CN105502346A - Carbon aerogel prepared from chitin aerogel and preparation method thereof - Google Patents
Carbon aerogel prepared from chitin aerogel and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses carbon aerogel prepared from chitin aerogel. Chitin nano-fiber aerogel is prepared by means of a mechanical method or a chemical oxidation method, and then the carbon aerogel is obtained through a method for carbonization under the inert gas shielding. The preparation method is simple, the technology is easy to control, the adopted oxidizing agent is the environment-friendly green solvent and is safe and free of toxicity, the green preparation technology is achieved, the cost is lowered, the obtained carbon aerogel is free of toxicity, the 3D network structure is obtained, the surface area is large, the porosity is high, and the certain mechanical strength is achieved.
Description
Technical field
The present invention relates to carbon aerogels, be specifically related to a kind of carbon aerogels utilizing chitin aerogel to prepare and preparation method thereof.
Background technology
Aerogel is generally be raw material by Resorcinol and formaldehyde, Resorcinol and formaldehyde, Phloroglucinol and formaldehyde, trimeric cyanamide and formaldehyde, mixture cresol and formaldehyde, phenol and furfural, the skeleton structure prepared by sol-gel and supercritical drying etc. and pore texture are all at the solid material of below 100nm, but this method raw material used is petroleum chemicals, with high costs, and huge pollution is caused to environment.Biomass chitin aerogel is then that cheaper starting materials is easy to get and decreases environmental pollution with the dried small shrimp crab shell of industrial waste for raw material.Chitin aerogel is a kind of Performances of Novel Nano-Porous meter level porous solid material with three-dimensional net structure, have low density, high-ratio surface sum high porosity, due to these characteristics, biomass chitin aerogel can be used as support of the catalyst, sorbent material etc., can be widely used in ultracapacitor, rechargeable cell and electrode materials, thus biomass chitin aerogel is the good precursor of carbon aerogels.
Carbon aerogels is a kind of carbon material prepared in phase late 1980s, and it is a kind of novel lightweight nanometer porous property cellulosic material.Carbon aerogels is obtained through high temperature cabonization by aerogel, maintains the contiguous network structure of aerogel.In carbonization process, the pyrolysis fracture of functional group does not destroy original network structure, but defines abundant pore texture (porosity (85 ~ 99%) and high specific surface area (500 ~ 2000m
2/ g), and carbon aerogels also has good conductivity (J.Sol-GelSci.Technol., 2004,31:1-5.).These performances of carbon aerogels make it can be widely used in the fields such as the energy, electronics, environmental protection, medicine and space science research.But the preparation technology of the carbon aerogels of general biological material is also immature, not only specific surface area is low, porosity is single but also electroconductibility is also poor for the carbon aerogels manufacturing out, limits the widespread use of carbon aerogels to a certain extent.
Existing method is all generally utilize Resorcinol and formaldehyde, Resorcinol and formaldehyde, Phloroglucinol and formaldehyde, trimeric cyanamide and formaldehyde, mixture cresol and formaldehyde, phenol and furfural to prepare aerogel, there is carbon aerogels porosity low, the problems such as specific surface is low.A kind of preparation method of carbon aerogels is disclosed in patent document " carbon aerogels, Its Preparation Method And Use " (CN101910058A), but the carbon aerogels source prepared by the method does not relate to natural biomass materials, particularly chitin raw material.
Summary of the invention
The object of the invention is to solve the existing carbon aerogels hole utilizing petrochemical materials to prepare to obtain in carbon aerogels process single, specific surface is low to be waited not enough, provides a kind of carbon aerogels utilizing chitin aerogel to prepare and preparation method thereof.
