CN106517144A - Method for preparing carbon nanofiber aerogel from wood - Google Patents

Method for preparing carbon nanofiber aerogel from wood Download PDF

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CN106517144A
CN106517144A CN201611010665.6A CN201611010665A CN106517144A CN 106517144 A CN106517144 A CN 106517144A CN 201611010665 A CN201611010665 A CN 201611010665A CN 106517144 A CN106517144 A CN 106517144A
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cellulose
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aerogel
wood
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CN106517144B (en
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俞书宏
李思成
梁海伟
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University of Science and Technology of China USTC
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/01Crystal-structural characteristics depicted by a TEM-image
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    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00Foams characterised by their properties
    • C08J2205/02Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026Aerogel, i.e. a supercritically dried gel
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02Cellulose; Modified cellulose

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Abstract

The invention provides a method for preparing carbon nanofiber aerogel from wood. The method comprises the following steps: a) pre-treating the wood to obtain wood pulp; b) mixing the wood pulp with tetramethylpiperidine oxide, sodium bromide and sodium hypochlorite for an oxidation reaction to obtain a cellulose suspension; c) performing suction filtration on the cellulose suspension, dispersing the cellulose suspension in water to obtain a homogeneous viscous nanometer cellulose solution; d) acidizing the nanometer cellulose solution in an acidic environment to obtain nanometer cellulose hydrogel; e) performing solvent exchanging on the nanometer cellulose hydrogel in acetone containing p-toluenesulfonic acid, performing drying with a CO2 supercritical drying method to obtain nanocellulose aerogel; f)performing high temperature pyrolysis on the nanocellulose aerogel in a tubular furnace inert gas atmosphere to obtain the carbon nanofiber aerogel. According to the method, the carbon nanofiber aerogel is prepared from the wood as a raw material and has characteristics of uniform diameter, low density and large specific surface area as well as properties of heat insulation, fire resistance and the like.

Description

A kind of method that carbon nano-fiber aeroge is prepared by timber
Technical field
The present invention relates to technical field of nano material, more particularly to a kind of side that carbon nano-fiber aeroge is prepared by timber Method.
Background technology
The carbon nano-fiber aeroge being made up of tridimensional network, with very low density, big specific surface area, high electricity The excellent physical property such as conductance and porous, is a kind of new material for receiving significant attention.Carbon aerogels can serve as catalysis Agent carrier, artificial-muscle, the electrode of ultracapacitor, absorbent and detector.Especially, it is ultralight or have elasticity Carbon aerogels have many application prospects.For example, the graphene-structured of ultralight N doping is used as absorbent and ultracapacitor Electrode, shows great absorptive capacity and special electric capacity;The elastic conductor that grapheme foam based on elasticity makes, in stretching With electric conductivity and electrical stability have been remained in that in the case of bending.
Various methods for preparing carbon aerogels are prior art discloses, such as Germany《Advanced material》(Advanced Materials, page 617 of 22 phase in 2010) a kind of dichlorobenzene solution for using ferrocene is disclosed as precursor, using chemistry Vapour deposition process come the method for preparing CNT sponge aeroge, the CNT sponge aeroge that this method is prepared with compared with Good engineering propertiess, but chemical vapor deposition needs the device of complex and expensive, and which is unable to large-scale production, prevents the method Prospects for commercial application.Germany《Applied chemistry》(AngewandteChemie International Edition, 51 phases in 2012 Page 5101) report by using glucose as precursor, carbon fibre airsetting is prepared on a large scale using hydrothermal carbonization process Glue, but use poisonous and expensive tellurium nano-wire as template during being somebody's turn to do, and this preparation process is not suitable for commercialization.Germany 《Applied chemistry》(AngewandteChemie International Edition, 2013 52 phase page 2925) reported one kind Ultralight, the method for elasticity and fire resisting carbon nano-fiber aeroge, although Bacterial cellulose be is prepared using bacterial fibers usually Typical biological material is planted, but industrialized fermentation preparation process remains a need for higher cost.
