CN109817941A - A kind of high capacity high efficiency sulphur/graphene composite material and preparation method thereof - Google Patents
A kind of high capacity high efficiency sulphur/graphene composite material and preparation method thereof Download PDFInfo
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- CN109817941A CN109817941A CN201910120151.3A CN201910120151A CN109817941A CN 109817941 A CN109817941 A CN 109817941A CN 201910120151 A CN201910120151 A CN 201910120151A CN 109817941 A CN109817941 A CN 109817941A
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of preparation method of high capacity high efficiency sulphur/graphene composite material, includes the following steps: that (1) prepares mixed solution A；(2) evenly dispersed silicon suspension is prepared；(3) mixed solution B is prepared；(4) hypo solution is configured；(5) mixed solution B that step 3 obtains, organic acid are added to organic solvent, sonic oscillation 2-10h obtains mixed solution C；(6) hypo solution that step 4 obtains and the mixed solution C that step 5 obtains are mixed, it at the uniform velocity stirs, in 25-100 DEG C of reflux 2-10h, then pours into initiator, stirring is stood, filtering, vacuum drying, obtains high capacity high efficiency sulphur/graphene composite material.A kind of preparation method of high capacity high efficiency sulphur/graphene composite material has high, high-efficient, good cycle the characteristic of capacity.
Description
Technical field
The present invention relates to a kind of preparation methods of composite material, and in particular to a kind of high capacity high efficiency sulphur/graphene is multiple
Condensation material and preparation method thereof.
Background technique
Main problem existing for China's current battery industry is environmental pollution and serious waste of resources, lithium ion battery conduct
A kind of novel energy-storing tool, energy density is high, and output power, self discharge is small, and cycle performance is superior, and operating temperature range is wide,
Region of discharge is steady, and volume utilization is high, is just gradually applied to multiple fields as green battery, becomes one of fungible energy source.
Based on the research to anode material for lithium-ion batteries, carbon material is concerned at present, but its capacity is lower, can not be solved
Certainly larger amount of problems of energy consumption.And graphene is as emerging carbon material and biggish electron mobility, world resistivity
Minimum, stability are good by favor.But due to attraction strong between graphene sheet layer, cause solid graphene due to
Assemble and loses monodisperse graphene with excellent properties such as high specific areas.
Come in, using the volumetric properties that the elemental sulfur with special construction is excellent, extensive source becomes the features such as cheap
As anode material for lithium-ion batteries by extensive concern, but it intrinsic electric conductivity is poor limits its application, and will affect
Electrode reaction in secondary cell, the variation of elemental sulfur own vol greatly affects its stable circulation in charge and discharge process
Property.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of high capacity high efficiency sulphur/graphene composite material, have
High, high-efficient, good cycle the characteristic of capacity.
In order to achieve the above-mentioned object of the invention, the technical scheme is that a kind of high capacity high efficiency sulphur/graphene is compound
The preparation method of material, includes the following steps:
(1) graphene powder, carbon nanotube are added in N-Methyl pyrrolidone, obtain mixed solution A；
(2) ethyl alcohol and distilled water are mixed to get mixed solvent, nano-silicon powder, ultrasonic 1- is added in the mixed solvent
3h obtains evenly dispersed silicon suspension；
(3) it being added in the mixed solution A that step 1 obtains into the silicon suspension that step 2 obtains, room temperature magnetic stirs 8-12h,
Obtain mixed solution B；
(4) sodium thiosulfate is mixed in deionized water, configures hypo solution；
(5) mixed solution B that step 3 obtains, organic acid are added to organic solvent, sonic oscillation 2-10h is mixed
Solution C；
(6) hypo solution that step 4 obtains and the mixed solution C that step 5 obtains are mixed, is at the uniform velocity stirred,
25-100 DEG C of reflux 2-10h, then initiator is poured into, stirring is stood, filtering, vacuum drying, obtains high capacity high efficiency sulphur/stone
Black alkene composite material.
Preferably, in step 1, graphene powder, carbon nanotube, N-Methyl pyrrolidone mass ratio be 5-8:3-6:
20-30。
Preferably, in step 2, ethyl alcohol, distilled water, nano-silicon powder mass ratio be 10-20:15-25:2-6.
Preferably, in step 3, silicon suspension, mixed solution A mass ratio be 8-12:30-40.
Preferably, in step 4, sodium thiosulfate, deionized water mass ratio be 2-6:10-20.
Preferably, in step 5, mixed solution B, organic acid, organic solvent mass ratio be 10-20:1-4:20-30.
Preferably, in step 6, hypo solution, mixed solution C, initiator, mass ratio be 8-12:30-40:
1-3。
Preferably, in step 5, organic acid is one of oxalic acid, dichloroacetic acid, trichloroacetic acid, gluconic acid, You Jirong
Agent is one of tetrahydrofuran, acetone, butanone.
The invention has the following advantages: a kind of preparation method of high capacity high efficiency sulphur/graphene composite material, tool
There is high, high-efficient, good cycle the characteristic of capacity；Graphene, carbon nanotube, nano-silicon powder progress is compound, not only may be used
To improve conductivity, cyclical stability can also be improved；Sodium thiosulfate and organic acid reaction rate easily pass through reaction temperature
The mass ratio of regulation or sodium thiosulfate and organic acid regulates and controls.
Specific embodiment
Embodiment 1
A kind of preparation method of high capacity high efficiency sulphur/graphene composite material, includes the following steps:
(1) graphene powder, carbon nanotube are added in N-Methyl pyrrolidone, obtain mixed solution A；Graphene powder
End, carbon nanotube, N-Methyl pyrrolidone mass ratio be 5:3:20；
(2) ethyl alcohol and distilled water are mixed to get mixed solvent, in the mixed solvent be added nano-silicon powder, ultrasonic 1h,
Obtain evenly dispersed silicon suspension；Ethyl alcohol, distilled water, nano-silicon powder mass ratio be 10:15:2；
(3) it is added in the mixed solution A that step 1 obtains into the silicon suspension that step 2 obtains, room temperature magnetic stirs 8h, obtains
To mixed solution B；Silicon suspension, mixed solution A mass ratio be 8:30；
(4) sodium thiosulfate is mixed in deionized water, configures hypo solution；Sodium thiosulfate, deionized water
Mass ratio be 2:10；
(5) mixed solution B that step 3 obtains, oxalic acid are added to tetrahydrofuran, sonic oscillation 2h obtains mixed solution
C；Mixed solution B, oxalic acid, tetrahydrofuran mass ratio be 10:1:20；
(6) hypo solution that step 4 obtains and the mixed solution C that step 5 obtains are mixed, is at the uniform velocity stirred,
25 DEG C of reflux 2h, then initiator is poured into, stirring is stood, filtering, vacuum drying, and it is compound to obtain high capacity high efficiency sulphur/graphene
Material；Hypo solution, mixed solution C, initiator, mass ratio be 8:30:1.
Embodiment 2
A kind of preparation method of high capacity high efficiency sulphur/graphene composite material, includes the following steps:
(1) graphene powder, carbon nanotube are added in N-Methyl pyrrolidone, obtain mixed solution A；Graphene powder
End, carbon nanotube, N-Methyl pyrrolidone mass ratio be 8:6:30；
(2) ethyl alcohol and distilled water are mixed to get mixed solvent, in the mixed solvent be added nano-silicon powder, ultrasonic 3h,
Obtain evenly dispersed silicon suspension；Ethyl alcohol, distilled water, nano-silicon powder mass ratio be 20:25:6；
(3) it is added in the mixed solution A that step 1 obtains into the silicon suspension that step 2 obtains, room temperature magnetic stirs 12h, obtains
To mixed solution B；Silicon suspension, mixed solution A mass ratio be 12:40；
(4) sodium thiosulfate is mixed in deionized water, configures hypo solution；Sodium thiosulfate, deionized water
Mass ratio be 6:20；
(5) mixed solution B that step 3 obtains, dichloroacetic acid are added to acetone, sonic oscillation 10h obtains mixed solution
C；Mixed solution B, dichloroacetic acid, acetone mass ratio be 20:4:30；
(6) hypo solution that step 4 obtains and the mixed solution C that step 5 obtains are mixed, is at the uniform velocity stirred,
100 DEG C of reflux 10h, then initiator is poured into, stirring is stood, filtering, vacuum drying, and it is multiple to obtain high capacity high efficiency sulphur/graphene
Condensation material；Hypo solution, mixed solution C, initiator, mass ratio be 12:40:3.
Embodiment 3
A kind of preparation method of high capacity high efficiency sulphur/graphene composite material, includes the following steps:
(1) graphene powder, carbon nanotube are added in N-Methyl pyrrolidone, obtain mixed solution A；Graphene powder
End, carbon nanotube, N-Methyl pyrrolidone mass ratio be 6:4:25；
(2) ethyl alcohol and distilled water are mixed to get mixed solvent, in the mixed solvent be added nano-silicon powder, ultrasonic 2h,
Obtain evenly dispersed silicon suspension；Ethyl alcohol, distilled water, nano-silicon powder mass ratio be 15:20:4；
(3) it is added in the mixed solution A that step 1 obtains into the silicon suspension that step 2 obtains, room temperature magnetic stirs 9h, obtains
To mixed solution B；Silicon suspension, mixed solution A mass ratio be 10:35；
(4) sodium thiosulfate is mixed in deionized water, configures hypo solution；Sodium thiosulfate, deionized water
Mass ratio be 4:15；
(5) mixed solution B that step 3 obtains, trichloroacetic acid are added to butanone, sonic oscillation 5h obtains mixed solution
C；Mixed solution B, trichloroacetic acid, butanone mass ratio be 15:2:30；
(6) hypo solution that step 4 obtains and the mixed solution C that step 5 obtains are mixed, is at the uniform velocity stirred,
40 DEG C of reflux 5h, then initiator is poured into, stirring is stood, filtering, vacuum drying, and it is compound to obtain high capacity high efficiency sulphur/graphene
Material；Hypo solution, mixed solution C, initiator, mass ratio be 10:35:2.
Embodiment 4
A kind of preparation method of high capacity high efficiency sulphur/graphene composite material, includes the following steps:
(1) graphene powder, carbon nanotube are added in N-Methyl pyrrolidone, obtain mixed solution A；Graphene powder
End, carbon nanotube, N-Methyl pyrrolidone mass ratio be 7:5:28；
(2) ethyl alcohol and distilled water are mixed to get mixed solvent, in the mixed solvent be added nano-silicon powder, ultrasonic 2h,
Obtain evenly dispersed silicon suspension；Ethyl alcohol, distilled water, nano-silicon powder mass ratio be 18:22:5；
(3) it is added in the mixed solution A that step 1 obtains into the silicon suspension that step 2 obtains, room temperature magnetic stirs 10h, obtains
To mixed solution B；Silicon suspension, mixed solution A mass ratio be 10:37；
(4) sodium thiosulfate is mixed in deionized water, configures hypo solution；Sodium thiosulfate, deionized water
Mass ratio be 5:18；
(5) mixed solution B that step 3 obtains, gluconic acid are added to tetrahydrofuran, sonic oscillation 8h is mixed
Solution C；Mixed solution B, gluconic acid, tetrahydrofuran mass ratio be 18:3:28；
(6) hypo solution that step 4 obtains and the mixed solution C that step 5 obtains are mixed, is at the uniform velocity stirred,
80 DEG C of reflux 8h, then initiator is poured into, stirring is stood, filtering, vacuum drying, and it is compound to obtain high capacity high efficiency sulphur/graphene
Material；Hypo solution, mixed solution C, initiator, mass ratio be 10:36:2.
Claims (8)
1. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material, which comprises the steps of:
(1) graphene powder, carbon nanotube are added in N-Methyl pyrrolidone, obtain mixed solution A；
(2) ethyl alcohol and distilled water are mixed to get mixed solvent, nano-silicon powder are added in the mixed solvent, ultrasonic 1-3h is obtained
To evenly dispersed silicon suspension；
(3) it is added in the mixed solution A that step 1 obtains into the silicon suspension that step 2 obtains, room temperature magnetic stirs 8-12h, obtains
Mixed solution B；
(4) sodium thiosulfate is mixed in deionized water, configures hypo solution；
(5) mixed solution B that step 3 obtains, organic acid are added to organic solvent, sonic oscillation 2-10h obtains mixed solution
C；
(6) hypo solution that step 4 obtains and the mixed solution C that step 5 obtains are mixed, is at the uniform velocity stirred, in 25-
100 DEG C of reflux 2-10h, then initiator is poured into, stirring is stood, filtering, vacuum drying, obtains high capacity high efficiency sulphur/graphene
Composite material.
2. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material according to claim 1, feature exist
In, in step 1, graphene powder, carbon nanotube, N-Methyl pyrrolidone mass ratio be 5-8:3-6:20-30.
3. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material according to claim 1, feature exist
In, in step 2, ethyl alcohol, distilled water, nano-silicon powder mass ratio be 10-20:15-25:2-6.
4. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material according to claim 1, feature exist
In, in step 3, silicon suspension, mixed solution A mass ratio be 8-12:30-40.
5. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material according to claim 1, feature exist
In, in step 4, sodium thiosulfate, deionized water mass ratio be 2-6:10-20.
6. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material according to claim 1, feature exist
In, in step 5, mixed solution B, organic acid, organic solvent mass ratio be 10-20:1-4:20-30.
7. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material according to claim 1, feature exist
In, in step 6, hypo solution, mixed solution C, initiator, mass ratio be 8-12:30-40:1-3.
8. a kind of preparation method of high capacity high efficiency sulphur/graphene composite material according to claim 1, feature exist
In in step 5, organic acid is one of oxalic acid, dichloroacetic acid, trichloroacetic acid, gluconic acid, and organic solvent is tetrahydro furan
It mutters, one of acetone, butanone.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104600268A (en) * | 2015-01-16 | 2015-05-06 | 中国计量学院 | Method for preparing polyaniline/sulfur/graphene composite material |
| CN105576203A (en) * | 2015-12-23 | 2016-05-11 | 厦门大学 | Graphene/silicone/carbon nano tube composite material and preparation method and application thereof |
| CN107785554A (en) * | 2017-10-26 | 2018-03-09 | 陕西聚洁瀚化工有限公司 | The preparation method of lithium-sulfur cell graphene nano sulphur composite positive pole |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104600268A (en) * | 2015-01-16 | 2015-05-06 | 中国计量学院 | Method for preparing polyaniline/sulfur/graphene composite material |
| CN105576203A (en) * | 2015-12-23 | 2016-05-11 | 厦门大学 | Graphene/silicone/carbon nano tube composite material and preparation method and application thereof |
| CN107785554A (en) * | 2017-10-26 | 2018-03-09 | 陕西聚洁瀚化工有限公司 | The preparation method of lithium-sulfur cell graphene nano sulphur composite positive pole |
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