A kind of method utilizing chitin aerogel to prepare carbon aerogels provided by the invention; it is characterized in that the method first processes chitin by the method for mechanical process or chemical oxidation; then obtain chitin fiber aerogel through super-dry, finally under protection of inert gas, charing can obtain carbon aerogels.Preparation process of the present invention is simple, and technology controlling and process is easy, and oxygenant used belongs to environment-friendly solvent, safety non-toxic, realize green preparation process, again reduce cost, and prepared carbon aerogels is nontoxic, 3D network structure, high-ratio surface, porosity is high and have certain mechanical strength.The carbon aerogels material of preparation is in absorption, photochemical catalysis, lithium electricity, the super aspect such as electric can extensively utilize, the cheap Biological resources of this preparation method's efficiency utilization simultaneously, prepared the carbon aerogels of structure excellence by chitin nano fiber, improve its use value, also provide new thinking and countermeasure for efficiency utilization chitin aerogel resource.
Technical scheme of the present invention is:
Utilize a carbon aerogels prepared by chitin aerogel, method that chitin nano fiber aerogel carbonizes then under protection of inert gas is made to utilize the method for mechanical process or chemical oxidation to prepare.
Utilize a carbon aerogels prepared by chitin aerogel, realized by following steps:
(1) dried small shrimp, crab shell are utilized chemical extracting removes lipid, acid treatment removes inorganic salt,
The method of the impurity such as alkaline purification deproteinize carries out purifying;
(2) dried small shrimp after purifying, crab shell are by the method preparation 1wt% dispersion liquid of mill;
(3) above-mentioned scattered dispersion liquid is added phosphoric acid salt or acetate buffer solution, 300 ~ 1000rpm on magnetic stirring apparatus, normal temperature and pressure stirs 5 ~ 30min;
(4) dispersion liquid that step (2) obtains directly is added TEMPO and NaBr, after being uniformly dispersed, add NaClO, the mol ratio of TEMPO:NaBr:NaClO is 1:10:20 ~ 50, react under stirring, utilize the NaOH of 0.1 ~ 5mol/L to control the pH of dispersion liquid 10 ~ 11, reaction 1 ~ 12h, add ethanol termination reaction, ethanol: the mol ratio of NaClO is 1:10 ~ 500; Or the dispersion liquid that step (3) obtains is added TEMPO and NaClO, after being uniformly dispersed, add NaClO
2, TEMPO:NaClO:NaClO
2mol ratio be 1:10 ~ 50:100, react under stirring, by container closure heat, finally add ethanol termination reaction, ethanol: the mol ratio of NaClO is ethanol: NaClO
2=1:100 ~ 1000;
(5) repeatedly rinse the dispersion liquid deionized water that step (4) obtains to neutrality, carry out nanofiber process 10 ~ 180min, then by centrifugal treating, rotating speed is: 1000 ~ 10000rpm, and 5 ~ 10min gets supernatant liquor; Or by treatment on ion exchange columns, flow out with 0.1 ~ 5mL/s;
(6) with higher alcohols, the hydrogel after process is replaced, obtain chitin fiber alcogel, by the alcogel obtained, after drying, namely obtain chitin aerogel;
(7) by chitin nano fiber aerogel in tube furnace under protection of inert gas 400 ~ 1300 DEG C, insulation 1 ~ 3h, then lowers the temperature, can obtain carbon aerogels; Or chitin nano fiber aerogel is warmed up to 200 ~ 400 DEG C of insulation 60 ~ 120min in tube furnace under air condition, then under protection of inert gas, be warmed up to 400 ~ 1200 DEG C of insulation 1 ~ 5h, then lower the temperature, can carbon aerogels be obtained.
Preferably, the mill in described step (2) refers to and includes but not limited to mechanical mill, high-pressure homogeneous, mechanical glue mill, defibrator process, mill process; After being disposed, deposit at being placed in 4 DEG C.
Preferably, described step (3), in add phosphate buffer soln after, adjust pH be 6 ~ 8; After adding acetate buffer solution, regulate pH to be 3 ~ 5, add carbonate buffer solution, adjust pH to be 6 ~ 8.
Preferably, dispersion liquid is heated to 60 ~ 80 DEG C in (4) by described step, under mechanical stirring state, reaction times t is 60 ~ 180min, the volume ratio adding dispersion liquid in dehydrated alcohol and step (4) is 0.1 ~ 2:10, can obtain chitin nano fiber dispersion liquid.
