CN102335616A - Synthesis method of novel visible-light photocatalyst indium sulfide - Google Patents
Synthesis method of novel visible-light photocatalyst indium sulfide Download PDFInfo
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- CN102335616A CN102335616A CN201110205646XA CN201110205646A CN102335616A CN 102335616 A CN102335616 A CN 102335616A CN 201110205646X A CN201110205646X A CN 201110205646XA CN 201110205646 A CN201110205646 A CN 201110205646A CN 102335616 A CN102335616 A CN 102335616A
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- indium sulfide
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- light photocatalyst
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Abstract
The invention relates to a synthesis method of a novel visible-light photocatalyst indium sulfide, belonging to the technical field of preparation of photocatalysts. The method comprises the following steps: weighing indium chloride tetrahydrate, dissolving the indium chloride tetrahydrate in deionized water, adding acetic acid to regulate the pH value to 1-3, and adding thioacetamide solution, wherein the concentration of indium ions is 0.025 mol/L, and the In/S mol ratio is 1:4-1:10; heating the obtained mixed solution to constant temperature so as to carry out hydrothermal reaction for 4-8 hours while regulating the temperature to 80 DEG C, and cooling at room temperature; and carrying out vacuum filtration under reduced pressure, washing, and drying to obtain the orange indium sulfide powder. The indium sulfide prepared by the method provided by the invention is in a ball-flower shape, and has the advantages of large specific area and uniform size; and the indium sulfide powder is in a cubic structure. The indium sulfide can be used as a visible-light photocatalyst, and has good degradation effect on organic dyes (such as methyl orange).
Description
Technical field
The synthetic method of a kind of novel visible photochemical catalyst indium sulfide involved in the present invention belongs to the preparing technical field of photochemical catalyst.
Background technology
Methyl orange is a kind of well-known sulfonic acid azo dyes indicator, is widely used in aspects such as dyeing, food, paper pulp, leather, printing, weaving.In these industry, methyl orange is a kind of common water pollutant, and it is non-harmful material that number of research projects is endeavoured to methyl orange degradation.Biodegradation process seldom is applied in the textile sewage because have poisonous residual dye filler, surfactant and other harmful accrete existence.Advanced photooxidation technology is imperative, and various photochemical catalysts can be used for handling waste water, and photocatalysis is a kind ofly to be different from conventional alternative method and to be studied extensively and profoundly.Organic pollution water treatment in recent years, particularly utilizing solar energy to carry out the organic sewage processing is a very active subject.Photocatalysis is compared with other method for treating water and is had many good qualities, and for example utilizes eco-friendly oxidant oxygen, gentle reaction condition, and normal temperature and pressure just can carry out down, and the organic pollution of low concentration also can be oxidized etc.Titanium dioxide is the high efficiency semiconductor catalyst of one type of extensive use, but it only has activity under ultraviolet light, to not response of the visible light more than 400 nanometers; Visible light is the chief component of sunshine; Also be the major part of indoor light, so titanium dioxide is subject to indoor application, visible light is had the photochemical catalyst of the induction space that grows a lot; Wherein one of achievement is exactly through adding metal or nonmetal titanium dioxide is carried out modification, as mixes vanadium, chromium, nitrogen, carbon, sulphur etc.In general, these photochemical catalysts that mix type still can not have desirable absorption at visible region, or they are unstable in photocatalytic process, active low.
People are devoted to develop new material on the other hand, traditional visible-light photocatalyst or unstable under illumination, and like cadmium sulfide, cadmium selenide etc., or activity is lower under illumination, like tungstic acid and di-iron trioxide etc.Indium sulfide be one non-titania-based, than TiO 2-based catalyst visible-light photocatalyst more efficiently, it can efficiently utilize the energy of solar spectrum; Quantum efficiency is improved greatly; Forefathers report that most of sulfide are very promising visible-light photocatalysts, yet a lot of sulfide issues green anode photoetch, instability in illumination; Bleaching has very high activity to indium sulfide to organic dyestuff under visible light, and the stable in properties reusable edible.
Summary of the invention
The objective of the invention is to deficiency to existing photochemical catalyst; Catalytic activity is low or character is unstable; The method of a simple preparation high activity and stable visible-light photocatalyst is provided, can have produced the photochemical catalyst indium sulfide powder of efficiently taking off dyestuff in the waste water.Its technology is simple, and is with low cost, is suitable for large-scale production and application.
In order to realize this purpose, the present invention adopts inidum chloride, and acetic acid and thioacetamide are raw material, being lower than under 100 ℃ the aqueous environment, has obtained to have cubic structure, and specific area is big, the indium sulfide powder of homogeneous grain size and highly crystalline.