Therefore, for the popularization and application on a large scale of carbon nano-fiber aeroge, find a kind of preparation method of low cost It is current urgent problem.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide one kind to prepare carbon nano-fiber aeroge by timber Method, the timber that raw material is widely present for nature, preparation cost are very low.
The invention provides a kind of method that carbon nano-fiber aeroge is prepared by timber, including:
A) timber is carried out into pre-treatment, obtains wood pulp;
B) above-mentioned wood pulp is mixed with tetramethyl piperidine oxides, sodium bromide and sodium hypochlorite, carries out oxidation reaction, obtain Cellulose suspension;
C) after by above-mentioned cellulose suspension sucking filtration, it is dispersed in water, breaks up, obtains homogeneous thick nano-cellulose Solution;
D) above-mentioned nano-cellulose solution is acidified under sour environment, is obtained nanofiber hydrogel;
E) above-mentioned nanofiber hydrogel is carried out into solvent exchange in the acetone containing p-methyl benzenesulfonic acid, using CO2It is super Critical seasoning is dried, and obtains nano-cellulose aerogel;
F) nano-cellulose aerogel is obtained into carbon nano-fiber aeroge in the pyrolysis of tube furnace high temperature.
The present invention adopts timber that carbon nano-fiber aeroge is prepared for raw material first, and common wood is carried out front place first Reason, obtains wood pulp.Preferably, sodium hydroxide solution and acid sodium chlorite solution's multi-reflow are respectively adopted, obtain what is bleached Wood pulp.
The sodium hydroxide solution is preferably sodium hydrate aqueous solution, and its mass concentration is preferably 5wt%~10wt%, more Preferably 7wt%.
The acid sodium chlorite solution is preferably acid sodium chlorite aqueous solution, and its mass concentration is preferably 0.5wt% ~1.5wt%, more preferably 1wt%.
Then wood pulp is mixed with tetramethyl piperidine oxides (TEMPO), sodium bromide and sodium hypochlorite, carries out aoxidizing instead Should, obtain cellulose suspension.
Preferably, the mass body of the solid content of the wood pulp, tetramethyl piperidine oxides, sodium bromide and liquor natrii hypochloritises Product is than being (1g):(0.01~0.03g):(0.05~0.2g):(5~15mL), more preferably (1g):(0.016g):(0.1g): (10ml), the mass content of the liquor natrii hypochloritises is preferably 5wt%~15wt%, more preferably 9wt%.
The liquor natrii hypochloritises are preferably aqueous sodium hypochlorite solution.
The temperature of the oxidation reaction is preferably 20 DEG C~25 DEG C, and the time is preferably 4h~10h.
The oxidation reaction is preferably carried out under alkaline environment, and the pH value of the alkaline environment is preferably 10~103.
Then the cellulose suspension obtained after oxidation is carried out into sucking filtration, the thick white shape material for obtaining is scattered in water In, break up, obtain homogeneous thick nano-cellulose solution.
The application is broken up and is not particularly limited to described, only need to carry out slight mechanical treatment to cellulose, preferably , described breaing up is to use blender, and rotating speed is preferably 37000~50000 turns/min.
It is currently preferred, after breaing up, in being additionally included in cell crushing instrument, carry out supersound process.
Then above-mentioned nano-cellulose solution is acidified under sour environment, is obtained nanofiber hydrogel.
The acid compound adopted to the sour environment of the invention is simultaneously not particularly limited, preferably to the nano-cellulose Hydrochloric acid is added to carry out acidification in solution.
The pH value of the sour environment is preferably 2~3.
Then above-mentioned nanofiber hydrogel is carried out into solvent exchange in the acetone containing p-methyl benzenesulfonic acid, is reused CO2Supercritical drying is dried, and obtains nano-cellulose aerogel.
Preferably, the mass ratio of the nanofiber hydrogel solid content and p-methyl benzenesulfonic acid is 5~15: 1, more preferably For 10:1.
The time of the solvent exchange is 3~4 days.
Preferably, the CO2The temperature of supercritical drying sample room is 50 DEG C, and pressure is 9.0MPa.