Preferably, the nanofiber process described in described step (5) includes but not limited to ultrasonic grinding, high speed shear process, the process of rubber mill tool, mechanical mill.
Preferably, the critical point drying of drying mode to be drying medium be carbonic acid gas, supercritical drying, vacuum-drying, lyophilize in described step (6).
Preferably, the higher alcohols described in described step (6) includes but not limited to the trimethyl carbinol, propyl carbinol, ethylene glycol, glycerol, hexalin.
Preferably, described step (7) rare gas element is nitrogen or argon gas or helium or neon or carbonic acid gas or nitrogen is argon-mixed or nitrogen and hydrogen mixture or argon hydrogen gas mixture.
Preferably, by chitin nano fiber aerogel in tube furnace under protection of inert gas 400 ~ 1300 DEG C in described step (7), control heat-up rate 2 DEG C/min ~ 10 DEG C/min, insulation 1 ~ 3h, then with the cooling of 10 DEG C/min speed, carbon aerogels can be obtained; ; Or under air condition; control heat-up rate 2 DEG C/min ~ 10 DEG C/min; by room temperature to 200 DEG C ~ 350 DEG C; then insulation 60 ~ 120min is carried out; subsequently under protection of inert gas, control heat-up rate 5 DEG C/min ~ 10 DEG C/min, be warmed up to 600 ~ 1200 DEG C; insulation 1h ~ 3h, then lowers the temperature with 10 DEG C/min speed.
The present invention has the following advantages:
1, the TEMPO used due to the present invention belongs to environment-friendly solvent, and security is high, thus both can not produce toxicity to the carbon aerogels of preparation, also can not bring corrosion to plant and instrument, bring pollution to environment.
2, the raw material used due to the present invention is mainly the tankage such as the dried small shrimp crab shell of industrial waste, not only cheap and easy to getly also reduces environmental pollution.
3, due to the core drying that the present invention uses, carbonization device is simply common, does not need to add expensive device.And the higher alcohols displacement liquid fusing point used is lower, does not even need separately to add refrigerating apparatus, therefore tests green preparation process by low cost.
4, the higher alcohols of the present invention, solves the gel network structure caused due to capillary existence and the problem such as to cave in, make the carbon aerogels of acquisition have meticulous homogeneous structure.
5, the carbon aerogels prepared by the present invention not only has 3D network, high-specific surface area and have green non-poisonous advantage, and raw material is also cheap and easy to get simultaneously.
6, preparation process of the present invention is simply controlled.
7, the carbon aerogels prepared of the present invention is of many uses, and can be used for ultracapacitor, the specific demand such as biological medicine and aeronautical material, belongs to high value added product.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the carbon aerogels that specific embodiment 1 obtains;
Fig. 2 is the XRD figure of the carbon aerogels that specific embodiment 2 obtains;
Fig. 3 is the N of the carbon aerogels that specific embodiment 2 obtains
2adsorption/desorption curve;
Fig. 4 is the FTIR figure of the carbon aerogels that specific embodiment 3 obtains;
Fig. 5 is the Raman figure of the carbon aerogels that specific embodiment 4 obtains.
Embodiment
Following examples only for illustration of the present invention, but are not used for limiting invention scope of the present invention.The technician of this technical field can make improvement and the adjustment of some non-intrinsically safes according to the content of foregoing invention.
