CN115707652B - 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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- CN115707652B CN115707652B CN202211367521.1A CN202211367521A CN115707652B CN 115707652 B CN115707652 B CN 115707652B CN 202211367521 A CN202211367521 A CN 202211367521A CN 115707652 B CN115707652 B CN 115707652B
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 82
- 239000012528 membrane Substances 0.000 title claims abstract description 60
- 239000002699 waste material Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002994 raw material Substances 0.000 title claims abstract description 18
- 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
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 20
- 239000008247 solid mixture Substances 0.000 claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- 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
- 239000004695 Polyether sulfone Substances 0.000 claims description 32
- 229920006393 polyether sulfone Polymers 0.000 claims description 32
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 31
- 239000003990 capacitor 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 22
- 229940011182 cobalt acetate Drugs 0.000 claims description 22
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 22
- 229940078494 nickel acetate Drugs 0.000 claims description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 8
- 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 5
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 239000012943 hotmelt Substances 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
Classifications
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- 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 taking 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 waste filter membrane into a solution containing a metal compound, adding a vulcanization accelerator, and uniformly stirring to obtain a mixed material liquid; (2) Reacting the mixed material liquid in nitrogen atmosphere at 200-250 ℃ for 10-20 h, filtering after the reaction is finished, and taking solid; (3) And (3) reacting the solid in a nitrogen atmosphere at 700-900 ℃ for 1-2 h, and taking a solid mixture after the reaction to obtain the carbon material. Compared with the carbon material prepared by adopting the conventional high-temperature catalytic reaction, the carbon material prepared by adopting the method can obviously improve the specific capacity and the service life of the supercapacitor.
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 supercapacitor.
Background
The double-layer capacitor is a super capacitor, is between a battery and a capacitor, is a novel energy storage device, and can be used as a battery with extremely large capacity. Compared with a battery adopting an electrochemical principle, the electric double layer capacitor has the characteristics of short charging time, long service life, good temperature characteristic, energy conservation, environmental protection and the like because the charge and discharge processes of the electric double layer capacitor do not involve material changes at all.
The polyethersulfone filter membrane is a membrane material prepared by hot melt adhesion of polyethersulfone superfine fibers, and belongs to PES membranes for deep filtration; is widely used in industry. Due to the large-scale use in industry, a large amount of waste polyethersulfone filter membranes are generated. However, how to treat the waste polyethersulfone filter membrane is an urgent technical problem to be solved.
The inventor provides a solution for preparing a carbon material by taking a waste polyethersulfone filter membrane as a raw material and carrying out catalytic reaction at high temperature. However, the inventors found in the study that the specific capacity and the service life of the carbon material prepared by adopting the conventional high-temperature catalytic reaction are not high, and the specific capacity and the service life of the carbon material serving as a negative electrode material are required 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 taking 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, which uses the waste polyethersulfone filter membrane as the raw material, can obviously improve the specific capacity and service life of the super capacitor compared with the carbon material prepared by the conventional high-temperature catalytic reaction when applied to the super capacitor.
The technical problems to be solved by the invention are realized by the following technical scheme:
the method for preparing the carbon material by taking the waste filter membrane as the raw material is characterized by comprising the following steps:
(1) Cutting the waste filter membrane, adding the cut waste filter membrane into a solution containing a metal compound, adding a vulcanization accelerator, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in nitrogen atmosphere at 200-250 ℃ for 10-20 h, filtering after the reaction is finished, and taking solid;
(3) And (3) reacting the solid in a nitrogen atmosphere at 700-900 ℃ for 1-2 h, and taking a solid mixture after the reaction 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; a great number of experiments show 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 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 that the selection of the metal compounds is very critical in the research, and the carbon materials prepared by selecting different metal compounds have different improvements on the specific capacity and the service life of the super capacitor. The inventor has shown through a great deal of experimental study that the carbon material prepared when the metal compound is cobalt acetate or nickel acetate is applied to the super capacitor, 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 adopting 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 2-4:1;
most preferably, the weight ratio of cobalt acetate to nickel acetate is 3:1.
The inventor has surprisingly found in further research that by adopting the method of the invention, the specific capacity and the service life of the super capacitor can be synergistically improved by the carbon material prepared when the metal compound consists of cobalt acetate and nickel acetate; the specific capacity and the service life of the super capacitor are improved to a degree which is greatly higher than that of a carbon material prepared by using cobalt acetate or nickel acetate as a metal compound.
Preferably, 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%.