Finally the nano-cellulose aerogel is pyrolyzed in tube furnace high temperature, you can obtain carbon nano-fiber airsetting Glue.
Present invention utilizes the catalytic dehydration of p-methyl benzenesulfonic acid prevents nano-cellulose aerogel in pyrolytic process Contraction and aggregation, so that successfully carbon nano-fiber aeroge is prepared for raw material by timber first.
It is currently preferred, the heating schedule of the high temperature pyrolysis be 500 DEG C before heating rate be 2 DEG C/min, 500 DEG C It is 5 DEG C/min afterwards.
The liter warming middle-JIAO of the high temperature pyrolysis, keeps 1h at 500 DEG C.
The final pyrolysis temperature of the high temperature pyrolysis is 800 DEG C, and final temperature is kept for 1~2 hour.
The cooling process of the high temperature pyrolysis be 500 DEG C before rate of temperature fall be 5 DEG C/min, after 500 DEG C be Temperature fall.
The shielding gas of the high temperature pyrolysis is argon or nitrogen.
Compared with prior art, the invention provides a kind of method for preparing carbon nano-fiber aeroge by timber, including: A) timber is carried out into pre-treatment, obtains wood pulp;B) above-mentioned wood pulp is mixed with tetramethyl piperidine oxides, sodium bromide and sodium hypochlorite Close, carry out oxidation reaction, obtain cellulose suspension;C), after by above-mentioned cellulose suspension sucking filtration, it is dispersed in water, breaks up, Obtain homogeneous thick nano-cellulose solution;D) above-mentioned nano-cellulose solution is acidified under sour environment, is obtained To nanofiber hydrogel;E) above-mentioned nanofiber hydrogel is carried out into solvent friendship in the acetone containing p-methyl benzenesulfonic acid Change, using CO2Supercritical drying is dried, and obtains nano-cellulose aerogel;F) by the nano-cellulose aerogel Carbon nano-fiber aeroge is obtained in the pyrolysis of tube furnace high temperature.
The present invention is realized by raw material of common timber first and prepares carbon nano-fiber aerogel material, using containing Oxygen-derived free radicals reagent (TEMPO) is peeled off to cellulose, obtains cellulose nano-fibrous;Nanofiber is made under sour environment Plain solution forms hydrogel;Then nanofiber hydrogel is carried out after solvent displacement with the acetone soln containing p-methyl benzenesulfonic acid Supercritical drying obtains nano-cellulose aerogel;Nano-cellulose aerogel is pyrolyzed to obtain in tube furnace atmosphere of inert gases To final product carbon nano-fiber aeroge, and then there is provided a kind of new method for preparing carbon nano-fiber aerogel material. The carbon nano-fiber diameter for arriving is more homogeneous, in 5~10nm, less than 10nm.The carbon nano-fiber aeroge for obtaining has relatively low Density, test result indicate that, its density be 10~20mg/cm3, while specific surface area is larger, its BET specific surface area is 703.7389m2/g, possesses the characteristics such as good insulating refractory.
In addition, the preparation method of the carbon nano-fiber aeroge of present invention offer is simple, reproducible, raw material is In the timber that nature is widely present, therefore it is very easy to realize extensive preparation.
Description of the drawings
Fig. 1 is the transmission electron microscope photo of the nano-cellulose that the embodiment of the present invention 1 is provided;
Fig. 2 is the atomic force microscopy of the nano-cellulose that the embodiment of the present invention 1 is provided;
Fig. 3 is the digital photograph of the nanofiber hydrogel that the embodiment of the present invention 1 is provided;
Fig. 4 is the stereoscan photograph of the nano-cellulose aerogel that the embodiment of the present invention 2 is provided;
Fig. 5 is the stereoscan photograph of the carbon nano-fiber aeroge that the embodiment of the present invention 2 is provided;
Fig. 6 is the digital photograph of the cellulose nano-fibrous thin film that the embodiment of the present invention 2 is provided;
Fig. 7 is the transmission electron microscope photo of the carbon nano-fiber that the embodiment of the present invention 2 is provided.
