CN115504451A - Carbon aerogel with high specific surface area and preparation method thereof - Google Patents
Carbon aerogel with high specific surface area and preparation method thereof Download PDFInfo
- Publication number
- CN115504451A CN115504451A CN202211320350.7A CN202211320350A CN115504451A CN 115504451 A CN115504451 A CN 115504451A CN 202211320350 A CN202211320350 A CN 202211320350A CN 115504451 A CN115504451 A CN 115504451A
- Authority
- CN
- China
- Prior art keywords
- surface area
- carbon aerogel
- specific surface
- high specific
- aerogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000178 monomer Substances 0.000 claims abstract description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 16
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005011 phenolic resin Substances 0.000 claims abstract description 16
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000004964 aerogel Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 230000032683 aging Effects 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 9
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 238000000352 supercritical drying Methods 0.000 claims abstract description 8
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 238000001879 gelation Methods 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000000758 substrate Substances 0.000 claims abstract description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 14
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229960004011 methenamine Drugs 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 7
- 150000001299 aldehydes Chemical class 0.000 claims description 6
- 239000007772 electrode material Substances 0.000 claims description 5
- 239000008098 formaldehyde solution Substances 0.000 claims description 5
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004887 air purification Methods 0.000 claims description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 229920002866 paraformaldehyde Polymers 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000006258 conductive agent Substances 0.000 claims description 2
- 239000008236 heating water Substances 0.000 claims description 2
- 239000007773 negative electrode material Substances 0.000 claims description 2
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 2
- 229960001553 phloroglucinol Drugs 0.000 claims description 2
- 230000002431 foraging effect Effects 0.000 claims 1
- 150000001298 alcohols Chemical class 0.000 abstract 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000000969 carrier Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001599 direct drying Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002210 supercritical carbon dioxide drying Methods 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a carbon aerogel with high specific surface area and a preparation method thereof, wherein the carbon aerogel is obtained by preparing sol by a high-temperature hydrothermal method, and then sequentially performing gelation, aging, drying and high-temperature carbonization, and the specific surface area of the carbon aerogel is 1100-1600 m 2 (ii) in terms of/g. The preparation method comprises the following steps: taking a phenol monomer and an aldehyde monomer as reaction substrates, a methanol solution as a solvent and sodium carbonate as a catalyst, reacting for a certain time under the reflux of a high-temperature water bath, adding a hexamethylenetetramine solution, uniformly stirring, and then putting into hot water for gel aging to obtain an alcogel; then, carrying out supercritical drying to obtain phenolic resin aerogel; and finally, carbonizing under the protection of inert gas to obtain the carbon aerogel. The method can improve the reaction rate, improve the specific surface area of the carbon aerogel, simultaneously take alcohols as a solvent, do not need solvent replacement, shorten the preparation period, and inhibit the volume shrinkage in a supercritical drying mode.
Description
Technical Field
The invention relates to the technical field of aerogels, in particular to phenolic resin-based carbon aerogel and a preparation method thereof.
Background
Carbon aerogel (also called carbon aerogel) is a novel three-dimensional porous material, and has the advantages of small density, good conductivity, large porosity and large specific surface area (usually 600-1000 m) 2 The,/g) and the like. At present, resorcinol and formaldehyde are used as precursors in the main method for preparing the carbon aerogel, phenolic aerogel is obtained through sol-gel reaction, solvent replacement and normal-pressure drying, and the carbon aerogel is obtained through carbonization. However, solvent replacement requires a large amount of liquid with low surface tension such as ethanol, acetone, etc. to repeatedly replace water in the wet gel, and is complicated in steps, long in time, and not suitable for large-scale industrial production.
