CN102092708B - Method for preparing phenol-formaldehyde carbon aerogel in low alkali - Google Patents
Method for preparing phenol-formaldehyde carbon aerogel in low alkali Download PDFInfo
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Abstract
The invention relates to a method for preparing phenol-formaldehyde carbon aerogel in low alkali, belonging to the field of aerogel preparation. The method comprises the following steps of: by using phenol and formaldehyde as reactive monomers, resorcin as an auxiliary monomer and a nucleating agent, strong alkali as a catalyst and water as a solvent, aging after heating gelatin at the temperature between 70 DEG C and 100 DEG C to obtain an organic wet gel; carrying out organic solvent displacement on the organic wet gel so that the organic solvent is filled with gel; carrying out supercritical drying on the organic wet gel after displacement to obtain organic aerogel; and carbonizing the organic aerogel in an inert atmosphere to obtain the required carbon aerogel. The carbon aerogel prepared by the invention comprises a great deal of mesopores, micropores and some macropores; the specific surface of BET reaches up to 680 sq.m./g; the pore volume reaches up to 1.042 cu.cm./g; the material cost is low; the gel can be obtained after reaction in the catalytic concentration of low alkali; the method has important meanings for the research of phenol-formaldehyde carbon aerogel, and simultaneously has important promoter action for scale industrial production.
Description
Technical field
The present invention relates to the technique of preparation low density P-F charcoal-aero gel under a kind of low base catalyst concentration.
Background technology
Because the 3 D stereo network structure of charcoal-aero gel uniqueness, a large amount of mesopore, high specific surface area and the good characteristics such as electrical property, be considered in preparation electrode of super capacitor, support of the catalyst, there is potential application in the fields such as electro-adsorption material, hydrogen storage material, have huge market outlook.Therefore, since the end of the eighties in last century, Pekala etc. have prepared since the charcoal-aero gel first, and preparation and the applied research of relevant charcoal-aero gel both at home and abroad causes people's concern continuously.Thereby how the correlative study group of the states such as the present U.S., Japan, Germany will reduce the cost of charcoal-aero gel and strengthen this problem pendulum of its market competitiveness in extremely important position, the units such as Shanxi coalification institute of the domestic Chinese Academy of Sciences, Zhongshan University, East China University of Science, Beijing University of Chemical Technology, Dalian University of Technology have also carried out this research on the one hand successively, and make some progress and achievement.
Traditional charcoal-aero gel preparation process needs experience: the process that Resorcinol and formalin colloidal sol-organic water gel-organic solvent exchange-supercritical drying-organic aerogel-charing-charcoal-aero gel is such, preparation cycle is long, supercritical drying process complexity also has certain danger, and stock yard dihydroxy-benzene price is relatively high, causes the market competitiveness of the charcoal-aero gel of gained greatly to reduce.Therefore; consider from technical process and material choice; adopting more on the technique, the drying mode of simple economy replaces supercritical drying; and adopt phenol the most cheap in the phenols to replace the relatively high Resorcinol of price as raw material on the raw material; thereby reduction cost; strengthen the market competitiveness of charcoal-aero gel, impel its early mass-producing and suitability for industrialized production.