Embodiment 1:
1. rinsed well by discarded shrimp shell, crushed after being dried crosses 80 eye mesh screens, obtains powdered biomass;
2. get the dried small shrimp after 1g pulverizing, first utilize sherwood oil ethanol by 2:1 extracting, remove some organism, the method for the impurity such as KOH process deproteinize carries out purifying to dried small shrimp, adds 1wt%NaClO under then utilizing Glacial acetic acid to regulate pH=4.5 condition
2in 75 DEG C of heating 2h bleaching;
3. the dried small shrimp after bleaching is formulated as 1wt% dispersion liquid, obtains the thick chitin dispersion liquid of 1wt% by the method for mechanical mill;
4. phosphate buffer soln is added above-mentioned dispersion liquid, regulate dispersion liquid pH=7,500rpm on magnetic stirring apparatus, normal temperature and pressure stirs 10min, and chitin is better disperseed;
5. add TEMPO and NaClO after, be uniformly dispersed and add NaClO again
2, TEMPO:NaClO:NaClO
2mol ratio is 1:10:100, rapidly container closure is heated to 70 DEG C of reaction 2h, adds 10mL ethanol termination reaction after reaction terminates;
6. the dispersion liquid deionized water obtained is rinsed repeatedly to neutrality, then use ultrasonic grinder (1500W) ultrasonic 2h, obtain the uniform dispersion liquid of chitin;
7. the chitin dispersion liquid obtained is carried out centrifugal treating, rotating speed is 8000rpm, and the treatment time is 3min, gets supernatant liquid, can obtain hydrogel;
8. pair hydrogel trimethyl carbinol obtained above carries out displacement and obtains chitin alcogel, by the alcogel that obtains at-80 DEG C of freezing 1h, namely obtains chitin aerogel after lyophilize;
9. by chitin aerogel at tube furnace N
2be heated to 800 DEG C of insulation 2h with 5 DEG C/min under protection, then lower the temperature rapidly with 10 DEG C/min and can obtain the good carbon aerogels of pattern.
Embodiment 2:
1, rinse well at the crab shell of industrial waste, dry, pulverize 80 eye mesh screens, obtain crab shell powder; Get the crab shell powder after 1g pulverizing, first utilize benzene: ethanol, by 2:1 extracting, removes some organism, the method for the impurity such as recycling NaOH process deproteinize carries out purifying to crab shell, adds 1wt%NaClO under then utilizing Glacial acetic acid to regulate pH=4.5 condition
2in 75 DEG C of heating 2h bleaching, then washing is to neutral, is configured to the solution of 1wt%, deposits at 4 DEG C;
2. get the above-mentioned dispersion liquid of 400mL, after stirring, add the phosphate buffer soln of 300mLpH=6.8, regulate dispersion liquid pH to be 6.8 ± 0.2.
3. add TEMPO and NaClO after, be uniformly dispersed and add NaClO again
2, TEMPO:NaClO:NaClO
2mol ratio is 1:10:100, rapidly container closure is heated to 80 DEG C of reaction 3h, adds 20mL ethanol termination reaction after reaction terminates;
4. repeatedly rinse the dispersion liquid deionized water obtained to neutrality, then mechanical mill obtains the chitin nano fiber dispersion liquid of diameter Distribution at 15 ~ 100nm;
5. the chitin dispersion liquid obtained is carried out centrifugal treating, rotating speed is 5000rpm, and the treatment time is 5min, gets supernatant liquid, can obtain hydrogel;
6. pair hydrogel trimethyl carbinol obtained is replaced, and by the alcogel that obtains at-20 DEG C of freezing 4h, namely obtains chitin aerogel after lyophilize;
7. chitin aerogel is placed in tube furnace and is heated to 250 DEG C with 5 DEG C/min, insulation 120min, then at Ar
2be heated to 800 DEG C of insulation 1.5h with 10 DEG C/min under protection, lower the temperature rapidly with 10 DEG C/min subsequently and can obtain the good carbon aerogels of pattern.