Specific embodiment
In order to further illustrate the present invention, carbon nano-fiber is prepared by timber to what the present invention was provided with reference to embodiment The method of aeroge is described in detail.
In following embodiment, each raw material is and buys from the market.
Embodiment 1
Wood pulp (solid content 26.67%) after 3.75g is bleached is distributed in 100mL water, after stirring, and is added 0.016g, 0.1mmol tetramethyl piperidine oxides and 0.1g, 1mmol sodium bromide, adjust the secondary of 10ml9% using the hydrochloric acid of 1M Sodium chlorate solution is 10 to pH, the liquor natrii hypochloritises that pH is 10 is added in dispersion liquid, is persistently stirred, is detected molten using pH meter The pH changes of liquid, it is 10~10.3 that the sodium hydroxide of Deca 1M makes solution keep pH during the course of the reaction, after 4~10h of reaction, is taken out Filter, Jing after many deionized water rinsings is dispersed in the thick white shape material after sucking filtration in 100ml water.By the dispersion liquid for obtaining The mechanical treatment in blender, rotating speed about 37000/min, obtains nanofiber after supersound process after stirring in cell crushing instrument Plain solution.
To in nano-cellulose solution described in 20mL 0.6wt%, the hydrochloric acid of Deca 1M is 2 to pH, by receiving for now being formed Rice cellulose aquagel is placed in 12h in dilute hydrochloric acid solution, obtains firm nanofiber hydrogel.Hereafter, by nanofiber Hydrogel carries out solvent displacement in being placed on the acetone soln containing p-methyl benzenesulfonic acid, keep cellulose solid content and p-methyl benzenesulfonic acid Mass ratio be 10:1, solvent is changed twice for 24 hours, and solvent time swap is 3~4 days.By the nanometer after the replacement solvent Cellulose gel carries out carbon dioxide supercritical fluid drying and obtains nano-cellulose aerogel, and supercritical drying parameter setting is 50 ℃、9.0MPa。
The nano-cellulose aerogel for obtaining is placed in into the pyrolysis of tube furnace high temperature, temperature-rise period is with the speed of 2 DEG C/min Rate is warming up to 500 DEG C, after keeping 1h, then with the ramp of 5 DEG C/min to 800 DEG C, after keeping 1h, with the speed of 5 DEG C/min 500 DEG C are cooled to, 500 DEG C naturally cool to room temperature later.With nitrogen as the atmosphere gas being pyrolyzed in whole process.Final To carbon nano-fiber aeroge.
Transmission electron microscope observation is carried out to the nano-cellulose solution, as a result referring to Fig. 1.As shown in Figure 1, implement Nano-cellulose prepared by example 1 is fully peeled off, well it is dispersed in aqueous.Lower-left accompanying drawing is prepared for embodiment 1 Nano-cellulose solution digital photograph.
Atomic force microscope observation is carried out to the nano-cellulose solution, as a result referring to Fig. 2.As shown in Figure 2, embodiment 1 nano-cellulose for preparing fully is peeled off, well it is dispersed in aqueous, the result of Fig. 2 is mutual with the result of Fig. 1 Confirmation.
Fig. 3 is the firm cellulose nano-fibrous hydrogel, from the figure 3, it may be seen that the cellulose that embodiment 1 is prepared Nanofiber hydrogels are translucent.
Embodiment 2
Wood pulp (solid content 26.67%) after 3.75g is bleached is distributed in 100mL water, after stirring, and is added 0.016g, 0.1mmol tetramethyl piperidine oxides and 0.1g, 1mmol sodium bromide, adjust the secondary of 10ml 9% using the hydrochloric acid of 1M Sodium chlorate solution is 10 to pH, the liquor natrii hypochloritises that pH is 10 is added in dispersion liquid, is persistently stirred, is detected molten using pH meter The pH changes of liquid, it is 10~10.3 that the sodium hydroxide of Deca 1M makes solution keep pH during the course of the reaction, after 4~10h of reaction, is taken out Filter, Jing after many deionized water rinsings is dispersed in the thick white shape material after sucking filtration in 100ml water.By the dispersion liquid for obtaining The mechanical treatment in blender, rotating speed about 37000/min, obtains nanofiber after supersound process after stirring in cell crushing instrument Plain solution.