The synthetic method of a kind of novel visible photochemical catalyst indium sulfide of the present invention is characterized in that, may further comprise the steps:
(a) take by weighing four hydration inidum chloride (InCl
34H
2O) be dissolved in the deionized water, adding its pH value of acetic acid adjusting is 1-3, adds thioacetamide (CH then
2CSNH
2) solution, the concentration of indium ion is 0.025mol/L, wherein the ratio of In and S amount of substance is 1: 4-1: 10;
(b) mixed solution that obtains in the step (a) is carried out heated at constant temperature and make it reaction, regulating temperature is 80 ℃, hydro-thermal reaction 4-8 hour, and the room temperature cooling;
(c) decompress filter, washing, drying obtains orange red indium sulfide powder.
Take by weighing 0.10 gram indium sulfide and place 1 * 10
-5In the methyl orange solution of mol/L (absorbance is approximately 1.0), carry out the Photocatalytic Activity for Degradation test.Adopt the German Bruker Advance D-8X of company ray powder diffraction appearance (Cu K α radiation,
) to measure the structure of prepared film.Adopt the microscopic appearance of the prepared film of HitachiS-4800N determination of electron microscopy.Adopt the light source of 500W xenon lamp, adopt optical filter elimination ultraviolet light, utilize fan for cooling to keep catalytic degradation front and back temperature consistent in the catalytic process as photocatalytic degradation methyl orange.
The present invention adopts simple solution methods to prepare efficient stable photochemical catalyst indium sulfide.Utilize method provided by the invention can synthesize high-purity indium sulfide powder, the particle size of this powder is about 3-5 μ m, and granule-morphology is a bouquet shape, and specific area is big, and size is even, and it is big to have specific area, and the indium sulfide powder of gained is a cubic structure.As visible-light photocatalyst, organic dyestuff (like methyl orange) there is good degradation effect, 2.5 hours degradation rates can reach more than 90% in the test of indium sulfide visible light degraded methyl orange.The present invention has technology simple with respect to the production of other method, synthetic advantage easily.
Description of drawings
Fig. 1 is for pressing the XRD figure spectrum of embodiment 1 resulting indium sulfide powder;
Fig. 2 is the stereoscan photograph of the indium sulfide powder that obtains by embodiment 1;
Fig. 3 separates the abosrption spectrogram of methyl orange for the indium sulfide powder visible light irradiation that obtains by embodiment 1 descends;
Fig. 4 is the degradation effect figure of methyl orange (λ max=464nm) under the indium sulfide powder visible light irradiation that obtains by embodiment 1.
The specific embodiment
Further illustrate substantive distinguishing features of the present invention and remarkable advantage through embodiment below, the present invention only is confined to the embodiment that stated by no means.
Embodiment 1
(a) take by weighing four an amount of hydration inidum chloride (InCl
34H
2O) be dissolved in the deionized water, adding its pH value of acetic acid adjusting is 1, adds thioacetamide (CH then
2CSNH
2) solution, the concentration of indium ion is 0.025mol/L, wherein the ratio of In and S amount of substance is 1: 4;
(b) mixed solution that obtains in the step (a) is put into the baking oven heating and make it reaction, regulating temperature is 80 ℃, hydro-thermal reaction 6 hours, room temperature cooling;
(c) decompress filter, washing, drying obtains orange red indium sulfide powder, and the x-ray diffractogram of powder of product is seen Fig. 1.
(d) take by weighing 0.10 gram indium sulfide and place 1 * 10
-5In the methyl orange solution of mol/L (absorbance is approximately 1.0), carry out the Photocatalytic Activity for Degradation test.
Embodiment 2
(a) take by weighing four an amount of hydration inidum chloride (InCl
34H
2O) be dissolved in the deionized water, adding its pH value of acetic acid adjusting is 2, adds thioacetamide (CH then
2CSNH
2) solution, the concentration of indium ion is 0.025mol/L, wherein the ratio of In and S amount of substance is 1: 4;
(b) mixed solution that obtains in the step (a) is put into the baking oven heating and make it reaction, regulating temperature is 80 ℃, hydro-thermal reaction 4 hours, room temperature cooling;
(c) decompress filter, washing, drying obtains orange red indium sulfide powder.
(d) take by weighing 0.10 gram indium sulfide and place 1 * 10
-5In the methyl orange solution of mol/L (absorbance is approximately 1.0), carry out the Photocatalytic Activity for Degradation test.
