific surface area and small average pore diameter, which indicates that the natural polymer conductive aerogels have excellent toughness and adsorbability;
from the comparison of the experimental data of examples 1,2, 3 and comparative examples 1 and 2, it can be found that when the natural polymer conductive aerogel is prepared, the alpha, omega-dihydroxydimethylsiloxane oligomer is added, and under the catalysis of 2,2,6, 6-tetramethylpiperidine oxide, the residual hydroxyl groups and generated carboxyl groups of the microcrystalline cellulose are crosslinked with the alpha, omega-dihydroxydimethylsiloxane oligomer to form a long-chain wrapped modified nanocellulose wet gel with a three-dimensional network structure, so that the strength of the modified nanocellulose wet gel is increased, and the toughness of the conductive aerogel is enhanced, but the toughness of the conductive aerogel cannot be enhanced only by using the alpha, omega-dihydroxydimethylsiloxane oligomer;
from the comparison of the experimental data of example 1, example 2, example 3 and comparative example 3, it can be seen that, during freeze drying, ammonium bicarbonate is added into the modified nanocellulose wet gel, the modified nanocellulose wet gel is aminated, a bridge is formed inside the wet gel, the aerogel with larger pores is divided, air impingement is reduced, the specific surface area of the conductive aerogel is increased, and the adsorption capacity is enhanced, and when ammonium bicarbonate is not added, the prepared conductive aerogel has larger average pore diameter and weaker adsorption capacity.
From the comparison of the experimental data of example 1, example 2, example 3 and comparative example 4, it can be seen that hydrogen is omitted during the sintering process, and only nitrogen is used as the shielding gas, so that the average pore diameter of the aerogel is larger, the specific surface area is smaller, which indicates that the shielding gas not only can supplement ammonia gas to continue the reaction, but also reduces the influence of carbon dioxide generated during drying on the adsorption of the aerogel.
From the comparison of the experimental data of example 1, example 2, example 3 and comparative example 5, it can be seen that, after the modified chitosan is obtained by modifying chitosan with sulfur, the modified chitosan/nanocellulose composite porous aerogel containing sulfur is prepared by compounding with nanocellulose, the average pore size is small, the specific surface area is large, but alpha, omega-dihydroxydimethylsiloxane oligomer and 2,2,6, 6-tetramethylpiperidine oxide are not used, so that the toughness is poor, which indicates that under the catalysis of 2,2,6, 6-tetramethylpiperidine oxide, alpha, omega-dihydroxydimethylsiloxane oligomer can react with microcrystalline cellulose to form a three-dimensional network structure with strong toughness.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. A preparation method of natural polymer conductive aerogel sequentially comprises the following steps: preparing modified nano cellulose wet gel, preparing aerogel, and preparing natural high-molecular conductive aerogel; the preparation method is characterized in that the preparation of the modified nano-cellulose wet gel comprises the steps of putting pretreated microcrystalline cellulose into ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide, and then adding alpha, omega-dihydroxy dimethyl siloxane oligomer for reaction to prepare the modified nano-cellulose wet gel.
2. The method for preparing the natural polymer conductive aerogel according to claim 1, wherein the aerogel preparation process comprises adding an ammonium bicarbonate solution into the acetone-treated modified nanocellulose wet gel, sealing, heating to 40-50 ℃, reacting, and performing freeze drying and low-temperature vacuum drying to obtain the aerogel.
3. The method for preparing natural polymer conductive aerogel according to claim 1, wherein the preparation of natural polymer conductive aerogel comprises: and placing the aerogel in a tubular furnace, replacing the air in the furnace with a mixed gas of hydrogen and nitrogen, and sintering at high temperature to obtain the natural polymer conductive aerogel.