Take nano-cellulose solution described in 10ml 0.4wt% and cover full about 7cm glass culture dishs bottom so far, by glass Culture dish is placed in 1~2h in 80 DEG C of baking ovens, obtains nano-cellulose transparent membrane.
To in nano-cellulose solution described in 20mL 0.6wt%, the hydrochloric acid of Deca 1M is 2 to pH, by receiving for now being formed Rice cellulose aquagel is placed in 12h in dilute hydrochloric acid solution, obtains firm nanofiber hydrogel.Hereafter, by nanofiber Hydrogel carries out solvent displacement in being placed on the acetone soln containing p-methyl benzenesulfonic acid, keep cellulose solid content and p-methyl benzenesulfonic acid Mass ratio be 10:1, solvent is changed twice for 24 hours, and solvent time swap is 3~4 days.By the nanometer after the replacement solvent Cellulose gel carries out carbon dioxide supercritical fluid drying and obtains nano-cellulose aerogel, and supercritical drying parameter setting is 50 ℃、9.0MPa。
The nano-cellulose aerogel for obtaining is placed in into the pyrolysis of tube furnace high temperature, temperature-rise period is with the speed of 2 DEG C/min Rate is warming up to 500 DEG C, after keeping 1h, then with the ramp of 5 DEG C/min to 800 DEG C, after keeping 1h, with the speed of 5 DEG C/min 500 DEG C are cooled to, 500 DEG C naturally cool to room temperature later.With nitrogen as the atmosphere gas being pyrolyzed in whole process.Final To carbon nano-fiber aeroge.
A small amount of above-mentioned carbon nano-fiber aeroge is taken in 5ml centrifuge tubes, 4ml ethanol solution, supersound process 1~2 is added Hour obtains the carbon nano-fiber alcohol dispersion liquid of black, and the dispersion liquid is used to prepare transmission electron microscope sign sample Product.
Field emission scanning electron microscope observation is carried out to the nano-cellulose aerogel, as a result referring to Fig. 4, Fig. 4 is The stereoscan photograph of the nano-cellulose aerogel that the embodiment of the present invention 2 is provided, as shown in Figure 4, the present invention obtains Nanowire The diameter of dimension aeroge is more uniform, is 5nm or so.Digital photograph of the lower-left accompanying drawing for nano-cellulose aerogel.
Field emission scanning electron microscope observation is carried out to the carbon nano-fiber aeroge, as a result referring to Fig. 5, Fig. 5 is The stereoscan photograph of the carbon nano-fiber aeroge that the embodiment of the present invention 2 is provided, as shown in Figure 5, the present invention obtains carbon nanometer The diameter of fiber aeroge is more uniform, is 5nm or so.Digital photograph of the lower-left accompanying drawing for carbon nano-fiber aeroge.Fig. 5 with Fig. 4 contrasts understand, before and after pyrolytic process, the nanofiber in aeroge is not assembled, and has remained in that original nanometer Fiber aeroge state.
Fig. 6 is the digital photograph of the nano-cellulose transparent membrane that the embodiment of the present invention 2 is provided, it will be appreciated from fig. 6 that of the invention The nano-cellulose thin film prepared in embodiment 2 has the high grade of transparency.
Transmission electron microscope observation is carried out to the carbon nano-fiber alcohol dispersion liquid sample, as a result referring to Fig. 7, Fig. 7 The transmission electron microscope photo of the carbon nano-fiber alcohol dispersion liquid sample to provide in the embodiment of the present invention 2, as shown in Figure 7 Carbon nano-fiber prepared by the present invention is not mutually assembled, and diameter Distribution is uniform, is 5nm or so.Lower-left accompanying drawing is carbon Nanowire The digital photograph of dimension alcohol dispersion liquid.
From above-described embodiment, the present invention has successfully prepared carbon nano-fiber aeroge with timber as raw material.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that right For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out Some improvement and modification, these improve and modification is also fallen in the protection domain of the claims in the present invention.