At present, many improvement have been made in the preparation technology of charcoal-aero gel by the unit such as Zhongshan University, East China University of Science, adopt the constant pressure and dry (be us common drying mode) of cheap and simple to replace the supercritical drying of complex and expensive, thereby reduced largely its cost, but the Resorcinol that its raw material uses has then restricted the further reduction of charcoal-aero gel cost largely; The units such as Dalian University of Technology replace expensive Resorcinol with comparatively cheap meta-cresol, have also reduced to a certain extent the cost of charcoal-aero gel; But because the price of phenol is the cheapest, so the first-selection of cost charcoal-aero gel raw material.Adopting phenol is the low activity problem of the relative Resorcinol of phenol as the greatest problem of raw material, this is owing to the cloud density of phenyl ring on the phenol is low than Resorcinol, be unfavorable for the substitution reaction with formaldehyde, for addressing this problem, according to document (Dingcai Wu, Ruowen Fu, Low-density organic and carbon aerogelsfrom the sol-gel polymerization of phenol with formaldehy, Journal ofnon-crystalline solids 2005,351:915-921) report, the units such as Zhongshan University adopt the highly basic (mol ratio P/C≤10.5) of higher concentration as catalyzer, making phenol conversion is the phenol negative oxygen ion, thereby the cloud density on the increase phenyl ring, improve reactive behavior, but this method need to be used a large amount of alkali, is unfavorable for protection of the environment, equipment during to scale operation has very large corrosion, does not also meet this concept of Green Chemistry of present promotion; Report according to Chinese patent (CN 1923679A), it is that reaction monomers is at aqueous phase that the units such as East China University of Science adopt the mixture of phenol, formaldehyde, nitrogen-containing aromatic compound and alkyl substituted phenol, after highly basic adjusting ph value of aqueous phase is 8～11, make charcoal-aero gel through sol-gel method, but because nitrogen-containing aromatic compound in the monomer whose, therefore contain a certain amount of nitrogen element in the charcoal-aero gel that makes, this application for some aspect is disadvantageous.
In sum, no matter the existing charcoal-aero gel (P-F system etc.) that adopts the sol-gel method preparation is the performance at product, or in that all having aspect the commercial finished product must improved place.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology hanging down synthesizing phenol-formaldehyde charcoal-aero gel under the base catalyst concentration.
For achieving the above object, the present invention is with phenol and formaldehyde (formalin, 37～40wt%) is reaction monomers, diphenol is for helping monomer and nucleator between benzene, highly basic is catalyzer, water is solvent, after heating 1～24 hour gel between 70 ℃ to 100 ℃, between 60 ℃ to 100 ℃ aging 1～5 day organic wet gel; Place organic solvent to carry out solvent exchange 2～5 days the organic wet gel that obtains, make organic solvent be full of gel; Then, adopt the method for supercritical drying that organic wet gel drying was got organic aerogel in 1～10 hour; With this organic aerogel in inert atmosphere between 500～1200 ℃ charing 1～5 hour required charcoal-aero gel; Used each material mixture ratio is: the mol ratio P/F of phenol and formaldehyde is 0.2～1; The mol ratio P/R of phenol and Resorcinol is 2～20; The mol ratio P/C of phenol and highly basic is 2～100; Reactant total concn PFR% is 10～60wt%.
The specific embodiment of the inventive method is:
(1). phenol, formaldehyde, Resorcinol, highly basic and water are mixed and stir according to predetermined formulation, afterwards in the reaction cartridge bottle and sealing, obtain gel in heating (being generally 1～24 hour) between room temperature to 100 ℃ afterwards.
(2). the gel that (1) is obtained place between room temperature to 100 ℃ aging (be generally 24 hours～5 days) more than 24 hours organic wet gel.
(3). organic temperature gel that (2) are obtained places acetone to carry out solvent exchange and (is generally 2 days～5 days) more than 2 days, makes organic solvent be full of gel.
(4). organic wet gel that (3) are obtained, kept under its super critical condition 1～3 hour as supercritical medium with the organic solvent identical with replacement solvent, made organic aerogel.
Or organic wet gel that will be obtained by (3), kept under its super critical condition 1～3 hour as supercritical medium with sherwood oil (30～60 ℃ of boiling points) after the organic solvent displacement, made organic aerogel.
Or organic wet gel that will be obtained by (3) take carbonic acid gas as drying medium, kept under its super critical condition 1～3 hour after the organic solvent displacement, made organic aerogel.
(5). the organic aerogel of (4) gained is placed charring furnace; under protection of inert gas, heat charing; carbonization temperature (is generally 500～1200 ℃) more than 500 ℃; carbonization time (was generally 1～5 hour) more than 1 hour; naturally cool to afterwards room temperature, obtain charcoal-aero gel.
Further, described alkali catalyst is sodium hydroxide or potassium hydroxide, and said organic solvent is ethanol, propyl alcohol, Virahol or acetone.Described rare gas element is nitrogen or argon gas.
