CN102335616A - Synthesis method of novel visible-light photocatalyst indium sulfide - Google Patents

Synthesis method of novel visible-light photocatalyst indium sulfide Download PDF

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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
indium
light photocatalyst
visible light
temperature
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汪浩
高志华
刘晶冰
朱满康
严辉
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Beijing University of Technology
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Abstract

一种新型可见光光催化剂硫化铟的合成方法,属于光催化剂的制备技术领域。包括以下步骤:称取四水合氯化铟溶解于去离子水中,加入醋酸调节其pH值为1-3,然后加入硫代乙酰胺溶液,铟离子的浓度为0.025mol/L,其中In和S物质的量的比为1∶4-1∶10;将得到的混合溶液进行恒温加热使之反应,调节温度为80℃,水热反应4-8小时,室温冷却;减压抽滤,洗涤,干燥,得到橙红色硫化铟粉末。本发明方法制备的硫化铟形貌为花球形,比表面积大,大小均匀,所得的硫化铟粉体为立方结构。它作为可见光光催化剂,对有机染料(如甲基橙)有良好的降解效果。The invention discloses a synthesis method of a novel visible light photocatalyst indium sulfide, which belongs to the technical field of photocatalyst preparation. The method comprises the following steps: weighing indium chloride tetrahydrate and dissolving it in deionized water, adding acetic acid to adjust its pH value to 1-3, and then adding thioacetamide solution, the concentration of indium ion is 0.025mol/L, wherein In and S The ratio of the amount of substances is 1:4-1:10; the obtained mixed solution is heated at a constant temperature to make it react, the temperature is adjusted to 80°C, the hydrothermal reaction is carried out for 4-8 hours, and it is cooled at room temperature; suction filtration under reduced pressure, washing, Dry to obtain orange-red indium sulfide powder. The appearance of the indium sulfide prepared by the method of the invention is flower-shaped, the specific surface area is large, and the size is uniform, and the obtained indium sulfide powder has a cubic structure. As a visible light photocatalyst, it has a good degradation effect on organic dyes (such as methyl orange).

Description

A kind of synthetic method of novel visible photochemical catalyst indium sulfide
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,
Figure BDA0000077513140000031
) 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)

1.一种新型可见光光催化剂硫化铟的合成方法,其特征在于,包括以下步骤:1. a kind of synthetic method of novel visible light photocatalyst indium sulfide, is characterized in that, comprises the following steps: (a)称取四水合氯化铟(InCl3·4H2O)溶解于去离子水中,加入醋酸调节其pH值为1-3,然后加入硫代乙酰胺(CH2CSNH2)溶液,铟离子的浓度为0.025mol/L,其中In和S物质的量的比为1∶4-1∶10;(a) Weigh indium chloride tetrahydrate (InCl 3 4H 2 O) and dissolve it in deionized water, add acetic acid to adjust its pH to 1-3, then add thioacetamide (CH 2 CSNH 2 ) solution, indium The concentration of ions is 0.025mol/L, and the ratio of In and S substances is 1:4-1:10; (b)将步骤(a)中得到的混合溶液进行恒温加热使之反应,调节温度为80℃,水热反应4-8小时,室温冷却;(b) Heating the mixed solution obtained in step (a) at a constant temperature to make it react, adjusting the temperature to 80° C., hydrothermally reacting for 4-8 hours, and cooling at room temperature; (c)减压抽滤,洗涤,干燥,得到橙红色硫化铟粉末。(c) Suction filtration under reduced pressure, washing and drying to obtain orange-red indium sulfide powder.
CN201110205646XA 2011-07-21 2011-07-21 Synthesis method of novel visible-light photocatalyst indium sulfide Pending CN102335616A (en)

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Cited By (16)

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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 hierarchical structure 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
US20230249161A1 (en) * 2020-08-31 2023-08-10 Soochow University Z-type heterojunction composite material of tungsten oxide nanorod/titanium carbide quantum dot/indium sulfide nanosheet, preparation method therefor and application thereof

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Cited By (23)

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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 hierarchical structure 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 A kind of preparation method of visible light catalyst of core-shell structure
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
US20230249161A1 (en) * 2020-08-31 2023-08-10 Soochow University Z-type heterojunction composite material of tungsten oxide nanorod/titanium carbide quantum dot/indium sulfide nanosheet, preparation method therefor and application thereof
US12318763B2 (en) * 2020-08-31 2025-06-03 Soochow University Z-type heterojunction composite material of tungsten oxide nanorod/titanium carbide quantum dot/indium sulfide nanosheet, preparation method therefor and application 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
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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