Embodiment 3:
1. by the dried small shrimp of industrial waste, pulverize 80 eye mesh screens, obtain dried small shrimp powder;
2. get the dried small shrimp powder after 1g pulverizing, first utilize phenylethyl alcohol by 2:1 extracting, remove some organism, the method for the impurity such as recycling NaOH process deproteinize carries out purifying to dried small shrimp, adds 1.5wt%NaClO under then utilizing Glacial acetic acid to regulate pH=4 condition
2in 80 DEG C of heating 1.5h bleaching, then washing is to neutral, is configured to the solution of 1wt%, deposits 4 DEG C of preservations;
3. get the above-mentioned dispersion liquid of 400mL, directly TEMPO and NaBr is added after stirring, after being uniformly dispersed, add NaClO, the mol ratio of TEMPO:NaBr:NaClO is 1:10:30, reacts under stirring, utilizes 0.1 ~ 5mol/LNaOH to control the pH of dispersion liquid 10 ± 0.2, reaction 3h, adds 20mL ethanol termination reaction;
4. the dispersion liquid deionized water obtained is rinsed repeatedly to neutrality, then use ultrasonic grinder (1500W) by ultrasonic for this dispersion liquid 1.5h;
5. couple dispersion liquid 5000rpm obtained, centrifugal 10min, gets supernatant liquid;
6. pair this dispersion liquid trimethyl carbinol is replaced, and by the alcogel that obtains at-20 DEG C of freezing 4h, namely obtains chitin aerogel after lyophilize;
7. by chitin aerogel at tube furnace at Ar
2be heated to 800 DEG C of insulation 1.5h with 10 DEG C/min under protection, then lower the temperature rapidly with 10 DEG C/min and can obtain the good carbon aerogels of pattern.
Embodiment 4:
1. rinsed well by discarded shrimp shell, crushed after being dried crosses 80 eye mesh screens, obtains dried small shrimp powder;
2. get dried small shrimp powder obtained above to add alkali lye and process, de-Partial Protein, then adds process in hydrochloric acid and sloughs mineral salt, finally join in benzene, ethanol or acetone and process, slough pigment, lipid material, filter the dried small shrimp powder obtaining depigmentation, fat, mineral salt and albumen;
3. shrimp shell meal end obtained above is configured to the dried small shrimp dispersion liquid of 1wt% by mechanical mill
4. get above-mentioned dispersion liquid 400mL, directly add TEMPO and NaBr, after being uniformly dispersed, add NaClO, the mol ratio of TEMPO:NaBr:NaClO is 1:10:40, reacts under stirring, utilizes the NaOH of 2mol/L to control the pH=10.5 of dispersion liquid, reaction 3h, adds 20mL ethanol termination reaction;
5. obtain dispersion liquid washing to neutral by above-mentioned, then carry out nanometer fibrillation process by ultrasonic grinder, the power 1200W of ultrasonic fibrillation process, the time of nanometer fibrillation process is 30min, obtains nanofibrils dispersion liquid;
6. the chitin nanofibrils dispersion liquid obtained is carried out centrifugal treating, get supernatant liquor;
7. pair dispersion liquid obtained above utilizes the trimethyl carbinol to replace, and obtains alcogel, by the alcogel that obtains at-80 DEG C of freezing 1h, namely obtains chitin aerogel after lyophilize;
8. by chitin nanoporous aerogel at tube furnace at Ar
2be heated to 800 DEG C of insulation 2h with 10 DEG C/min under protection, lower the temperature rapidly with 10 DEG C/min subsequently and can obtain the good carbon aerogels of pattern.
Embodiment 5:
1. rinsed well by discarded crab shell, crushed after being dried crosses 80 eye mesh screens, obtains crab shell powder;
2. get crab shell powder obtained above to add alkali lye and process, de-Partial Protein, then adds process in hydrochloric acid and sloughs mineral salt, finally join in benzene, ethanol or acetone and process, slough pigment, lipid material, filter the crab shell powder obtaining depigmentation, fat, mineral salt and albumen;
3. the crab shell powder obtained is configured to the dispersion liquid of 1wt% by mechanical mill, is placed in 4 DEG C of preservations;
4. get above-mentioned dispersion liquid 200mL, directly add TEMPO and NaBr, after being uniformly dispersed, add NaClO, the mol ratio of TEMPO:NaBr:NaClO is 1:10:35, reacts under stirring, utilizes the NaOH of 0.5mol/L to control the pH=10.5 of dispersion liquid, reaction 2h, adds 10mL ethanol termination reaction;
5., by extremely neutral for above-mentioned dispersion liquid washing, by rubber mill process, carry out nanometer fibrillation process, process uses power to be 2500W, and the time of process is 10min, obtains nanofibrils dispersion liquid;
6. the dispersion liquid obtained is carried out centrifugal treating, get supernatant liquor, then with trimethyl carbinol displacement, obtain chitin alcosol;
7. by the alcosol that obtains-80 DEG C of freezing 1h, then lyophilizes, obtain chitin aerogel;
8. chitin aerogel is heated to 250 DEG C with 2 DEG C/min in tube furnace air, insulation 120min, then at Ar
2be heated to 1000 DEG C of insulation 1h with 10 DEG C/min under protection then to lower the temperature rapidly with 10 DEG C/min and can obtain the good carbon aerogels of pattern.
