CN115707652A - Method for preparing carbon material by taking waste ultrafiltration membrane as raw material and application of carbon material in preparation of supercapacitor - Google Patents
Method for preparing carbon material by taking waste ultrafiltration membrane as raw material and application of carbon material in preparation of supercapacitor Download PDFInfo
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- CN115707652A CN115707652A CN202211367521.1A CN202211367521A CN115707652A CN 115707652 A CN115707652 A CN 115707652A CN 202211367521 A CN202211367521 A CN 202211367521A CN 115707652 A CN115707652 A CN 115707652A
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- carbon material
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 84
- 239000012528 membrane Substances 0.000 title claims abstract description 58
- 239000002699 waste material Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002994 raw material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000108 ultra-filtration Methods 0.000 title claims abstract description 7
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 63
- 239000003990 capacitor Substances 0.000 claims abstract description 33
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000008247 solid mixture Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000004073 vulcanization Methods 0.000 claims abstract description 9
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 30
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 23
- 229940011182 cobalt acetate Drugs 0.000 claims description 23
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 23
- 229940078494 nickel acetate Drugs 0.000 claims description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 8
- 239000004695 Polyether sulfone Substances 0.000 description 25
- 229920006393 polyether sulfone Polymers 0.000 description 25
- 238000010008 shearing Methods 0.000 description 8
- 238000011160 research Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000007773 negative electrode material Substances 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- ZGDWHDKHJKZZIQ-UHFFFAOYSA-N cobalt nickel Chemical compound [Co].[Ni].[Ni].[Ni] ZGDWHDKHJKZZIQ-UHFFFAOYSA-N 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of carbon material preparation, and particularly discloses a method for preparing a carbon material by using a waste ultrafiltration membrane as a raw material and application of the carbon material in preparation of a supercapacitor. The method for preparing the carbon material by taking the waste filter membrane as the raw material comprises the following steps: (1) Cutting the waste filter membrane, adding the cut filter membrane into a solution containing a metal compound, adding a vulcanization accelerator, and uniformly stirring to obtain a mixed feed liquid; (2) Reacting the mixed feed liquid in a nitrogen atmosphere at 200-250 ℃ for 10-20 h, filtering after the reaction is finished, and taking a solid; (3) Reacting the solid in nitrogen atmosphere at 700-900 ℃ for 1-2 h, and taking the reacted solid mixture to obtain the carbon material. The carbon material prepared by the method is applied to the super capacitor, and compared with the carbon material prepared by the conventional high-temperature catalytic reaction, the carbon material can obviously improve the specific capacity and prolong the service life of the super capacitor.
Description
Technical Field
The invention relates to the technical field of carbon material preparation, in particular to a method for preparing a carbon material by taking a waste ultrafiltration membrane as a raw material and application of the carbon material in preparation of a super capacitor.
Background
The double-electric-layer capacitor is one kind of super capacitor, is between a battery and a capacitor, is a novel energy storage device, and the extremely large capacity of the super capacitor can be used as the battery. Compared with a battery adopting an electrochemical principle, the double-electric-layer capacitor has the advantages that the charge-discharge process of the double-electric-layer capacitor does not involve the change of substances at all, so that the double-electric-layer capacitor has the characteristics of short charging time, long service life, good temperature characteristic, energy conservation, environmental friendliness and the like.
The polyethersulfone filter membrane is a membrane material prepared by hot-melting and bonding polyethersulfone superfine fibers, and belongs to a PES membrane for deep filtration; is widely used in industry. Due to the industrial scale use, a large amount of waste polyethersulfone filter membranes are generated. However, how to treat the waste polyethersulfone filter membrane becomes a technical problem to be solved urgently.
The inventor of the invention provides a solution for preparing a carbon material by taking a waste polyether sulfone filter membrane as a raw material and carrying out a catalytic reaction on the waste polyether sulfone filter membrane at a high temperature. However, the inventors found in the research that the carbon material prepared by the conventional high-temperature catalytic reaction is used as a negative electrode material for a super capacitor, and the specific capacity and the service life of the carbon material are not high and need to be further improved.
Disclosure of Invention
In order to overcome at least one technical problem in the prior art, the invention firstly provides a method for preparing a carbon material by using a waste ultrafiltration membrane as a raw material and the carbon material. Research shows that the carbon material prepared by the method of the invention by using the waste polyether sulfone filter membrane as the raw material is applied to the super capacitor, and compared with the carbon material prepared by the conventional high-temperature catalytic reaction, the carbon material can obviously improve the specific capacity and prolong the service life of the super capacitor.