4. The preparation method of the natural polymer conductive aerogel according to claim 1, comprising the following steps:
(1) placing pretreated microcrystalline cellulose in ionic liquid with the mass 20-30 times of that of the microcrystalline cellulose, uniformly stirring the ionic liquid to dissolve the ionic liquid, adding alpha and omega-dihydroxydimethylsiloxane oligomers with the mass 0.3-0.5 time of that of the microcrystalline cellulose, and stirring the mixture at room temperature and 150-300 rpm for 24-28 hours to prepare modified nanocellulose wet gel;
(2) adding an ammonium bicarbonate solution which is 0.15-0.3 time of the mass of the modified nanocellulose wet gel and 10-25% of the mass of the modified nanocellulose wet gel into the acetone-treated modified nanocellulose wet gel, sealing, heating to 40-50 ℃, reacting for 30-50 min, transferring to a freeze dryer, and immediately carrying out freeze drying and low-temperature vacuum drying treatment to prepare aerogel;
(3) placing the aerogel in a tubular furnace, and replacing the air in the furnace with a mixed gas of hydrogen and nitrogen, wherein the mass ratio of the nitrogen to the hydrogen is 0.5: 1-1: 1, heating to 800-1000 ℃ at a speed of 4-5 ℃/min, preserving heat for 2-3 h, and cooling to room temperature to obtain the natural polymer conductive aerogel.
5. The method for preparing natural polymer conductive aerogel according to claim 4, wherein in the step (1): the process for pretreating the microcrystalline cellulose comprises the following steps: dispersing microcrystalline cellulose in a formic acid solution with the mass fraction of 3-5% being 50-60 times of the mass of the microcrystalline cellulose, performing ultrasonic treatment at 20 ℃ and 50-60 kHz for 3-5 h, adding distilled water with the mass being 100-200 times of the mass of the microcrystalline cellulose, and performing rapid filtration by using filter paper under a vacuum condition to obtain the pretreated microcrystalline cellulose.
6. The method for preparing natural polymer conductive aerogel according to claim 4, wherein in the step (1): in the ionic liquid, the mass ratio of the imidazole ionic liquid to the 2,2,6, 6-tetramethyl piperidine oxide is 10: 0.05-10: 0.15.
7. the method for preparing natural polymer conductive aerogel according to claim 4, wherein in the step (1): the preparation method of the alpha, omega-dihydroxy dimethyl siloxane oligomer comprises the following steps: octamethylcyclotetrasiloxane, acetic anhydride and aluminum oxide in a mass ratio of 5: 1: 0.08-5: 1.5: 0.1, mixing, placing in a three-neck flask, heating to 120 ℃, carrying out reflux reaction for 8-10 h, cooling to 50 ℃, carrying out suction filtration, washing the filtrate for 3-5 times by using a mixed solution of sodium chloride and ammonium bicarbonate with the mass fraction of 10%, placing in the three-neck flask after washing, adding deionized water with the mass of 2-3 times that of octamethylcyclotetrasiloxane, reacting for 3-4 h at 70 ℃, cooling to room temperature, washing for 3-5 times by using the deionized water, separating liquid, and carrying out reduced pressure distillation to obtain the alpha, omega-dihydroxydimethylsiloxane oligomer.
8. The method for preparing natural polymer conductive aerogel according to claim 4, wherein in the step (2): the process of treating the modified nanocellulose wet gel by acetone comprises the following steps: and immersing the modified nano-cellulose wet gel in acetone, replacing the acetone once every 24 hours and three times to obtain the acetone-treated modified nano-cellulose wet gel.
9. The method for preparing natural polymer conductive aerogel according to claim 4, wherein in the step (2): during freeze drying, the freezing temperature is-48 to-52 ℃, the freezing time is 12 to 15 hours, and during low-temperature vacuum drying treatment, the pressure is 1Pa, and the drying time is 48 hours.
10. The method for preparing natural polymer conductive aerogel according to claim 9, wherein the natural polymer conductive aerogel prepared by the method comprises the following raw materials by weight: 20-30 parts of modified nano cellulose wet gel and 3-9 parts of ammonium bicarbonate solution; the modified nano-cellulose wet gel is prepared by dissolving microcrystalline cellulose in ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide, and adding alpha, omega-dihydroxy dimethyl siloxane oligomer after dissolving; the ionic liquid is imidazole ionic liquid containing 2,2,6, 6-tetramethyl piperidine oxide; the mass fraction of the ammonium bicarbonate solution is 10-25%.
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