CN109850870A discloses a method for rapidly preparing carbon aerogel, which uses industrial phenolic resin as raw material, hexamethylenetetramine as curing agent, ethylene glycol and water as solvent, after mixing, performs sol-gel reaction at a certain temperature, obtains phenolic aerogel through drying under normal pressure, and then carbonizes at high temperature to obtain carbon aerogel. The technical scheme takes ethylene glycol as a solvent, and the phenolic aerogel can be obtained by direct drying without solvent replacement, so that the preparation period of the carbon aerogel is shortened to a certain extent, but the industrial phenolic resin serving as the raw material has high crosslinking degree, and the prepared carbon aerogel has small specific surface area which is less than 800m 2 And/g, the carbon aerogel with high specific surface area cannot be obtained, normal pressure drying is adopted during drying, and the internal structure of the carbon aerogel collapses due to volume shrinkage caused by the existence of capillary force, so that the specific surface area is further reduced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the carbon aerogel with the high specific surface area and the preparation method thereof, and aims to solve the technical problems of small specific surface area, long preparation period and high cost of the carbon aerogel.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the high specific surface area carbon aerogel is prepared by preparing sol by a high-temperature hydrothermal method, and then sequentially performing gelation, aging, drying and high-temperature carbonization, and the specific surface area is 1100-1600 m 2 /g。
Further, the invention also provides a preparation method of the carbon aerogel with high specific surface area, which comprises the following steps:
1) Taking a phenol monomer and an aldehyde monomer as reaction substrates, a methanol solution as a solvent and sodium carbonate as a catalyst, reacting for a certain time under the reflux of a heating water bath, adding a hexamethylene tetramine solution, uniformly stirring, and then putting into hot water for gel aging to obtain alcohol gel;
2) Carrying out supercritical drying on the alcogel to obtain phenolic resin aerogel;
3) And carbonizing the phenolic resin aerogel under the protection of inert gas to obtain the carbon aerogel. Wherein, the hexamethylene tetramine solution is a cross-linking agent and a catalyst, and can participate in the reaction to accelerate the curing.
Further, the molar ratio of the phenolic monomer to the aldehyde monomer is 1:0.5 to 5; the molar ratio of the phenolic monomer to the methanol is 1:5 to 27; the molar ratio of the phenolic monomer to the sodium carbonate is 300-1000: 1; the volume fraction of the methanol in the methanol solution is 60 (v/v)% -92 (v/v)%. The concentration of methanol is too low, the water content is higher, the specific surface area is reduced after drying, and therefore the volume fraction of methanol is larger.
Further, the molar ratio of the phenolic monomer to the hexamethylene tetramine in the step 1) is (1-20): 1.
further, the phenolic monomer is one or more of resorcinol, hydroquinone and phloroglucinol; the aldehyde monomer is one or more of formaldehyde solution, furfural solution and solid paraformaldehyde.
Further, the water bath temperature in the step 1) is 75-90 ℃, and the reaction time is 60-120 min.
Further, the temperature of the water bath in the step 1) is 75-80 ℃, and the reaction time is 60-90 min.
Further, the aging temperature of the alcogel in the step 1) is 45-70 ℃, and the aging time is 24-72 hours. The aging temperature and the aging time are controlled within the range, so that the structure of the aerogel can be further strengthened, and the excessive volume shrinkage during drying is prevented.
Further, the temperature rising rate of carbonization in the step 3) is 2-7 ℃/min, the temperature rises to 800-1400 ℃, the temperature is kept for 1-3 h, and the product is naturally cooled to the room temperature.
Compared with the prior art, the invention has the following beneficial effects:
1. the carbon aerogel disclosed by the invention has a high specific surface area, completely meets the requirements of air purification, catalyst carriers and electrode materials, and can be widely applied to the fields of supercapacitors, colored wastewater treatment, hydrogen storage and the like.
2. The invention creatively researches a carbonization treatment to achieve the high specific surface area and has short time. The gel is prepared by adopting a high-temperature hydrothermal method, so that the reaction rate can be improved, the crosslinking degree of the phenolic resin can be controlled by controlling the reaction time, and the matching of the phenolic resin with small crosslinking degree and a crosslinking agent is more favorable for forming micropores in the carbonization process, so that the specific surface area of the carbon aerogel is improved. Meanwhile, supercritical drying is adopted in a drying mode, so that the damage to an aerogel framework caused by solvent volatilization can be effectively inhibited, and the problem that the specific surface area is further reduced due to the fact that the volume is shrunk due to the existence of capillary force to cause collapse of the internal structure of the carbon aerogel due to normal-pressure drying can be solved.
3. The solvent used in the invention is alcoholic solution with higher concentration, can control the water content in the reaction system, does not need solvent replacement, further shortens the reaction time, and is beneficial to industrial large-scale production. Researches show that the preparation period of the carbon aerogel prepared by the method is only about 2 days, the production efficiency is greatly improved, and the cost is low.
Drawings
FIG. 1 is a process flow diagram of a carbon aerogel preparation process of the present invention;
FIG. 2 is a schematic representation of the practice of the present inventionN of example 1 2 Adsorption isotherms.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described below with reference to specific examples, but the embodiments of the present invention are not limited thereto.
The process flow diagram of the invention is shown in figure 1.
