CN109794261A - A kind of one-step method prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method - Google Patents
A kind of one-step method prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method Download PDFInfo
- Publication number
- CN109794261A CN109794261A CN201910085636.3A CN201910085636A CN109794261A CN 109794261 A CN109794261 A CN 109794261A CN 201910085636 A CN201910085636 A CN 201910085636A CN 109794261 A CN109794261 A CN 109794261A
- Authority
- CN
- China
- Prior art keywords
- mixed solution
- composite photo
- hydroxyl
- catalyst
- samarium oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of one-step method to prepare indium sulfide/hydroxyl samarium oxide composite photo-catalyst method, first by In (NO3)3·4.5H2O, which dissolves in, forms solution in deionized water, then according to elemental mole ratios nIn:ns=1:3 weighs thioacetamide and is added in above-mentioned solution, stirs to get mixed solution A;Secondly Sm (NO is weighed3)3·6H2O, according to molar ratio nIn:nSm=1:(0.4~0.7) it is added in mixed solution A, stir to get mixed solution B;Mixed solution B is finally subjected to homogeneous hydro-thermal reaction, to after reaction, take out product, distinguishes centrifuge washing several times through deionized water and dehydrated alcohol, then drying to obtain In2S3/ SmOOH composite photo-catalyst.The method of the present invention is heated evenly, easy to control, other miscellaneous phases are not present in resulting product, utilization rate is high, and institute is low using cost of material, is easy to get to target product, effectively improves photocatalytic activity and stability, it can be used for pollutant in degradation of organic waste water, alleviate problem of environmental pollution.
Description
Technical field
The present invention relates to one kind with six nitric hydrate samariums, and indium nitrate and thioacetamide are the preparation vulcanization of raw material one-step method
Indium/hydroxyl samarium oxide composite photo-catalyst method.
Background technique
In today that industry and economy are increasingly flourishing, the problems such as energy shortage, environmental pollution, becomes more and more prominent, finds
It is new that prepare clean energy resource very urgent with the material of environmental problem is improved.Composite material prepared by the present invention is to solve to work as
The water pollution problems of preceding society, material can be converted into chemical energy using luminous energy come the organic pollutant in water body of degrading.
Indium sulfide is a kind of crystal of spinel structure as a kind of defect semiconductor material, and forbidden bandwidth is
2.0eV, has preferable visible light-responded, is the material for preparing a kind of great development prospect of visible light catalyst.Mesh
Before, the method for preparing indium sulfide mainly has: microwave-hydrothermal method [Pang, ZJ;Zhang,ML;Huang,L;et al.Synthesis
of In2S3thin film directly onto conductive substrates via PVP-assisted
Microwave irradiation method [J] .MATERIALS LETTERS.2018:210:66-69], sol-gel method
[Wen,Xiao-Ju;Niu,Cheng-Gang;Zhang,Lei.Sol-gel derived In2S3buffer layers for
inverted organic photovoltaic cells[J].SOLAR ENERGY.2014,108:230-237].It is wherein micro-
Wave hydro-thermal method has many advantages, such as that the reaction time is short, easy to operate, but there are certain risk in its reaction process;Colloidal sol-is solidifying
Glue method colloidal sol and gelation in preparation materials process is not easy to control, and it is non-uniform scarce that there are the indium sulfide material partial sizes of preparation
Point.
Oxyhydroxide is a kind of more special oxide, is made of hydroxide ion and a certain metal oxide
Compound, can regard that hydroxide is converted into the intermediate product of oxide as, report that more is to have FeOOH at present
(FeOOH), the oxyhydroxides such as hydroxy nickel oxide (NiOOH), and there is good chemical property, but hydroxyl samarium oxide
(SmOOH) report is seldom.The method for preparing hydroxyl samarium oxide at present mainly has: flux growth metrhod [Hiroaki, samata;
Masashi,Hanioka;Tadashi,C;et al.Synthesis and magnetic properties of SmOOH
crystals[J].JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS.2016,398:82-85].But it helps
Solvent method needs to grow crystal from melting salt solvent at high temperature, and required energy is higher, higher cost.