The technical problem to be solved by the invention is realized by the following technical scheme:
a method for preparing a carbon material by taking a waste filter membrane as a raw material is characterized by comprising the following steps:
(1) Cutting waste filter membranes into pieces, adding the pieces into a solution containing a metal compound, adding a vulcanization accelerator, and uniformly stirring to obtain a mixed feed liquid;
(2) Reacting the mixed feed liquid in a nitrogen atmosphere at 200-250 ℃ for 10-20 h, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid in nitrogen atmosphere at 700-900 ℃ for 1-2 h, and taking the reacted solid mixture to obtain the carbon material.
The invention provides a brand-new method for preparing a carbon material by taking a waste filter membrane as a raw material; the inventor shows through a large number of experiments that the carbon material prepared by the method is applied to the super capacitor, and compared with the carbon material prepared by adopting the conventional high-temperature catalytic reaction, the specific capacity and the service life of the super capacitor can be obviously improved.
Preferably, the waste filter membrane is a waste polyethersulfone filter membrane.
Preferably, the metal compound in step (1) is selected from cobalt acetate or nickel acetate.
The inventor finds in research that the selection of metal compounds is very critical, and the carbon materials prepared by selecting different metal compounds have different specific capacities and service lives of the supercapacitors. The inventor shows through a large number of experimental researches that when the metal compound is cobalt acetate or nickel acetate, the prepared carbon material is applied to the super capacitor, and compared with the carbon material prepared by adopting the conventional high-temperature catalytic reaction, the specific capacity and the service life of the super capacitor can be obviously improved. However, the carbon material prepared by other metal compounds is applied to the super capacitor, and the specific capacity and the service life of the super capacitor cannot be obviously improved.
Preferably, the metal compound in step (1) consists of cobalt acetate and nickel acetate; wherein the weight ratio of the cobalt acetate to the nickel acetate is 2-4;
most preferably, the weight ratio of cobalt acetate to nickel acetate is 3.
The inventor surprisingly finds out in further research that the carbon material prepared by the method provided by the invention when the metal compound consists of cobalt acetate and nickel acetate can synergistically improve the specific capacity and service life of the supercapacitor; the improvement degree of the specific capacity and the service life of the super capacitor is greatly higher than that of a carbon material prepared by selecting cobalt acetate or nickel acetate as a metal compound.
Preferably, in the solution containing the metal compound in the step (1), the mass concentration of the metal compound is 10 to 15%.
Most preferably, the mass concentration of the metal compound is 12%.
Preferably, in the step (1), the ratio of the used filter membrane, the vulcanization accelerator and the solution containing the metal compound is 20-40 g: 1-3 g: 100-200 mL.
Most preferably, in the step (1), the ratio of the used filter membrane, the vulcanization accelerator and the solution containing the metal compound is 30g:2g:150mL.
Preferably, the vulcanization accelerator described in step (1) is thiourea.
Preferably, in the step (2), the mixed solution is reacted for 15 hours at 220 ℃ in a nitrogen atmosphere.
Preferably, in step (3), the solid mixture is reacted at 800 ℃ for 1.5h in a nitrogen atmosphere.
The invention also provides application of the carbon material prepared by the method in preparation of a capacitor.
Preferably, the capacitor is a super capacitor.
Has the advantages that: the invention firstly provides a brand-new method for preparing a carbon material by taking a waste ultrafiltration membrane as a raw material and the carbon material. Research shows that the carbon material prepared by the method is applied to the super capacitor by taking the waste polyether sulfone filter membrane as the raw material, and compared with the carbon material prepared by the conventional high-temperature catalytic reaction, the carbon material can obviously improve the specific capacity and prolong the service life of the super capacitor.
Detailed Description
The present invention is further explained below with reference to specific examples, which are not intended to limit the present invention in any way.
Example 1
(1) Shearing waste polyethersulfone filter membranes, adding the filter membranes into a solution containing metal compounds, adding thiourea, and uniformly stirring to obtain a mixed feed liquid;
(2) Reacting the mixed feed liquid for 15 hours at 220 ℃ in a nitrogen atmosphere, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid for 1.5 hours at 800 ℃ in a nitrogen atmosphere, and taking a solid mixture after the reaction to obtain the carbon material;
in the step (1), the dosage ratio of the waste polyether sulfone filter membrane, the thiourea and the solution containing the metal compound is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12%; the metal compound is cobalt acetate.
Example 2
(1) Shearing waste polyethersulfone filter membranes, adding the filter membranes into a solution containing metal compounds, adding thiourea, and uniformly stirring to obtain a mixed feed liquid;
(2) Reacting the mixed material liquid for 15 hours at 220 ℃ in a nitrogen atmosphere, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid for 1.5 hours at 800 ℃ in a nitrogen atmosphere, and taking a solid mixture after the reaction to obtain the carbon material;
in the step (1), the dosage ratio of the waste polyether sulfone filter membrane, the thiourea and the solution containing the metal compound is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12 percent; the metal compound is nickel acetate.