Preferably, in the step (1), the amount ratio of the waste filter membrane, the vulcanization accelerator and the metal compound-containing solution is 20 to 40g: 1-3 g: 100-200 mL.
Most preferably, in the step (1), the amount ratio of the waste filter membrane, the vulcanization accelerator and the metal compound-containing solution is 30g:2g:150mL.
Preferably, the vulcanization accelerator in step (1) is thiourea.
Preferably, in the step (2), the mixed solution is reacted at 220 ℃ for 15 hours in a nitrogen atmosphere.
Preferably, in step (3), the solid mixture is reacted at 800 ℃ for 1.5h under nitrogen atmosphere.
The invention also provides an application of the carbon material prepared by the method in preparation of the capacitor.
Preferably, the capacitor is a super capacitor.
The beneficial effects are 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 of the invention, which uses the waste polyethersulfone filter membrane as the raw material, can obviously improve the specific capacity and service life of the super capacitor compared with the carbon material prepared by the conventional high-temperature catalytic reaction when applied to 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) Cutting the waste polyethersulfone filter membrane, adding the cut waste polyethersulfone filter membrane into a solution containing a metal compound, adding thiourea, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in a nitrogen atmosphere at 220 ℃ for 15 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 800 ℃ for 1.5 hours, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyethersulfone filter membrane, thiourea and the solution containing the metal compound in the step (1) 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) Cutting the waste polyethersulfone filter membrane, adding the cut waste polyethersulfone filter membrane into a solution containing a metal compound, adding thiourea, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in a nitrogen atmosphere at 220 ℃ for 15 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 800 ℃ for 1.5 hours, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyethersulfone filter membrane, thiourea and the solution containing the metal compound in the step (1) is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12%; the metal compound is nickel acetate.
Example 3
(1) Cutting the waste polyethersulfone filter membrane, adding the cut waste polyethersulfone filter membrane into a solution containing a metal compound, adding thiourea, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in a nitrogen atmosphere at 220 ℃ for 15 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 800 ℃ for 1.5 hours, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyethersulfone filter membrane, thiourea and the solution containing the metal compound in the step (1) is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12%; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 3:1.
Example 4
(1) Cutting the waste polyethersulfone filter membrane, adding the cut waste polyethersulfone filter membrane into a solution containing a metal compound, adding thiourea, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in nitrogen atmosphere at 250 ℃ for 10 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 900 ℃ for 1h, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyethersulfone filter membrane, 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%; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 4:1.
Example 5
(1) Cutting the waste polyethersulfone filter membrane, adding the cut waste polyethersulfone filter membrane into a solution containing a metal compound, adding thiourea, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in nitrogen atmosphere at 200 ℃ for 20 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 700 ℃ for 2 hours, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyethersulfone filter membrane, thiourea and the solution containing the metal compound in the step (1) is 30g:3g:200mL; in the solution containing the metal compound, the mass concentration of the metal compound is 15%; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 2:1.
Example 6
(1) Cutting the waste polyethersulfone filter membrane, adding the cut waste polyethersulfone filter membrane into a solution containing a metal compound, adding thiourea, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in a nitrogen atmosphere at 220 ℃ for 15 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 800 ℃ for 1.5 hours, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyethersulfone filter membrane, thiourea and the solution containing the metal compound in the step (1) is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12%; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 1:3.
Example 7
(1) Cutting the waste polyethersulfone filter membrane, adding the cut waste polyethersulfone filter membrane into a solution containing a metal compound, adding thiourea, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in a nitrogen atmosphere at 220 ℃ for 15 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in nitrogen atmosphere at 800 ℃ for 1.5 hours, and taking a solid mixture after the reaction to obtain the carbon material;
the dosage ratio of the waste polyethersulfone filter membrane, thiourea and the solution containing the metal compound in the step (1) is 30g:2g:150mL; in the solution containing the metal compound, the mass concentration of the metal compound is 12%; the metal compound consists of cobalt acetate and nickel acetate in a weight ratio of 1:1.
Comparative example 1
Cutting waste polyethersulfone filter membrane, reacting for 1.5 hours at 800 ℃ in nitrogen atmosphere by adopting 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 a binder PVDF as a negative electrode material in a mass ratio of 90:5:5, respectively, to prepare a negative electrode sheet. And uniformly mixing graphene and carbon black and a binder PVDF according to a mass ratio of 90:5:5 to obtain a positive electrode plate. The positive plate and the negative plate are adopted to form a super capacitor, and the specific capacity retention rate (service life) after 50000 times of circulation are tested; the test results are shown in Table 1.