Summary of the invention
The purpose of the present invention is to provide a kind of one-step method to prepare indium sulfide/hydroxyl samarium oxide composite photo-catalyst side
Method, to overcome defect of the existing technology, the method for the present invention is heated evenly, easy to control, and there is no other are miscellaneous for resulting product
Phase, utilization rate is high, and institute is low using cost of material, is easy to get to target product, effectively improves photocatalytic activity and stability, can use
The pollutant in degradation of organic waste water alleviates problem of environmental pollution.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of one-step method prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method, comprising the following steps:
Step 1: by In (NO3)3·4.5H2O, which dissolves in, forms solution in deionized water, then according to elemental mole ratios nIn:
ns=1:3 weighs thioacetamide and is added in above-mentioned solution, stirs to get mixed solution A;
Step 2: Sm (NO is weighed3)3·6H2O, according to molar ratio nIn:nSm=1:(0.4~0.7) it is added to mixed solution
In A, mixed solution B is stirred to get;
Step 3: carrying out homogeneous hydro-thermal reaction for mixed solution B, to after reaction, take out product, through deionized water and
Dehydrated alcohol distinguishes centrifuge washing several times, then drying to obtain In2S3/ SmOOH composite photo-catalyst.
Further, 1.145g In (NO is added in step 1 in every 30mL deionized water3)3·4.5H2O。
Further, mixing time is 60min in step 2 and step 3.
Further, mixed solution B is subjected to homogeneous hydro-thermal reaction in step 3 specifically: be transferred to mixed solution B
In homogeneous water heating kettle, it is put into homogeneous reactor, 40%~60%, reaction temperature control is 160~180 DEG C for packing ratio control,
Reaction time control is 10~16h.
Further, dry for vacuum drying in step 3.
Further, drying temperature is 60 DEG C in step 3, drying time 5h.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention is with indium nitrate (In (NO3)3·4.5H2O), thioacetamide (CH3CSNH2), six nitric hydrate samarium (Sm
(NO)3·6H2It O is) raw material, using homogeneous hydro-thermal method, in the In of pure phase2S3Compound a small amount of SmOOH material, a step on nanosphere
Synthesize In2S3/ SmOOH catalysis material.This method is heated evenly, easy to control, other miscellaneous phases are not present in resulting product, is utilized
Rate is high, and institute is low using cost of material, is easy to get to target product, effectively improves photocatalytic activity and stability, can be used for degrading
Organic waste water pollutant alleviates problem of environmental pollution, obtained In2S3/ SmOOH composite photo-catalyst photocatalytic is above
Pure In2S3, SmOOH material.With methyl orange (MO) be degradation product, as radiation of visible light 150min, degradation efficiency reach 90% with
On.
Detailed description of the invention
Fig. 1 is In prepared by embodiment 32S3The XRD diagram of/SmOOH composite photo-catalyst;
Fig. 2 is In2S3Degradation MO degradation figure;
Fig. 3 is In2S3The In prepared with embodiment 32S3The degradation rate figure of the degradation MO of/SmOOH.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of one-step method prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method, comprising the following steps:
(1) by the In (NO of 1.145g3)3·4.5H2O dissolves in 30ml deionized water, according to elemental mole ratios nIn:ns=
1:3 weighs quantitative thioacetamide, is slowly added in above-mentioned solution, persistently stirs 60min, obtains mixed solution A.
(2) a certain amount of Sm (NO is then weighed3)3·6H2O, according to molar ratio nIn:nSm=1:0.4~0.7 is slowly added to
Into mixed solution A, mixed solution B is obtained after stirring 60min.
(3) mixed solution B is transferred in homogeneous water heating kettle, is put into homogeneous reactor, packing ratio control 40%~
60%, reaction temperature control is 160~180 DEG C, reacts 10~16h.
(4) to after reaction, take out product, distinguish centrifuge washing 4~6 times through deionized water and dehydrated alcohol, it is dry
In can be obtained in 5h2S3/ SmOOH composite photo-catalyst.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
(1) by the In (NO of 1.145g3)3·4.5H2O dissolves in 30ml deionized water, according to elemental mole ratios nIn:ns=
1:3 weighs quantitative thioacetamide, is slowly added in above-mentioned solution, persistently stirs 60min, obtains mixed solution A.
(2) a certain amount of Sm (NO is then weighed3)3·6H2O, according to molar ratio nIn:nSm=1:0.4 is slowly added into mixed
It closes in liquid A, obtains mixed liquid B after stirring 60min.
(3) mixed solution B is transferred in homogeneous water heating kettle, is put into homogeneous reactor, packing ratio control is reacted 40%
Temperature control is 160 DEG C, reacts 10h.
(4) to after reaction, take out reactant, at distinguishing centrifuge washing 4 times, 60 DEG C through deionized water and dehydrated alcohol
In can be obtained in vacuum drying 5h2S3/ SmOOH composite photo-catalyst.
Embodiment 2
(1) by the In (NO of 1.145g3)3·4.5H2O dissolves in 30ml deionized water, according to elemental mole ratios nIn:ns=
1:3 weighs quantitative thioacetamide, is slowly added in above-mentioned solution, persistently stirs 60min, obtains mixed solution A.