Example 3
(1) Shearing waste polyether sulfone filter membranes, adding the filter membranes into a solution containing a metal compound, adding thiourea, and stirring uniformly to obtain a mixed feed liquid;
(2) Reacting the mixed material liquid for 15 hours at 220 ℃ in a nitrogen atmosphere, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid at 800 ℃ for 1.5h in a nitrogen atmosphere, and taking a reacted solid mixture to obtain the carbon material;
in the step (1), the dosage ratio of the waste polyether sulfone filter membrane, the thiourea and the solution containing the metal compound is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12 percent; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 3.
Example 4
(1) Shearing waste polyether sulfone filter membranes, adding the filter membranes into a solution containing a metal compound, adding thiourea, and stirring uniformly to obtain a mixed feed liquid;
(2) Reacting the mixed material liquid for 10 hours at 250 ℃ in a nitrogen atmosphere, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid at 900 ℃ for 1h in a nitrogen atmosphere, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyether sulfone filter membrane, the thiourea and the solution containing the metal compound in the step (1) is 20g:1g:100mL; in the solution containing the metal compound, the mass concentration of the metal compound is 10 percent; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 4.
Example 5
(1) Shearing waste polyethersulfone filter membranes, adding the filter membranes into a solution containing metal compounds, adding thiourea, and uniformly stirring to obtain a mixed feed liquid;
(2) Reacting the mixed material liquid for 20 hours at 200 ℃ in a nitrogen atmosphere, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid at 700 ℃ for 2h in a nitrogen atmosphere, and taking a solid mixture after the reaction to obtain the carbon material;
in the step (1), the dosage ratio of the waste polyether sulfone filter membrane, the thiourea and the solution containing the metal compound is 30g:3g:200mL; in the solution containing the metal compound, the mass concentration of the metal compound is 15 percent; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 2.
Example 6
(1) Shearing waste polyether sulfone filter membranes, adding the filter membranes into a solution containing a metal compound, adding thiourea, and stirring uniformly to obtain a mixed feed liquid;
(2) Reacting the mixed feed liquid for 15 hours at 220 ℃ in a nitrogen atmosphere, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid at 800 ℃ for 1.5h in a nitrogen atmosphere, and taking a reacted solid mixture to obtain the carbon material;
in the step (1), the dosage ratio of the waste polyether sulfone filter membrane, the thiourea and the solution containing the metal compound is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12 percent; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 1.
Example 7
(1) Shearing waste polyether sulfone filter membranes, adding the filter membranes into a solution containing a metal compound, adding thiourea, and stirring uniformly to obtain a mixed feed liquid;
(2) Reacting the mixed material liquid for 15 hours at 220 ℃ in a nitrogen atmosphere, filtering after the reaction is finished, and taking a solid;
(3) Reacting the solid at 800 ℃ for 1.5h in a nitrogen atmosphere, and taking a reacted solid mixture to obtain the carbon material;
in the step (1), the dosage ratio of the waste polyether sulfone filter membrane, the thiourea and the solution containing the metal compound is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12 percent; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 1.
Comparative example 1
Shearing waste polyether sulfone filter membranes into pieces, reacting for 1.5 hours at 800 ℃ in a nitrogen atmosphere by adopting a cobalt-nickel metal catalyst, and taking a solid mixture after the reaction to obtain the carbon material;
the carbon materials prepared in examples 1 to 7 and comparative example 1 were uniformly mixed with carbon black and binder PVDF 5 in a mass ratio of 90. Uniformly mixing graphene, carbon black and a binder PVDF according to a mass ratio of 90. The positive plate and the negative plate are adopted to form a super capacitor, and the specific capacity retention rate (service life) after 50000 cycles are tested; the test results are shown in Table 1.
Table 1.
| Specific capacity (F/g) | Specific capacity retention (%) | |
| Example 1 the resulting carbon Material | 151F/g | 84％ |
| Example 2 the resulting carbon Material | 133F/g | 76％ |
| Example 3 the resulting carbon Material | 228F/g | 97％ |
| Example 4 the resulting carbon Material | 204F/g | 94％ |
| Example 5 the resulting carbon Material | 187F/g | 90％ |
| Example 6 carbon Material | 139F/g | 80％ |
| Example 7 the resulting carbon Material | 147F/g | 82％ |
| Carbon material prepared in comparative example 1 | 98F/g | 62％ |
As can be seen from the experimental data in table 1, when the carbon materials prepared in examples 1 and 2 are used as the negative electrode material in the super capacitor, the specific capacitance and specific capacity retention rate are significantly higher than those of the carbon material prepared in comparative example 1; this indicates that: the carbon material prepared by the method is applied to the super capacitor, and compared with the carbon material prepared by the conventional high-temperature catalytic reaction, the carbon material prepared by the method has the advantages that the specific capacity of the super capacitor can be obviously improved, and the service life of the super capacitor is prolonged.