The invention provides the new way of preparation low density P-F charcoal-aero gel under the low base catalyst concentration of a water.Namely adopt Resorcinol as helping monomer and nucleator, make Resorcinol under strong base concentrations at first with the oxymethylene polymerization nucleation, the formation reaction intermediate, this intermediate again with phenol and the further polymerization generating three-dimensional of formaldehyde dimensional network structure, thereby phenol and formaldehyde are reacted to each other under low base catalyst concentration obtain organogel, supercritical drying behind the solvent exchange, charing makes charcoal-aero gel.After adding a certain amount of Resorcinol, this technique can be hanged down (mol ratio P/C≤100 under the base catalyst concentration at water, this moment, the pH value of solution was 6.0～7.5) obtain organogel (having avoided occurring because the catalyzer deficiency obtains the phenomenon of solid precipitation), carbon aerogel particle size after the charing is little, porosity is high, and specific surface area is large.Compared with prior art; the raw material phenol cost of use of the present invention is the cheapest; and can under the prerequisite of alkali as catalyzer of relatively small amount, make charcoal-aero gel; this is being very large progress aspect preparation of phenol formaldehyde (PF) based charcoal aerogel; further study important role for it; while also is conducive to environmental protection and meets the concept of Green Chemistry, and can alleviate the use of alkali for the corrosion of production unit, easier mass-producing and suitability for industrialized production.
Principal feature of the present invention is: (1) adopts water-soluble monomer is raw material, and water is as reaction solvent; (2) when gel polymerisation, add Resorcinol as helping monomer and nucleator, obtain organogel thereby phenol and formaldehyde are reacted to each other under low base catalyst concentration; (3) organogel gets organic aerogel through the solvent exchange supercritical drying.
The prepared charcoal-aero gel of the present invention contains a large amount of mesopores, micropore and some macropores, and the BET specific surface area is up to 680m
2/ g, pore volume is up to 1.042cm
3g
-1And raw materials cost is low, and can react under low base catalysis concentration and obtain gel, the research important in inhibiting of Pyrogentisinic Acid-formaldehyde charcoal-aero gel; its further research is laid a solid foundation, simultaneously its mass-producing and suitability for industrialized production are played important promoter action.
Below the invention will be further described by drawings and Examples.
Description of drawings
Fig. 1 is the SEM figure of the charcoal-aero gel for preparing of the present invention;
Fig. 2 is the nitrogen adsorption isothermal line of embodiment 6,
Fig. 3 is the nitrogen adsorption isothermal line of embodiment 10.
As can be seen from Figure 1, the charcoal-aero gel that the present invention makes contains some micropores, abundant mesopore and the macropore that can regulate and control content, and the BET specific surface area is up to 680m
2/ g, pore volume is up to 1.042cm
3g
-1, the network particle diameter is about 10～60 nanometers.