(2) a certain amount of Sm (NO is then weighed3)3·6H2O, according to molar ratio nIn:nSm=1:0.5 is slowly added into mixed
It closes in liquid A, obtains mixed liquid B after stirring 60min.
(3) mixed solution B is transferred in homogeneous water heating kettle, is put into homogeneous reactor, packing ratio control is reacted 50%
Temperature control is 170 DEG C, reacts 12h.
(4) to after reaction, take out reactant, at distinguishing centrifuge washing 5 times, 60 DEG C through deionized water and dehydrated alcohol
In can be obtained in vacuum drying 5h2S3/ SmOOH composite photo-catalyst.
Embodiment 3
(1) by the In (NO of 1.145g3)3·4.5H2O dissolves in 30ml deionized water, according to elemental mole ratios nIn:ns=
1:3 weighs quantitative thioacetamide, is slowly added in above-mentioned solution, persistently stirs 60min, obtains mixed solution A.
(2) a certain amount of Sm (NO is then weighed3)3·6H2O, according to molar ratio nIn:nSm=1:0.7 is slowly added into mixed
It closes in liquid A, obtains mixed liquid B after stirring 60min.
(3) mixed solution B is transferred in homogeneous water heating kettle, is put into homogeneous reactor, packing ratio control is reacted 60%
Temperature control is 180 DEG C, reacts 16h.
(4) to after reaction, take out reactant, at distinguishing centrifuge washing 6 times, 60 DEG C through deionized water and dehydrated alcohol
In can be obtained in vacuum drying 5h2S3/ SmOOH composite photo-catalyst.
Fig. 1 is In prepared by the embodiment of the present invention 32S3The XRD diagram of/SmOOH composite photo-catalyst, can from figure
It is right to respectively correspond standard card PFD 32-0456 (indium sulfide), PFD13-0618 (hydroxyl samarium oxide) institute for prepared sample out
It answers, main peak is clear, and object is compared pure, and Fig. 2 is pure phase In2S3Degradation figure, in 150 minutes degradation rates 80.64%, Fig. 3 was of the invention real
Apply In prepared by example 32S3/ SmOOH, degradation rate is increased to percent 94.6% after 150 minutes, it is seen that prepared by the present invention
Composite material compared with phase pure material, degradation efficiency is significantly improved.
Claims (6)
1. a kind of one-step method prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method, which is characterized in that including following step
It is rapid:
Step 1: by In (NO3)3·4.5H2O, which dissolves in, forms solution in deionized water, then according to elemental mole ratios nIn:ns=
1:3 weighs thioacetamide and is added in above-mentioned solution, stirs to get mixed solution A;
Step 2: Sm (NO is weighed3)3·6H2O, according to molar ratio nIn:nSm=1:(0.4~0.7) it is added in mixed solution A,
Stir to get mixed solution B;
Step 3: carrying out homogeneous hydro-thermal reaction for mixed solution B, to after reaction, take out product, through deionized water and anhydrous
Ethyl alcohol distinguishes centrifuge washing several times, then drying to obtain In2S3/ SmOOH composite photo-catalyst.
2. a kind of one-step method according to claim 1 prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method,
It is characterized in that, 1.145gIn (NO is added in step 1 in every 30mL deionized water3)3·4.5H2O。
3. a kind of one-step method according to claim 1 prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method,
It is characterized in that, mixing time is 60min in step 2 and step 3.
4. a kind of one-step method according to claim 1 prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method,
It is characterized in that, mixed solution B is subjected to homogeneous hydro-thermal reaction in step 3 specifically: mixed solution B is transferred to homogeneous hydro-thermal
In kettle, it is put into homogeneous reactor, 40%~60%, reaction temperature control is 160~180 DEG C for packing ratio control, the reaction time
Control is 10~16h.
5. a kind of one-step method according to claim 1 prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method,
It is characterized in that, it is dry for vacuum drying in step 3.