Claims (10)

1. a kind of method that carbon nano-fiber aeroge is prepared by timber, it is characterised in that include:
A) timber is carried out into pre-treatment, obtains wood pulp;
B) above-mentioned wood pulp is mixed with tetramethyl piperidine oxides, sodium bromide and sodium hypochlorite, carries out oxidation reaction, obtain fiber Plain suspension;
C) after by above-mentioned cellulose suspension sucking filtration, it is dispersed in water, breaks up, obtains homogeneous thick nano-cellulose molten Liquid;
D) above-mentioned nano-cellulose solution is acidified under sour environment, is obtained nanofiber hydrogel;
E) above-mentioned nanofiber hydrogel is carried out into solvent exchange in the acetone containing p-methyl benzenesulfonic acid, using CO2Supercritical drying Dry method is dried, and obtains nano-cellulose aerogel;
F) nano-cellulose aerogel is obtained into carbon nano-fiber aeroge in the pyrolysis of tube furnace high temperature.
2. preparation method according to claim 1, it is characterised in that the pre-treatment of the step a) is specially:
Sodium hydroxide solution and acid sodium chlorite solution's multi-reflow.
3. preparation method according to claim 1, it is characterised in that the solid content of the wood pulp, tetramethyl piperidine oxidation The mass volume ratio of thing, sodium bromide and liquor natrii hypochloritises is (1g):(0.01~0.03g):(0.05~0.2g):(5~ 15mL), the mass content of the liquor natrii hypochloritises is 5wt%~15wt%.
4. preparation method according to claim 1, it is characterised in that described breaing up is to use blender, and rotating speed is 37000 ~50000 turns/min.
5. preparation method according to claim 1, it is characterised in that the pH value of the sour environment is 2~3.
6. preparation method according to claim 1, it is characterised in that the nanofiber hydrogel solid content and to first The mass ratio of benzenesulfonic acid is 5~15:1.
7. preparation method according to claim 1, it is characterised in that the CO2The temperature of supercritical drying sample room is 40 DEG C~50 DEG C, pressure is 9.0MPa.
8. preparation method according to claim 1, it is characterised in that the heating schedule of the high temperature pyrolysis be 500 DEG C it Front heating rate is 2 DEG C/min, is 5 DEG C/min after 500 DEG C;The cooling process of the high temperature pyrolysis is 500 DEG C of speed of lowering the temperature before Rate is 5 DEG C/min, is Temperature fall after 500 DEG C.
9. preparation method according to claim 1, it is characterised in that the liter warming middle-JIAO of the high temperature pyrolysis, keeps at 500 DEG C 1h。
10. preparation method according to claim 1, it is characterised in that the final pyrolysis temperature of the high temperature pyrolysis is 800 DEG C~1200 DEG C, final temperature is kept for 2 hours.
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CN110330944A (en) * 2019-07-02 2019-10-15 同济大学 Derivative composite phase change energy-storing conductive material of natural timber and preparation method thereof
CN111180217A (en) * 2020-01-16 2020-05-19 西安工业大学 Organic domestic garbage derived carbon aerogel composite electrode material and preparation method thereof
CN111229136A (en) * 2018-11-29 2020-06-05 昆山科技大学 Method for detecting gas by using carbon aerogel adsorption material
CN111440353A (en) * 2020-04-26 2020-07-24 云南中烟工业有限责任公司 Preparation method of heat-conducting hydrophobic flame-retardant nano-cellulose aerogel
CN112110435A (en) * 2020-08-24 2020-12-22 宁波工程学院 Preparation method of bacterial cellulose-based carbon aerogel
CN112142034A (en) * 2020-09-27 2020-12-29 武汉理工大学 Preparation method of sulfur/carbon aerogel composite material
CN112662015A (en) * 2020-12-24 2021-04-16 中国科学技术大学 Flame-retardant nano-cellulose composite aerogel with oriented structure and preparation method thereof
CN113860312A (en) * 2021-10-28 2021-12-31 中国科学技术大学 Preparation method of anisotropic high-temperature-resistant silicon carbide aerogel heat insulation material
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