Table 1.
| Specific capacity (F/g) | Specific capacity retention (%) | |
| Carbon Material prepared in example 1 | 151F/g | 84％ |
| Example 2 carbon Material | 133F/g | 76％ |
| Example 3 carbon Material | 228F/g | 97％ |
| Example 4 carbon Material | 204F/g | 94％ |
| Example 5 carbon Material | 187F/g | 90％ |
| Example 6 carbon Material | 139F/g | 80％ |
| Example 7 carbon Material | 147F/g | 82％ |
| Comparative example 1 carbon Material | 98F/g | 62％ |
As can be seen from the experimental data in table 1, the carbon materials prepared in examples 1 and 2 are used as negative electrode materials in super capacitors, and the specific capacitance and specific capacity retention rate of the carbon materials are significantly higher than those of the carbon materials prepared in comparative example 1; this illustrates: 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 carbon material prepared by adopting the method can remarkably improve the specific capacity and the service life of the super capacitor.
As can be seen from the experimental data in table 1, the carbon materials prepared in examples 3 to 5 were used as negative electrode materials in super capacitors, and the specific capacitance and specific capacity retention rate were much higher than those of the carbon material prepared in comparative example 1 and much higher than those of the carbon materials prepared in examples 1 and 2. This illustrates: in the method, the selection of the metal compounds is very critical, and the carbon materials prepared by selecting different metal compounds have different improvement degrees on the specific capacity and the service life of the super capacitor; the specific capacity and the service life of the carbon material prepared when the metal compound consists of cobalt acetate and nickel acetate are greatly improved compared with those of the carbon material prepared by using 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 and the service life of the supercapacitor can be synergistically improved.
As can be seen from the experimental data in table 1, the carbon materials prepared in examples 6 and 7 are used as negative electrode materials in super capacitors, and the specific capacitance and specific capacity retention rate are not higher than those of the carbon materials prepared in examples 1 or 2; far less than the carbon materials prepared in examples 3-5; this illustrates: the dosage ratio of cobalt acetate to nickel acetate plays a decisive role in synergistically improving the specific capacity and the service life of the supercapacitor for the prepared carbon material. Only when the weight ratio of the cobalt acetate to the nickel acetate is 2-4:1, the prepared carbon material can synergistically improve the specific capacity and the service life of the supercapacitor; 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 (9)
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 of
The steps are as follows:
(1) Cutting the waste filter membrane, adding the cut waste filter membrane into a solution containing a metal compound, adding a vulcanization accelerator, and uniformly stirring to obtain a mixed material liquid;
(2) Reacting the mixed material liquid in a nitrogen atmosphere at 200-250 ℃ for 10-20 hours, filtering after the reaction is finished, and taking solid;
(3) Reacting the solid in a nitrogen atmosphere at 700-900 ℃ for 1-2 hours, and taking a solid mixture after the reaction to obtain the carbon material;
the metal compound in the step (1) consists of cobalt acetate and nickel acetate; wherein the weight ratio of the cobalt acetate to the nickel acetate is 2-4:1;
the vulcanization accelerator in the step (1) is thiourea;
in the step (1), the using amount 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;
the waste filter membrane is a waste polyethersulfone filter membrane.
2. The method for preparing carbon material by using waste ultrafiltration membrane as raw material according to claim 1, wherein the method comprises the following steps of
The weight ratio of the cobalt acetate to the nickel acetate is 3:1.
3. The method for preparing a carbon material by using a waste filter membrane as a raw material according to claim 1, wherein the mass concentration of the metal compound in the solution containing the metal compound in the step (1) is 10-15%.
4. The method for producing a carbon material using a waste filter membrane as a raw material according to claim 3, wherein the mass concentration of the metal compound in the solution containing the metal compound in the step (1) is 12%.
5. The method for producing a carbon material using a waste filter membrane as a raw material according to claim 1, wherein in the step (1), the ratio of the amount of the waste filter membrane, the vulcanization accelerator to the metal compound-containing solution is 30g:2g:150mL.
6. The method for producing a carbon material from a waste filter membrane according to claim 1, wherein in the step (2), the mixed solution is reacted at 220 ℃ for 15 hours in a nitrogen atmosphere.
7. The method for producing a carbon material using a waste filter membrane as a raw material according to claim 1, wherein in the step (3), the solid mixture is reacted at 800 ℃ for 1.5 hours in a nitrogen atmosphere.
8. The use of the carbon material prepared by the method of any one of claims 1 to 7 in the preparation of capacitors.
9. The use of claim 8, wherein the capacitor is a supercapacitor.
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