As can be seen from the experimental data in Table 1, the specific capacitance and the specific capacity retention rate of the carbon materials prepared in examples 3 to 5 applied to the supercapacitor as the negative electrode material are far higher than those of the carbon material prepared in comparative example 1 and the carbon materials prepared in examples 1 and 2. This indicates that: in the method, the selection of the metal compound is very critical, and the carbon material prepared by different metal compounds is different in the improvement degree of the specific capacity and the service life of the super capacitor; when the metal compound consists of cobalt acetate and nickel acetate, the specific capacity and the service life of the supercapacitor of the prepared carbon material are greatly improved compared with the carbon material prepared by selecting cobalt acetate or nickel acetate as the metal compound; the metal compound is a carbon material prepared from cobalt acetate and nickel acetate, so that the specific capacity of the supercapacitor can be synergistically improved, and the service life of the supercapacitor can be prolonged.
As can be seen from the experimental data in table 1, when the carbon materials prepared in examples 6 and 7 are used as the negative electrode material in the supercapacitor, the specific capacitance and the specific capacity retention rate are not higher than those of the carbon materials prepared in examples 1 or 2; much smaller than the carbon materials prepared in examples 3-5; this indicates that: the dosage ratio of the cobalt acetate to the nickel acetate plays a decisive role in synergistically improving the specific capacity and the service life of the supercapacitor of the prepared carbon material. The specific capacity and the service life of the supercapacitor can be synergistically improved only when the weight ratio of cobalt acetate to nickel acetate is 2-4; the carbon material prepared from cobalt acetate and nickel acetate in other weight ratios cannot synergistically improve the specific capacity and the service life of the supercapacitor.
Claims (10)
1. A method for preparing a carbon material by taking a waste filter membrane as a raw material is characterized by comprising the following steps:
(1) Cutting waste filter membranes into pieces, adding the pieces into a solution containing a metal compound, adding a vulcanization accelerator, and uniformly stirring to obtain a mixed feed liquid;
(2) Reacting the mixed material liquid for 10-20 h at 200-250 ℃ in nitrogen atmosphere, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 700-900 ℃ for 1-2 h, and taking the reacted solid mixture to obtain the carbon material.
2. The method for preparing a carbon material using a waste filter membrane as a raw material according to claim 1, wherein the metal compound in the step (1) is selected from cobalt acetate or nickel acetate.
3. The method for preparing the carbon material using the waste ultrafiltration membrane as the raw material according to claim 2, wherein the metal compound in the step (1) is composed of cobalt acetate and nickel acetate;
wherein the weight ratio of the cobalt acetate to the nickel acetate is 2-4;
most preferably, the weight ratio of cobalt acetate to nickel acetate is 3.
4. The method for preparing a carbon material from the waste filter membrane as claimed in claim 1, wherein the mass concentration of the metal compound in the solution containing the metal compound in the step (1) is 10 to 15%;
most preferably, the mass concentration of the metal compound is 12%.
5. The method for preparing a carbon material using a waste filter membrane as a raw material according to claim 1,
in the step (1), the dosage ratio of the waste filter membrane, the vulcanization accelerator and the solution containing the metal compound is 20-40 g: 1-3 g: 100-200 mL;
most preferably, in the step (1), the ratio of the amount of the waste filter membrane, the vulcanization accelerator and the solution containing the metal compound is 30g:2g:150mL.
6. The method for preparing a carbon material using a waste filter membrane as a raw material according to claim 1, wherein the vulcanization accelerator in the step (1) is thiourea.
7. The method for preparing a carbon material using a waste filter membrane as a raw material as claimed in claim 1, wherein the mixed solution is reacted at 220 ℃ for 15 hours in the nitrogen atmosphere in the step (2).
8. The method for preparing the carbon material using the waste filter membrane as the raw material as set forth in claim 1, wherein the solid mixture is reacted at 800 ℃ for 1.5 hours in a nitrogen atmosphere in the step (3).
9. Use of the carbon material prepared by the method of any one of claims 1 to 8 in the preparation of a capacitor.
10. The use according to claim 9, wherein the capacitor is a supercapacitor.
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