Embodiment
Embodiment 1: according to PFR%=30wt%; P/F=1/3; P/R=10/1; P/C=20/1 (C is potassium hydroxide); with 15.0 gram phenol; 1.75 gram Resorcinol; 0.45 gram potassium hydroxide; the formalin of 36 milliliters of 37wt% mixes and stirs; adding deionized water makes solution to 100m l and stirs again; this moment, the pH value of solution was 7.4; pour into afterwards in the ampoule and make it and seal; gel is 1 hour in 100 ℃ of water-baths; behind gel, move to the organogel that wore out 4 days to get in 80 ℃ of water-baths; then carried out solvent exchange 3 days with acetone again; acetone is full of in the pore structure of organogel; and then use the sherwood oil of 30～60 ℃ of boiling points to carry out the supercritical drying organogel 2 hours as supercritical medium; obtain organic aerogel, the last lower 500 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 5 hours.The density that records charcoal-aero gel is 0.520g/cm
3, the BET specific surface area is 682.97m
2/ g, pore volume are 1.042cm
3g
-1
Embodiment 2: according to PFR%=30wt%; P/F=1/3; P/R=10/1; P/C=25/1 (C is sodium hydroxide); with 15.0 gram phenol; 1.75 gram Resorcinol; 0.357 gram sodium hydroxide; the formalin of 36 milliliters of 38wt% mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 7.3; pour into afterwards in the ampoule and make it and seal; gel is 24 hours in 70 ℃ of water-baths; behind gel, move to the organogel that wore out 5 days to get in 80 ℃ of water-baths; then carried out solvent exchange 5 days with acetone again; acetone is full of in the pore structure of organogel; and then use acetone to carry out the supercritical drying organogel 5 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 2 hours.The density that records charcoal-aero gel is 0.535g/cm
3, the BET specific surface area is 531.55m
2/ g, pore volume are 0.684cm
3g
-1
Embodiment 3: according to PFR%=30wt%; P/F=1/3; P/R=10/1; P/C=30/1 (C is sodium hydroxide); with 15.0 gram phenol; 1.75 gram Resorcinol; 0.297 gram sodium hydroxide; the formalin of 36 milliliters of 39wt% mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 6.9; pour into afterwards in the ampoule and make it and seal; gel is 10 hours in 80 ℃ of water-baths; behind gel, move to the organogel that wore out 2 days to get in 60 ℃ of water-baths; then carried out solvent exchange 2 days with acetone again; acetone is full of in the pore structure of organogel; and then use carbonic acid gas to carry out the supercritical drying organogel 3 hours as supercritical medium; obtain organic aerogel, the last lower 1200 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 1 hour.The density that records charcoal-aero gel is 0.556g/cm
3, the BET specific surface area is 629.13m
2/ g, pore volume are 0.981cm
3g
-1
Embodiment 4: according to PFR%=30wt%; P/F=1/3; P/R=5/1; P/C=50/1 (C is potassium hydroxide); with 13.73 gram phenol; 3.215 gram Resorcinol; 0.164 gram potassium hydroxide; 32.32 the formalin of milliliter 40wt% mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 6.5; pour into afterwards in the ampoule and make it and seal; gel is 10 hours in 90 ℃ of water-baths; behind gel, move to the organogel that wore out 4 days to get in 80 ℃ of water-baths; then carried out solvent exchange 5 days with ethanol again; ethanol is full of in the pore structure of organogel; and then use ethanol to carry out the supercritical drying organogel 4 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 5 hours.The density that records charcoal-aero gel is 0.506g/cm
3, the BET specific surface area is 600.752m
2/ g, pore volume are 0.787cm
3g
-1
Embodiment 5: according to PFR%=30wt%; P/F=1/3; P/R=5/1; P/C=60/1 (C is potassium hydroxide); with 13.73 gram phenol; 3.215 gram Resorcinol; 0.1365 gram potassium hydroxide; 32.32 the formalin of milliliter 38.5wt% mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 6.2; pour into afterwards in the ampoule and make it and seal; gel is 15 hours in 100 ℃ of water-baths; behind gel, move to the organogel that wore out 5 days to get in 70 ℃ of water-baths; then carried out solvent exchange 5 days with propyl alcohol again; propyl alcohol is full of in the pore structure of organogel; and then use propyl alcohol to carry out the supercritical drying organogel 10 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 3 hours.The density that records charcoal-aero gel is 0.529g/cm
3, the BET specific surface area is 559.16m
2/ g, pore volume are 0.787cm
3g
-1
Embodiment 6: according to PFR%=30wt%; P/F=1/3; P/R=5/1; P/C=70/1 (C is potassium hydroxide); with 13.73 gram phenol; 3.215 gram Resorcinol; 0.117 gram potassium hydroxide; 32.32 the formalin of milliliter 37wt% mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 6.0; pour into afterwards in the ampoule and make it and seal; gel is 24 hours in 90 ℃ of water-baths; behind gel, move to the organogel that wore out 1 day to get in 80 ℃ of water-baths; then carried out solvent exchange 3 days with isopropyl acetone again; isopropyl acetone is full of in the pore structure of organogel; and then use isopropyl acetone to carry out the supercritical drying organogel 3 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 2 hours.The density that records charcoal-aero gel is 0.498/cm