Example 1
A preparation method of carbon aerogel with high specific surface area comprises the following steps:
taking 175g of anhydrous methanol, 25g of water, 48.25g of resorcinol, 26g of solid paraformaldehyde and 0.125g of sodium carbonate, putting the three-neck flask into a water bath kettle, setting the temperature of the water bath kettle at 80 ℃, heating and refluxing for 90min, and cooling to 55 ℃. And adding 20g of 4M hexamethylene tetramine solution into the three-neck flask, performing gel aging in hot water at 55 ℃ for 24 hours, and performing supercritical drying on the obtained sample for 8 hours by using carbon dioxide. And after drying, taking out the phenolic resin aerogel, and carbonizing in a high-temperature carbonization furnace to obtain the carbon aerogel. The carbonization temperature parameters are as follows: heating to 1000 deg.C at a heating rate of 3 deg.C/min, and maintaining for 60min.
N of example 1 2 The adsorption isotherms are shown in FIG. 2, and the specific surface area thereof was found to be 1508m by the BET multipoint method 2 The density of the sample is 0.315g/cm 3 。
Example 2
A preparation method of carbon aerogel with high specific surface area comprises the following steps:
114g of anhydrous methanol, 33g of resorcinol, 49.8g of formaldehyde solution (wherein the mass fraction of formaldehyde is 37%) and 0.096g of sodium carbonate are placed in a three-necked flask, uniformly stirred, placed in a water bath kettle, heated and refluxed for 90min at the water bath kettle temperature of 80 ℃ and cooled to 55 ℃. Then, 15g of 4M hexamethylenetetramine solution was added to the three-necked flask, the gel was aged in hot water at 55 ℃ for 24 hours, and the obtained sample was subjected to supercritical carbon dioxide drying for 8 hours. And after drying, taking out the phenolic resin aerogel, and carbonizing in a high-temperature carbonization furnace to obtain the carbon aerogel. The carbonization temperature parameters are as follows: heating to 1000 deg.C at a heating rate of 3 deg.C/min, and maintaining for 60min.
The specific surface area of the obtained carbon aerogel sample is 1132m 2 Per g, density 0.332g/cm 3 。
Example 3
A preparation method of carbon aerogel with high specific surface area comprises the following steps:
114g of anhydrous methanol, 33g of resorcinol, 49.8g of formaldehyde solution (wherein the mass fraction of formaldehyde is 37%) and 0.096g of sodium carbonate are placed in a three-necked flask, uniformly stirred, placed in a water bath kettle, heated and refluxed for 90min at the water bath kettle temperature of 80 ℃ and cooled to 55 ℃. And 8g of 4M cyclohexamethylene tetramine solution is added into the three-neck flask, the gel is aged for 48h in hot water at 55 ℃, and the obtained sample is placed in carbon dioxide for supercritical drying for 8h. And after drying, taking out the phenolic resin aerogel, and carbonizing in a high-temperature carbonization furnace to obtain the carbon aerogel. The carbonization temperature parameters are as follows: heating to 1400 deg.C at a heating rate of 3 deg.C/min, and maintaining for 60min.
The specific surface area of the obtained carbon aerogel sample is 1236m 2 (g) density of 0.3023g/cm 3 。
The effects of the inventive examples and comparative examples are compared as shown in table 1.
TABLE 1
Wherein, the comparative examples 1 and 2 are that resorcinol, formaldehyde solution and sodium carbonate solution are added into deionized water, the prepared solution is evenly stirred for 30min, then is sealed and put into a constant temperature oven, is treated for 4 days at 85 ℃, contains 5 percent ethanol (volume ratio) of water for 2 to 4 times, each time lasts for about 24h, then is dried under normal pressure, and the carbon aerogel is obtained by high-temperature carbonization after the ethanol is volatilized completely. And, the specific surface area of the carbon aerogels of comparative examples 1, 2 is less than 800m 2 A long process time, a high cost and discomfortCan be used in industrial production.
The carbon aerogel with high specific surface area prepared in the examples 1 to 3 is used for air purification, catalyst carriers, electrode materials and sewage treatment, and the characteristic of high specific surface area is fully utilized, so that the carbon aerogel has unexpected technical effects compared with the traditional products. For example, the carbon aerogel is used as a negative electrode active material, is homogenized with a small amount of conductive agent and binder, has a specific capacity of 700mAh/g, and is obviously superior to the charge-discharge performance of the traditional graphite (with the specific capacity of 360-372 mAh/g) electrode.