Claims (10)
1. the carbon aerogels utilizing chitin aerogel to prepare, method that chitin nano fiber aerogel carbonizes then under protection of inert gas is made to it is characterized in that utilizing the method for mechanical process or chemical oxidation to prepare.
2. the preparation method of carbon aerogels as claimed in claim 1, is characterized in that being realized by following steps:
(1) method of the impurity such as chemical extracting removes lipid, acid treatment removes inorganic salt, alkaline purification deproteinize is utilized to carry out purifying on dried small shrimp, crab shell;
(2) dried small shrimp after purifying, crab shell are by the method preparation 1wt% dispersion liquid of mill;
(3) above-mentioned scattered dispersion liquid is added phosphoric acid salt or acetate buffer solution, 300 ~ 1000rpm on magnetic stirring apparatus, normal temperature and pressure stirs 5-30min;
(4) dispersion liquid that step (2) obtains directly is added TEMPO and NaBr, after being uniformly dispersed, add NaClO, the mol ratio of TEMPO:NaBr:NaClO is 1:10:20 ~ 50, react under stirring, utilize the NaOH of 0.1 ~ 5mol/L to control the pH of dispersion liquid 10 ~ 11, reaction 1 ~ 12h, add ethanol termination reaction, ethanol: the mol ratio of NaClO is 1:10 ~ 500; Or the dispersion liquid that step (3) obtains is added TEMPO and NaClO, after being uniformly dispersed, add NaClO
2, TEMPO:NaClO:NaClO
2mol ratio be 1:10 ~ 50:100, react under stirring, by container closure heat, finally add ethanol termination reaction, ethanol: the mol ratio of NaClO is ethanol: NaClO
2=1:100 ~ 1000;
(5) repeatedly rinse the dispersion liquid deionized water that step (4) obtains to neutrality, carry out nanofiber process 10 ~ 180min, then by centrifugal treating, rotating speed is: 1000 ~ 10000rpm, and 5 ~ 10min gets supernatant liquor; Or by treatment on ion exchange columns, flow out with 0.1 ~ 5mL/s;
(6) with higher alcohols, the hydrogel after process is replaced, obtain chitin fiber alcogel, namely obtain chitin aerogel by after the alcogel drying obtained;
(7) by chitin nano fiber aerogel in tube furnace under protection of inert gas 400 ~ 1300 DEG C, insulation 1 ~ 3h, then lowers the temperature, can obtain carbon aerogels; Or chitin nano fiber aerogel is warmed up to 200 ~ 400 DEG C of insulation 60 ~ 120min in tube furnace under air condition, then under protection of inert gas, be warmed up to 400 ~ 1200 DEG C of insulation 1 ~ 5h, then lower the temperature, can carbon aerogels be obtained.
3. preparation method according to claim 2, the mill that it is characterized in that in step (2) refers to and includes but not limited to mechanical mill, high-pressure homogeneous, mechanical glue mill, defibrator process, mill process; After being disposed, deposit at being placed in 4 DEG C.
4. preparation method according to claim 2, after it is characterized in that adding phosphate buffer soln in step (3), adjusts pH to be 6 ~ 8; After adding acetate buffer solution, regulate pH to be 3 ~ 5, add carbonate buffer solution, adjust pH to be 6 ~ 8.
5. preparation method according to claim 2, it is characterized in that, in step (4), dispersion liquid is heated to 60 ~ 80 DEG C, under mechanical stirring state, reaction times is 60 ~ 180min, the volume ratio adding dispersion liquid in dehydrated alcohol and step (4) is 0.1 ~ 2:10, can obtain chitin nano fiber dispersion liquid.