3, the BET specific surface area is 477.72m
2/ g, pore volume are 0.770cm
3g
-1
Embodiment 7: according to PFR%=20wt%; P/F=1/3; P/R=10/1; P/C=20/1 (C is potassium hydroxide); with 9.505 gram phenol; 1.112 gram Resorcinol; 0.283 gram potassium hydroxide; 22.36 the formalin of milliliter 38.5wt% mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 7.4; pour into afterwards in the ampoule and make it and seal; gel is 8 hours in 90 ℃ of water-baths; behind gel, move to the organogel that wore out 4 days to get in 80 ℃ of water-baths; then carried out solvent exchange 3 days with acetone again; acetone is full of in the pore structure of organogel; and then to use boiling point be that 30～60 ℃ sherwood oil carried out the supercritical drying organogel 2 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 2 hours.The density that records charcoal-aero gel is 0.648g/cm
3, the BET specific surface area is 572.14m
2/ g, pore volume are 0.658cm
3g
-1
Embodiment 8: according to PFR%=60wt%; P/F=1/3; P/R=10/1; P/C=20/1 (C is sodium hydroxide); with 23.76 gram phenol; 2.78 gram Resorcinol; 0.7075 gram potassium hydroxide; 55.9 milliliter 38.5wt% formalin mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 7.5; pour into afterwards in the ampoule and make it and seal; gel is 6 hours in 90 ℃ of water-baths; behind gel, move to the organogel that wore out 5 days to get in 80 ℃ of water-baths; then carried out solvent exchange 3 days with acetone again; acetone is full of in the pore structure of organogel; and then to use boiling point be that 30～60 ℃ sherwood oil carried out the supercritical drying organogel 3 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 3 hours.The density that records charcoal-aero gel is 0.678g/cm
3, the BET specific surface area is 498.78m
2/ g, pore volume are 0.721cm
3g
-1
Embodiment 9: according to PFR%=30wt%; P/F=1/2; P/R=10/1; P/C=20/1 (C is potassium hydroxide); with 16.81 gram phenol; 1.967 gram Resorcinol; 0.501 gram potassium hydroxide; 26.36 milliliter 38.5wt% formalin mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 7.5; pour into afterwards in the ampoule and make it and seal; gel is 9 hours in 90 ℃ of water-baths; behind gel, move to the organogel that wore out 4 days to get in 80 ℃ of water-baths; then carried out solvent exchange 3 days with acetone again; acetone is full of in the pore structure of organogel; and then to use boiling point be that 30～60 ℃ sherwood oil carried out the supercritical drying organogel 2 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of nitrogen protection obtained charcoal-aero gel in 2 hours.The density that records charcoal-aero gel is 0.601g/cm
3, the BET specific surface area is 677.52m
2/ g, pore volume are 0.784cm
3g
-1
Embodiment 10: according to PFR%=30wt%; P/F=1/5; P/R=10/1; P/C=20/1 (C is sodium hydroxide); with 10.94 gram phenol; 1.28 gram Resorcinol; 1.087 gram potassium hydroxide; 42.87 milliliter 38.5wt% formalin mixes and stirs; adding deionized water makes solution to 100ml and stirs again; this moment, the pH value of solution was 7.3; pour into afterwards in the ampoule and make it and seal; gel is 7 hours in 90 ℃ of water-baths; behind gel, move to the organogel that wore out 4 days to get in 80 ℃ of water-baths; then carried out solvent exchange 3 days with acetone again; acetone is full of in the pore structure of organogel; and then to use boiling point be that 30～60 ℃ sherwood oil carried out the supercritical drying organogel 3 hours as supercritical medium; obtain organic aerogel, the last lower 900 ℃ of charings of argon shield obtained charcoal-aero gel in 2 hours.The density that records charcoal-aero gel is 0.446g/cm
3, the BET specific surface area is 604.05m
2/ g, pore volume are 0.623cm
3g
-1
Claims (5)
1. prepare the method for P-F charcoal-aero gel under the low alkali, it is characterized in that, take phenol and formaldehyde as reaction monomers, Resorcinol is as helping monomer and nucleator, highly basic is catalyzer, and water is solvent, and organic wet gel wears out to get behind heating gel between 70 ℃ to 100 ℃; Should carry out the organic solvent displacement by organic wet gel, and make organic solvent be full of gel; Organic wet gel supercritical drying after the displacement is got organic aerogel; The charing in inert atmosphere of this organic aerogel is got required charcoal-aero gel; Used each material mixture ratio is: the mol ratio P/F of phenol and formaldehyde is 0.2～1; The mol ratio P/R of phenol and Resorcinol is 2～20; The mol ratio P/C of phenol and highly basic is 2～100; Reactant total concn PFR% is 10～60wt%.