In conclusion, the phenolic resin is prepared by adopting a high-temperature hydrothermal method, the crosslinking degree of the phenolic resin can be controlled by controlling the reaction time, and the phenolic resin with small crosslinking degree and the curing agent are favorable for forming micropores in the carbonization process, so that the specific surface area of the carbon aerogel is increased. The specific surface area of the carbon aerogel prepared by the method reaches 1100m 2 More than g, can be widely applied to air purification, catalyst carriers, electrode materials and sewage treatment. The reaction rate of the invention is high, the process takes time and only takes two days to prepare the carbon aerogel with high specific surface area, the production efficiency is greatly improved, and the invention is suitable for industrial production. Meanwhile, supercritical drying is adopted in the invention, so that the problem that the specific surface area is reduced due to collapse of an internal structure caused by normal-pressure drying can be avoided. In addition, the density, the pore size distribution and the specific surface area are adjustable, and the post-treatment can be realized on the basis of carbon aerogel.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.
Claims (10)
1. The high specific surface area carbon aerogel is characterized in that sol is prepared by a high-temperature hydrothermal method, and then the sol is sequentially subjected to gelation, aging, drying and high-temperature carbonization to obtain the high specific surface area carbon aerogel with the specific surface area of 1100-1600 m 2 /g。
2. A preparation method of carbon aerogel with high specific surface area is characterized by comprising the following steps:
1) Taking a phenol monomer and an aldehyde monomer as reaction substrates, a methanol solution as a solvent and sodium carbonate as a catalyst, reacting for a certain time under reflux of a heating water bath, adding a solution of hexamethylene tetramine, uniformly stirring, and then putting into hot water for gel aging to obtain alcohol gel;
2) Carrying out supercritical drying on the alcogel to obtain phenolic resin aerogel;
3) Carbonizing the phenolic resin aerogel under the protection of inert gas to obtain the carbon aerogel of claim 1.
3. The method for preparing carbon aerogel with high specific surface area as recited in claim 2,
the molar ratio of the phenolic monomer to the aldehyde monomer is 1:0.5 to 5;
the molar ratio of the phenolic monomer to the methanol is 1:5 to 27;
the molar ratio of the phenolic monomer to the sodium carbonate is 300-1000: 1;
the volume fraction of methanol in the methanol solution is 60 (v/v)% -92 (v/v)%.
4. The method for preparing carbon aerogel with high specific surface area according to claim 2, wherein the molar ratio of the phenolic monomer to the hexamethylene tetramine in the step 1) is (1-20): 1.
5. the preparation method of the carbon aerogel with high specific surface area as in claim 2, wherein the phenolic monomer is one or more of resorcinol, hydroquinone and phloroglucinol; the aldehyde monomer is one or more of formaldehyde solution, furfural solution and solid paraformaldehyde.
6. The method for preparing the carbon aerogel with the high specific surface area as recited in claim 2, wherein the temperature of the water bath in the step 1) is 75-90 ℃, and the reaction time is 60-120 min.
7. The method for preparing carbon aerogel with high specific surface area according to claim 2, wherein the water bath temperature in the step 1) is 75-80 ℃, and the reaction time is 60-90 min.
8. The method for preparing carbon aerogel with high specific surface area according to claim 2, wherein the temperature for aging the alcogel in the step 1) is 45-70 ℃ and the aging time is 24-72h.
9. Use of the carbon aerogel having a high specific surface area, which is used in air purification, catalyst carrier, electrode material, and sewage treatment according to claim 1.