Embodiment 3
(a) take by weighing four an amount of hydration inidum chloride (InCl
34H
2O) be dissolved in the deionized water, adding its pH value of acetic acid adjusting is 3, adds thioacetamide (CH then
2CSNH
2) solution, the concentration of indium ion is 0.025mol/L, wherein the ratio of In and S amount of substance is 1: 6;
(b) mixed solution that obtains in the step 1 is put into the baking oven heating and make it reaction, regulating temperature is 80 ℃, hydro-thermal reaction 8 hours, room temperature cooling;
(c) decompress filter, washing, drying obtains orange red indium sulfide powder.
(d) take by weighing 0.10 gram indium sulfide and place 1 * 10
-5In the methyl orange solution of mol/L (absorbance is approximately 1.0), carry out the Photocatalytic Activity for Degradation test.
Embodiment 4
(a) take by weighing four an amount of hydration inidum chloride (InCl
34H
2O) be dissolved in the deionized water, adding its pH value of acetic acid adjusting is 3, adds thioacetamide (CH then
2CSNH
2) solution, the concentration of indium ion is 0.025mol/L, wherein the ratio of In and S amount of substance is 1: 10;
(b) mixed solution that obtains in the step (a) is put into the baking oven heating and make it reaction, regulating temperature is 80 ℃, hydro-thermal reaction 6 hours, room temperature cooling;
(c) decompress filter, washing, drying obtains orange red indium sulfide powder.
(d) take by weighing 0.10 gram indium sulfide and place 1 * 10
-5In the methyl orange solution of mol/L (absorbance is approximately 1.0), carry out the Photocatalytic Activity for Degradation test.
The effect of embodiment 2-4 basically also meets Fig. 1-Fig. 4 among the embodiment; Above-mentioned experimental result shows: the indium sulfide powder of gained is a cubic structure; And it is big to have specific area, and size evenly is similar to the granule-morphology of bouquet shape; Average crystal grain diameter is 3-5 μ m, and 2.5 hours degradation rates can reach more than 90% in the test of indium sulfide visible light degraded methyl orange.
Claims (1)
1. the synthetic method of a novel visible photochemical catalyst indium sulfide is characterized in that, may further comprise the steps:
(a) take by weighing four hydration inidum chloride (InCl
34H
2O) be dissolved in the deionized water, adding its pH value of acetic acid adjusting is 1-3, adds thioacetamide (CH then
2CSNH
2) solution, the concentration of indium ion is 0.025mol/L, wherein the ratio of In and S amount of substance is 1: 4-1: 10;
(b) mixed solution that obtains in the step (a) is carried out heated at constant temperature and make it reaction, regulating temperature is 80 ℃, hydro-thermal reaction 4-8 hour, and the room temperature cooling;
(c) decompress filter, washing, drying obtains orange red indium sulfide powder.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103785131A (en) * | 2014-02-18 | 2014-05-14 | 齐鲁工业大学 | Method for catalytically degrading organic pollutants |
| CN103962156A (en) * | 2014-05-15 | 2014-08-06 | 天津理工大学 | Nano indium sulfide photocatalyst as well as preparation method and application thereof |
| CN103990486A (en) * | 2014-05-29 | 2014-08-20 | 江苏大学 | Preparation method of indium sulfide/carbon nitride composite nano material |
| CN104843769A (en) * | 2015-04-09 | 2015-08-19 | 首都师范大学 | Method for controllable preparation ultrathin two dimensional indium sulfide nano-material through using metal ions, and use of material |
| CN104588039B (en) * | 2014-12-31 | 2016-09-14 | 山东玉皇新能源科技有限公司 | A kind of hierarchy indium sulfide photocatalyst and preparation method thereof |
| CN106000424A (en) * | 2016-06-03 | 2016-10-12 | 牛和林 | Indium sulfide photocatalyst with ultrahigh photocatalytic activity and preparation method and application thereof |
| CN107670674A (en) * | 2017-10-12 | 2018-02-09 | 湖南大学 | Indium sulfide material of rare earth element codope and its preparation method and application |
| CN108786923A (en) * | 2018-05-08 | 2018-11-13 | 上海应用技术大学 | A kind of preparation method of kernel-shell structure, visible light catalyst |
| CN110038594A (en) * | 2019-05-13 | 2019-07-23 | 东北师范大学 | A kind of preparation method of porous oxidation indium/indium sulfide heterojunction material |