2. in accordance with the method for claim 1, it is characterized in that described formaldehyde is the formalin of 37～40wt%.
3. according to claim 1 or 2 described methods, it is characterized in that specific embodiment is:
(1). phenol, formaldehyde, Resorcinol, highly basic and water are mixed and stir according to predetermined formulation, afterwards in the reaction cartridge bottle and sealing, between 70 ℃ to 100 ℃, heat afterwards and obtained gel in 1～24 hour;
(2). the gel that (1) is obtained placed between 60 ℃ to 100 ℃ aging 1～5 day, got organic wet gel;
(3). organic wet gel that (2) are obtained places organic solvent to carry out solvent exchange 2～5 days, makes organic solvent be full of gel;
(4). the organic wet gel after organic solvent displacement that will be obtained by (3),, under its super critical condition, kept 1～10 hour as supercritical medium take boiling point as 30～60 ℃ sherwood oil, make organic aerogel;
Or the organic wet gel after organic solvent displacement that will be obtained by (3), take carbonic acid gas as drying medium, under its super critical condition, kept 1～10 hour, make organic aerogel;
(5). the organic aerogel of (4) gained is placed charring furnace, under protection of inert gas, heat charing, 500～1200 ℃ of carbonization temperatures, carbonization time 1～5 hour naturally cools to room temperature afterwards, obtains charcoal-aero gel.
4. in accordance with the method for claim 3, it is characterized in that described alkali catalyst is sodium hydroxide or potassium hydroxide, said organic solvent is ethanol, propyl alcohol or acetone.
5. in accordance with the method for claim 3, it is characterized in that described rare gas element is argon gas.
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| CN102423668A (en) * | 2011-09-09 | 2012-04-25 | 中国人民解放军国防科学技术大学 | Preparation method of phenolic resin base carbon aerogel |
| CN103525377B (en) * | 2013-09-30 | 2017-01-04 | 安科智慧城市技术（中国）有限公司 | Collect the preparation method of hot material and there is collecting plate and the heat collector of this collection hot material |
| CN106013640B (en) * | 2016-05-28 | 2018-12-07 | 绍兴艺涵纺织有限公司 | A kind of air purification wall cloth |
| CN106829911A (en) * | 2016-09-19 | 2017-06-13 | 广东工业大学 | A kind of porous carbon electrode material and its preparation method and application |
| CN108316487B (en) * | 2018-01-20 | 2020-07-17 | 金粤幕墙装饰工程有限公司 | Inert aerogel and preparation method thereof |
| CN109133027B (en) * | 2018-07-25 | 2020-05-26 | 沈阳理工大学 | Method for preparing mesoporous carbon material by catalyzing phenolic polymerization with magnesium carbonate trihydrate |
| CN109734072B (en) * | 2019-03-11 | 2022-05-03 | 中国科学院合肥物质科学研究院 | Phenolic-based carbon aerogel material and preparation method thereof |
| CN110371947A (en) * | 2019-06-21 | 2019-10-25 | 庞定根 | A kind of preparation method of middle micropore charcoal-aero gel |
| CN111892420B (en) * | 2020-07-29 | 2022-05-03 | 南京工业大学 | Method for preparing massive titanium carbide, titanium nitride or titanium carbonitride aerogel |
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