10. The use of a high surface area carbon aerogel according to claim 9, wherein said carbon aerogel is used as a negative electrode active material, homogenized with a small amount of a conductive agent and a binder as an electrode material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211320350.7A CN115504451A (en) | 2022-10-26 | 2022-10-26 | Carbon aerogel with high specific surface area and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211320350.7A CN115504451A (en) | 2022-10-26 | 2022-10-26 | Carbon aerogel with high specific surface area and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115504451A true CN115504451A (en) | 2022-12-23 |
Family
ID=84511620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211320350.7A Pending CN115504451A (en) | 2022-10-26 | 2022-10-26 | Carbon aerogel with high specific surface area and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115504451A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009057902A1 (en) * | 2007-10-30 | 2009-05-07 | Korea Institute Of Science And Technology | Carbon aerogels for supercapacitors and method for manufacturing the same |
| KR20110030950A (en) * | 2009-09-18 | 2011-03-24 | 한국세라믹기술원 | Manufacturing method of carbon aerogel, manufacturing method of supercapacitor electrode, and manufacturing method of supercapacitor |
| 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 |
| CN109850870A (en) * | 2019-04-11 | 2019-06-07 | 中国科学院金属研究所 | A kind of high-strength carbon aeroge and its preparation method and application |
| CN114715878A (en) * | 2022-04-29 | 2022-07-08 | 上海活性炭厂有限公司 | Phenolic resin-based carbon aerogel and preparation method thereof |
-
2022
- 2022-10-26 CN CN202211320350.7A patent/CN115504451A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009057902A1 (en) * | 2007-10-30 | 2009-05-07 | Korea Institute Of Science And Technology | Carbon aerogels for supercapacitors and method for manufacturing the same |
| KR20110030950A (en) * | 2009-09-18 | 2011-03-24 | 한국세라믹기술원 | Manufacturing method of carbon aerogel, manufacturing method of supercapacitor electrode, and manufacturing method of supercapacitor |
| 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 |
| CN109850870A (en) * | 2019-04-11 | 2019-06-07 | 中国科学院金属研究所 | A kind of high-strength carbon aeroge and its preparation method and application |
| CN114715878A (en) * | 2022-04-29 | 2022-07-08 | 上海活性炭厂有限公司 | Phenolic resin-based carbon aerogel and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 杨永生: "细化工配方原理与剖析实验", 30 September 2021, 华中科技大学出版者, pages: 102 * |
| 魏炳波: "中国战略性新兴产业-前沿新材料 气凝胶", 31 October 2020, 中国铁道出版社有限公司, pages: 60 - 61 * |
| 黄常刚;唐永建;王朝阳;闫红梅;: "间苯三酚-甲醛气凝胶及其碳气凝胶的制备与表征", 强激光与粒子束, no. 06 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107827107B (en) | Preparation method of kapok-based hollow porous carbon micro-tube or porous carbon micro-strip | |
| CN107651662B (en) | Method for preparing boron-nitrogen double-doped carbon aerogel | |
| CN108484963B (en) | Method for preparing phenolic aerogel by normal pressure drying method and prepared phenolic aerogel | |
| CN109850870A (en) | A kind of high-strength carbon aeroge and its preparation method and application | |
| CN114715878B (en) | Phenolic resin-based carbon aerogel and preparation method thereof | |
| CN109251005B (en) | Preparation method of reinforced silica aerogel material | |
| CN108862234A (en) | A kind of preparation method of fibre reinforced carbon aerogel composite material | |
| KR20090118200A (en) | Method of manufacturing carbon aerogel and the carbon aerogel manufactured using the same | |
| CN110041552A (en) | Compound high temperature proton exchange film and preparation method thereof based on sulfonation aryl oxide type polybenzimidazoles Yu sulfonation polysilsesquioxane | |
| CN110745807B (en) | Carbon aerogel microsphere and preparation method thereof | |
| CN111498828A (en) | Method for preparing carbon aerogel by utilizing normal-pressure drying | |
| CN114015194B (en) | Polybenzoxazine aerogel and preparation method thereof | |
| CN108726501B (en) | A method of charcoal-aero gel is prepared with infiltration evaporation membrane separation device | |
| CN115504451A (en) | Carbon aerogel with high specific surface area and preparation method thereof | |
| CN102826534A (en) | Preparation method of organic aerogel and carbon aerogel | |
| CN112479205A (en) | Narrow-pore bamboo sheath activated carbon and preparation method thereof | |
| CN110804145A (en) | Hydrogel composite material with high thermal conductivity and electric conductivity and preparation method thereof | |
| CN107324339B (en) | A kind of carbonization silica aerogel and preparation method thereof | |
| CN115249817B (en) | Catalytic graphitization method of carbon paper material for fuel cell gas diffusion layer | |
| CN112142057B (en) | Aerogel and preparation method thereof based on constant-temperature constant-humidity drying | |
| CN115608283A (en) | Carbon aerogel-tantalum pentoxide interface evaporation composite material, preparation method and application thereof | |
| KR20150050451A (en) | Electrolyte membrane for fuel cell, preparation method thereof and the fuel cell comprising using the same | |
| CN110776664B (en) | Condensed type organic silicon resin aerogel and preparation method thereof | |
| CN113996324A (en) | For CO2Preparation method of SiC-C composite aerogel through photocatalytic reduction | |
| CN110950319A (en) | Method and apparatus for reducing density of carbon aerogel material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |