CN114452985B - CuSbS for photocatalytic carbon dioxide2Method for preparing nano tube material - Google Patents
CuSbS for photocatalytic carbon dioxide2Method for preparing nano tube material Download PDFInfo
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- CN114452985B CN114452985B CN202210132361.6A CN202210132361A CN114452985B CN 114452985 B CN114452985 B CN 114452985B CN 202210132361 A CN202210132361 A CN 202210132361A CN 114452985 B CN114452985 B CN 114452985B
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- diphenyl disulfide
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- 239000002071 nanotube Substances 0.000 title claims abstract description 21
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title 1
- 229910052799 carbon Inorganic materials 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- GUUVPOWQJOLRAS-UHFFFAOYSA-N Diphenyl disulfide Chemical compound C=1C=CC=CC=1SSC1=CC=CC=C1 GUUVPOWQJOLRAS-UHFFFAOYSA-N 0.000 claims abstract description 24
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 11
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 9
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims abstract description 8
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000002135 nanosheet Substances 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000000354 decomposition reaction 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
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002073 fluorescence micrograph Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- 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
- C01B32/40—Carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
Abstract
The invention discloses a preparation method of a CuSbS 2 nano-tube material for photocatalytic carbon dioxide, which comprises the following steps: dissolving copper acetate and diphenyl disulfide in a solvent A to prepare a solution A; step two: dissolving antimony trichloride and diphenyl disulfide in a solvent B to prepare a solution B; step three: mixing the solution A and the solution B, adding polyvinylpyrrolidone, mixing and stirring; step four: heating to 180 ℃, reacting for 24-48 hours, washing with water and alcohol, and centrifuging to obtain the nanotube. The nano tube prepared by the invention has the function of decomposing carbon dioxide by photocatalysis, has simple raw materials and relatively convenient reaction process, can be synthesized on a large scale, and has better photocatalysis capability compared with nano sheets.
Description
Technical Field
The invention relates to the field of environmental protection, in particular to a preparation method of a CuSbS 2 nano-tube material for photocatalytic carbon dioxide.
Background
With the development of the age, the energy crisis and the environmental pollution have been delayed, especially the emission of carbon dioxide can cause greenhouse effect, the prior art has been a major research topic, in which carbon dioxide is mainly decomposed into methane and carbon monoxide by photocatalysis of nano-sheets, but it is known that nano-sheets are sheet-shaped materials, the contact area is inferior to that of nanotube materials, and the conversion efficiency is not high.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of a CuSbS 2 nano-tube material for photocatalytic carbon dioxide.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation method of CuSbS 2 nano-tube material for photocatalysis of carbon dioxide,
Comprising
Step one: dissolving copper acetate and diphenyl disulfide in a solvent A to prepare a solution A;
step two: dissolving antimony trichloride and diphenyl disulfide in a solvent B to prepare a solution B;
Step three: mixing the solution A and the solution B, adding polyvinylpyrrolidone, mixing and stirring;
Step four: heating to 180 ℃, reacting for 24-48 hours, washing with water and alcohol, and centrifuging to obtain the nanotube.
As a further improvement of the present invention,
In the first step, the molar ratio of the copper acetate to the diphenyl disulfide is 1:1.
As a further improvement of the present invention,
In the first step, the solvent A is ethanol, and the dosage of the solvent A is 20ml of ethanol for each 1mmol of copper acetate.
As a further improvement of the present invention,
In the second step, the molar ratio of the antimony trichloride to the diphenyl disulfide is 1:1.
As a further improvement of the present invention,
In the second step, the dissolved B is ethanol, and 10ml of ethanol is used for each 1mmol of antimony trichloride.
As a further improvement of the present invention,
In the third step, the molecular weight of polyvinylpyrrolidone is 1300000.
As a further improvement of the present invention,
And in the third step, mixing and stirring time is 30min.
The nano tube prepared by the invention has the function of decomposing carbon dioxide by photocatalysis, has simple raw materials and relatively convenient reaction process, can be synthesized on a large scale, and has better photocatalysis capability compared with nano sheets.
Drawings
FIG. 1 is a 5 μm metric scanning electron microscope image of an embodiment of the present invention;
FIG. 2 is a diagram of a 4 μm metric scanning electron microscope in accordance with an embodiment of the present invention;
FIG. 3 is a 3 μm metric scanning electron microscope image of an embodiment of the present invention;
FIG. 4 is a2 μm metric scanning electron microscope image of an embodiment of the present invention;
FIG. 5 is an XED pattern of an embodiment of the present invention;
FIG. 6 is a graph of diffuse reflection of ultraviolet light in accordance with an embodiment of the present invention;
FIG. 7 is a fluorescence image of an embodiment of the present invention;
FIG. 8 is a graph of carbon monoxide production in accordance with an embodiment of the present invention;
fig. 9 is a graph of methane production for an embodiment of the present invention.
Detailed Description
The invention will be further described in detail with reference to examples of embodiments shown in the drawings.
As shown with reference to figures 1 to 9,
Examples:
step one: 1mmol of copper acetate and 1mmol of diphenyl disulfide are dissolved in 20ml of ethanol to prepare a solution A;
step two: 1mmol of antimony trichloride and 1mmo of diphenyl disulfide are dissolved in 10ml of ethanol to prepare a solution B;
step three: mixing the solution A and the solution B, adding polyvinylpyrrolidone (PVP-1300000), mixing and stirring;
Step four: heating to 180 ℃, reacting for 36 hours, respectively cleaning three times by deionized water and ethanol, and centrifuging to obtain the nanotube.
Test one: obtaining a scanning electron microscope image of the nano tube prepared in the embodiment through a scanning electron microscope; (as shown in figures 1 to 4); the material prepared by the invention is illustrated to be in a nanotube state.
And II, testing: XRD testing of the nanotubes prepared in the examples is carried out, and the chart of FIG. 5 shows that the obtained product is CuSbS 2.
And (3) testing: the ultraviolet diffuse reflection diagram is obtained by passing the nano tube prepared in the embodiment through a spectrometer, and as shown in fig. 6, the nano tube prepared by the invention has higher light absorption intensity and can be beneficial to enhancing the photocatalysis performance;
And (4) testing: the nanotubes prepared in the examples were passed through a fluorescence detector to obtain a fluorescence map, and as shown in fig. 7, the stronger fluorescence means that the more photogenerated carriers, the higher photocatalytic efficiency was caused.
Test five:
10mg of the sample of the example was dispersed in 22ml of a mixed solution of water and triethanolamine (volume ratio 10:1), respectively. Placing the mixture into a photocatalytic reaction container for continuous stirring after ultrasonic treatment for 1min, and repeatedly vacuumizing the container tank for 3 times by using a pump until the reaction system is in an ideal state without gas. And then introducing CO2 gas with atmospheric pressure, continuously irradiating for 6 hours by using a 300W xenon lamp, keeping the temperature of circulating cooling water at 15 ℃, feeding the gas in a 1ml reaction tank into gas chromatograph through an automatic sampler every 2 hours, detecting the gas chromatograph on line in real time, judging the reaction product and the production according to the peak outlet position and the peak outlet area, and as shown in fig. 8 and 9, respectively producing carbon monoxide and methane, wherein the carbon monoxide and the methane are produced with the passage of time. In the prior art, china patent No. 202011242716 discloses a preparation method and application of a CuSbS2/SnS2 nano-sheet composite material, wherein the preparation of CuSbS 2 nano-sheets and the photocatalysis effect of the CuSbS 2 nano-sheets are recorded in the embodiment, the 6-hour CO generation amount is 10 mu mol g < -1 >, the 6-hour methane generation amount is 25 mu mol g < -1 >, and the 6-hour CO generation amount is 15 mu mol g < -1 >, and the 6-hour methane generation amount is 43 mu mol g < -1 >; compared with CuSbS 2, the decomposition capacity of the nano-sheet is obviously improved, so that the nano-tube has better photocatalysis capacity compared with the nano-sheet.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (1)
1. A preparation method of a CuSbS 2 nano-tube material for photocatalytic carbon dioxide is characterized by comprising the following steps:
Comprising
Step one: dissolving copper acetate and diphenyl disulfide in a solvent A to prepare a solution A;
step two: dissolving antimony trichloride and diphenyl disulfide in a solvent B to prepare a solution B;
Step three: mixing the solution A and the solution B, adding polyvinylpyrrolidone, mixing and stirring;
step four: heating to 180 ℃, reacting for 24-48 hours, washing with water and alcohol, and centrifuging to obtain the nanotube;
in the first step, the molar ratio of the copper acetate to the diphenyl disulfide is 1:1;
In the first step, the solvent A is ethanol, and the dosage is 20ml of ethanol for each 1mmol of copper acetate;
in the second step, the molar ratio of the antimony trichloride to the diphenyl disulfide is 1:1;
In the second step, dissolving B into ethanol, wherein 10ml of ethanol is used for each 1mmol of antimony trichloride;
The molecular weight of polyvinylpyrrolidone in the step three is 1300000;
and in the third step, mixing and stirring time is 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210132361.6A CN114452985B (en) | 2022-02-14 | 2022-02-14 | CuSbS for photocatalytic carbon dioxide2Method for preparing nano tube material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210132361.6A CN114452985B (en) | 2022-02-14 | 2022-02-14 | CuSbS for photocatalytic carbon dioxide2Method for preparing nano tube material |
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| Publication Number | Publication Date |
|---|---|
| CN114452985A CN114452985A (en) | 2022-05-10 |
| CN114452985B true CN114452985B (en) | 2024-04-19 |
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| CN202210132361.6A Active CN114452985B (en) | 2022-02-14 | 2022-02-14 | CuSbS for photocatalytic carbon dioxide2Method for preparing nano tube material |
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| CN (1) | CN114452985B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482687A (en) * | 2013-09-27 | 2014-01-01 | 电子科技大学 | Preparation method for CZTS nano-particle material |
| CN110092418A (en) * | 2019-06-10 | 2019-08-06 | 重庆文理学院 | A kind of preparation method of the copper-based sulfide semiconductor nano material of ternary |
| CN110203971A (en) * | 2019-05-10 | 2019-09-06 | 金陵科技学院 | A kind of CuSbS2Nano particle and preparation method thereof, application |
| WO2021008210A1 (en) * | 2019-07-18 | 2021-01-21 | 陕西科技大学 | Method for preparing zn0.2cd0.8s/rgo photocatalytic material |
| CN112354546A (en) * | 2020-11-09 | 2021-02-12 | 绍兴文理学院 | CuSbS2/SnS2Preparation method and application of nanosheet composite material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015046876A2 (en) * | 2013-09-30 | 2015-04-02 | 재단법인대구경북과학기술원 | Solar cell having three-dimensional p-n junction structure and method for manufacturing same |
| CN110624576A (en) * | 2019-10-14 | 2019-12-31 | 哈尔滨师范大学 | Preparation method of BiOCl photocatalyst with super-strong degradation effect |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482687A (en) * | 2013-09-27 | 2014-01-01 | 电子科技大学 | Preparation method for CZTS nano-particle material |
| CN110203971A (en) * | 2019-05-10 | 2019-09-06 | 金陵科技学院 | A kind of CuSbS2Nano particle and preparation method thereof, application |
| CN110092418A (en) * | 2019-06-10 | 2019-08-06 | 重庆文理学院 | A kind of preparation method of the copper-based sulfide semiconductor nano material of ternary |
| WO2021008210A1 (en) * | 2019-07-18 | 2021-01-21 | 陕西科技大学 | Method for preparing zn0.2cd0.8s/rgo photocatalytic material |
| CN112354546A (en) * | 2020-11-09 | 2021-02-12 | 绍兴文理学院 | CuSbS2/SnS2Preparation method and application of nanosheet composite material |
Non-Patent Citations (1)
| Title |
|---|
| Polyvinylpyrrolidone-assisted novel copper antimony sulfide nanorods for highly efficient hydrogen evolution reaction;S. Swathi et al.，;《Fuel》;第314卷;全文 * |
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