6., according to preparation method according to claim 2, it is characterized in that the nanofiber process described in step (5) includes but not limited to ultrasonic grinding, high speed shear process, the process of rubber mill tool, mechanical mill.
7. preparation method according to claim 2, is characterized in that drying mode in step (6) to be vacuum-drying, lyophilize and drying medium is the critical point drying/supercritical drying of carbonic acid gas.
8. preparation method according to claim 2, is characterized in that the higher alcohols described in step (6) includes but not limited to the trimethyl carbinol, propyl carbinol, ethylene glycol, glycerol, hexalin.
9., according to the arbitrary described preparation method of claim 2 to 9, it is characterized in that step (7) rare gas element is nitrogen or argon gas or helium or neon or carbonic acid gas or nitrogen is argon-mixed or nitrogen and hydrogen mixture or argon hydrogen gas mixture.
10. preparation method according to claim 9, be characterised in that in step (7) and chitin nano fiber aerogel is placed in tube furnace, 400 ~ 1300 DEG C are warmed up under protection of inert gas, control heat-up rate 2 DEG C/min ~ 10 DEG C/min, insulation 1 ~ 3h, then with the cooling of 10 DEG C/min speed, carbon aerogels can be obtained; Or under air condition; control heat-up rate 2 DEG C/min ~ 10 DEG C/min; by room temperature to 200 DEG C ~ 350 DEG C; insulation 60 ~ 120min; subsequently under protection of inert gas, control heat-up rate 5 DEG C/min ~ 10 DEG C/min, be warmed up to 600 ~ 1200 DEG C; insulation 1h ~ 3h, then lowers the temperature with 10 DEG C/min speed.
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| CN110368977A (en) * | 2019-07-25 | 2019-10-25 | 广西科学院 | The preparation method and application of a kind of calcium and magnesium double activity center catalyst |
| CN112661154A (en) * | 2020-12-11 | 2021-04-16 | 河北工业大学 | Preparation method of graphene-containing high-adsorbability plant protein carbon aerogel |
| CN113087959A (en) * | 2021-05-18 | 2021-07-09 | 北华大学 | Preparation method of crop straw full-component aerogel, product and application thereof |
| CN114524674A (en) * | 2022-03-01 | 2022-05-24 | 中国科学院金属研究所 | Heat-proof, heat-insulation and load-bearing integrated light carbon-ceramic composite material and preparation method thereof |
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| CN106057485A (en) * | 2016-08-19 | 2016-10-26 | 南京林业大学 | Method for preparing super capacitor aerogel electrode material |
| CN108630344A (en) * | 2018-03-29 | 2018-10-09 | 浙江工业大学之江学院 | A kind of tensile wear-resistant carbon fiber cable |
| CN108298519A (en) * | 2018-03-30 | 2018-07-20 | 胡果青 | A kind of preparation method using the enhanced charcoal-aero gel of Ludox |
| CN110368977A (en) * | 2019-07-25 | 2019-10-25 | 广西科学院 | The preparation method and application of a kind of calcium and magnesium double activity center catalyst |
| CN110368977B (en) * | 2019-07-25 | 2022-04-19 | 广西科学院 | Preparation method and application of calcium-magnesium double-active-center catalyst |
| CN112661154A (en) * | 2020-12-11 | 2021-04-16 | 河北工业大学 | Preparation method of graphene-containing high-adsorbability plant protein carbon aerogel |
| CN112661154B (en) * | 2020-12-11 | 2023-03-10 | 河北工业大学 | Preparation method of graphene-containing high-adsorbability plant protein carbon aerogel |
| CN113087959A (en) * | 2021-05-18 | 2021-07-09 | 北华大学 | Preparation method of crop straw full-component aerogel, product and application thereof |
| CN114524674A (en) * | 2022-03-01 | 2022-05-24 | 中国科学院金属研究所 | Heat-proof, heat-insulation and load-bearing integrated light carbon-ceramic composite material and preparation method thereof |
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