| CN110721722A (en) * | 2019-10-29 | 2020-01-24 | 福建师范大学福清分校 | CuS/In2S3@C3N4Visible light response photocatalyst and preparation method thereof |
| CN113385195A (en) * | 2021-07-23 | 2021-09-14 | 兰州大学 | Preparation and application of tungsten disulfide/indium sulfide heterojunction photocatalytic material |
| CN113461046A (en) * | 2021-07-28 | 2021-10-01 | 四川恒瑞天成科技有限公司 | Comb-shaped nitrogen-doped indium sulfide gas-sensitive material, preparation method and application |
| CN114939422A (en) * | 2022-05-05 | 2022-08-26 | 华南理工大学 | Hydrophobic defect type indium sulfide photocatalyst and preparation and application thereof |
| US11439990B2 (en) * | 2019-05-23 | 2022-09-13 | Soochow University | Titanium carbide nanosheet/layered indium sulfide heterojunction and application thereof in degrading and removing water pollutants |
| CN115959701A (en) * | 2023-02-20 | 2023-04-14 | 西南交通大学 | Preparation method and application of 3D self-assembly hydrangea-shaped indium sulfide |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103785131B (en) * | 2014-02-18 | 2016-03-02 | 齐鲁工业大学 | A kind of method of catalyze and degrade organic pollutants |
| CN103785131A (en) * | 2014-02-18 | 2014-05-14 | 齐鲁工业大学 | Method for catalytically degrading organic pollutants |
| CN103962156A (en) * | 2014-05-15 | 2014-08-06 | 天津理工大学 | Nano indium sulfide photocatalyst as well as preparation method and application thereof |
| CN103990486A (en) * | 2014-05-29 | 2014-08-20 | 江苏大学 | Preparation method of indium sulfide/carbon nitride composite nano material |
| CN103990486B (en) * | 2014-05-29 | 2016-04-06 | 江苏大学 | The preparation method of a kind of indium sulfide/carbonitride composite nano materials |
| CN104588039B (en) * | 2014-12-31 | 2016-09-14 | 山东玉皇新能源科技有限公司 | A kind of hierarchy indium sulfide photocatalyst and preparation method thereof |
| CN104843769A (en) * | 2015-04-09 | 2015-08-19 | 首都师范大学 | Method for controllable preparation ultrathin two dimensional indium sulfide nano-material through using metal ions, and use of material |
| CN106000424A (en) * | 2016-06-03 | 2016-10-12 | 牛和林 | Indium sulfide photocatalyst with ultrahigh photocatalytic activity and preparation method and application thereof |
| CN107670674A (en) * | 2017-10-12 | 2018-02-09 | 湖南大学 | Indium sulfide material of rare earth element codope and its preparation method and application |
| CN107670674B (en) * | 2017-10-12 | 2019-09-10 | 湖南大学 | The indium sulfide material and its preparation method and application of rare earth element codope |
| CN108786923B (en) * | 2018-05-08 | 2021-04-20 | 上海应用技术大学 | Preparation method of core-shell structure visible light catalyst |
| CN108786923A (en) * | 2018-05-08 | 2018-11-13 | 上海应用技术大学 | A kind of preparation method of kernel-shell structure, visible light catalyst |
| CN110038594A (en) * | 2019-05-13 | 2019-07-23 | 东北师范大学 | A kind of preparation method of porous oxidation indium/indium sulfide heterojunction material |
| US11439990B2 (en) * | 2019-05-23 | 2022-09-13 | Soochow University | Titanium carbide nanosheet/layered indium sulfide heterojunction and application thereof in degrading and removing water pollutants |
| CN110721722A (en) * | 2019-10-29 | 2020-01-24 | 福建师范大学福清分校 | CuS/In2S3@C3N4Visible light response photocatalyst and preparation method thereof |
| CN113385195A (en) * | 2021-07-23 | 2021-09-14 | 兰州大学 | Preparation and application of tungsten disulfide/indium sulfide heterojunction photocatalytic material |
| CN113461046A (en) * | 2021-07-28 | 2021-10-01 | 四川恒瑞天成科技有限公司 | Comb-shaped nitrogen-doped indium sulfide gas-sensitive material, preparation method and application |
| CN114939422A (en) * | 2022-05-05 | 2022-08-26 | 华南理工大学 | Hydrophobic defect type indium sulfide photocatalyst and preparation and application thereof |
| CN114939422B (en) * | 2022-05-05 | 2023-08-18 | 华南理工大学 | Hydrophobic defect type indium sulfide photocatalyst and preparation and application thereof |
| CN115959701A (en) * | 2023-02-20 | 2023-04-14 | 西南交通大学 | Preparation method and application of 3D self-assembly hydrangea-shaped indium sulfide |
| CN115959701B (en) * | 2023-02-20 | 2024-04-26 | 西南交通大学 | Preparation method and application of 3D self-assembled hydrangea-shaped indium sulfide |
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Application publication date: 20120201 |