6. a kind of one-step method according to claim 5 prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method,
It is characterized in that, drying temperature is 60 DEG C in step 3, drying time 5h.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910085636.3A CN109794261B (en) | 2019-01-29 | 2019-01-29 | Method for preparing indium sulfide/hydroxyl samarium oxide composite photocatalyst by one-step method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910085636.3A CN109794261B (en) | 2019-01-29 | 2019-01-29 | Method for preparing indium sulfide/hydroxyl samarium oxide composite photocatalyst by one-step method |
Publications (2)
Publication Number | Publication Date |
---|---|
CN109794261A true CN109794261A (en) | 2019-05-24 |
CN109794261B CN109794261B (en) | 2021-12-07 |
Family
ID=66559070
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910085636.3A Active CN109794261B (en) | 2019-01-29 | 2019-01-29 | Method for preparing indium sulfide/hydroxyl samarium oxide composite photocatalyst by one-step method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109794261B (en) |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006256901A (en) * | 2005-03-17 | 2006-09-28 | Nissan Motor Co Ltd | Hydrogen production apparatus, hydrogen production method and hydrogen production system |
WO2007125998A1 (en) * | 2006-04-28 | 2007-11-08 | Ishihara Sangyo Kaisha, Ltd. | Photocatalyst, process for producing the photocatalyst, and photocatalyst coating agent, photocatalyst dispersion, and photocatalyst body using the photocatalyst |
JP2009066529A (en) * | 2007-09-13 | 2009-04-02 | Tokyo Univ Of Science | Photocatalyst, its manufacturing method, and method for generating hydrogen gas |
CN102020332A (en) * | 2009-09-15 | 2011-04-20 | 深圳市金达莱环保股份有限公司 | Dephosphorization method through adsorption |
CN102600790A (en) * | 2011-01-20 | 2012-07-25 | 中国科学院金属研究所 | Nanometer cerium oxide hydrate-based arsenic removing material, preparation method thereof and application in arsenic removing |
CN103657686A (en) * | 2013-12-02 | 2014-03-26 | 南昌航空大学 | Method for preparing SnIn4S photocatalyst through low-temperature coprecipitation method |
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 |
-
2019
- 2019-01-29 CN CN201910085636.3A patent/CN109794261B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006256901A (en) * | 2005-03-17 | 2006-09-28 | Nissan Motor Co Ltd | Hydrogen production apparatus, hydrogen production method and hydrogen production system |
WO2007125998A1 (en) * | 2006-04-28 | 2007-11-08 | Ishihara Sangyo Kaisha, Ltd. | Photocatalyst, process for producing the photocatalyst, and photocatalyst coating agent, photocatalyst dispersion, and photocatalyst body using the photocatalyst |
JP2009066529A (en) * | 2007-09-13 | 2009-04-02 | Tokyo Univ Of Science | Photocatalyst, its manufacturing method, and method for generating hydrogen gas |
CN102020332A (en) * | 2009-09-15 | 2011-04-20 | 深圳市金达莱环保股份有限公司 | Dephosphorization method through adsorption |
CN102600790A (en) * | 2011-01-20 | 2012-07-25 | 中国科学院金属研究所 | Nanometer cerium oxide hydrate-based arsenic removing material, preparation method thereof and application in arsenic removing |
CN103657686A (en) * | 2013-12-02 | 2014-03-26 | 南昌航空大学 | Method for preparing SnIn4S photocatalyst through low-temperature coprecipitation method |
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 |
Non-Patent Citations (3)
Title |
---|
HIROAKI SAMATA ET AL.: ""Synthesis and magnetic properties SmOOH crystals"", 《JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS》 * |
MENGHAN ZHANG ET AL.: ""Fabrication of a visible-light In2S3/BiPO4 heterojunction with enhanced photocatalytic activity"", 《NEW JOURNAL OR CHEMISTRY》 * |
张鑫: ""硫化铟复合纳米纤维材料的制备及其光催化性质研究"", 《中国博士学位论文全文数据库工程科技I辑》 * |
Also Published As
Publication number | Publication date |
---|---|
CN109794261B (en) | 2021-12-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105668632B (en) | A kind of tungsten bronze nanometer stub particle of variable valency metal catalysis and doping and preparation method thereof | |
CN111729675B (en) | ZIF-67-DERIVED Co 3 S 4 And ZnIn 2 S 4 Preparation method and application of formed composite photocatalyst | |
CN109913898B (en) | WO (WO)3/CuWO4Preparation method of/NiFe LDH ternary composite photoelectrode film | |
CN109806888B (en) | 1T-MoS2Modified ZnCoS solid solution hollow dodecahedron nanocomposite and preparation method and application thereof | |
CN108373175A (en) | Aluminium doped cobaltic-cobaltous oxide and its preparation method and application | |
CN107308957B (en) | Spherical Bi2S3/Bi2WO6Preparation method of heterojunction photocatalytic material | |
CN109037617A (en) | A kind of cobaltous selenide/nitrogen-doped carbon composite material and preparation method, application | |
CN107754822A (en) | A kind of preparation and its application based on CdSe/BiOCl composite photo-catalysts | |
CN103240073B (en) | Zn<2+>-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof | |
CN112875755B (en) | Preparation method of bismuth tungstate nano powder | |
CN105056973B (en) | Efficient Bi2S3-BiFeO3 composite visible-light-driven photocatalyst prepared through in-situ growth with chemical corrosion method and application of Bi2S3-BiFeO3 composite visible-light-driven photocatalyst | |
CN110075875A (en) | It is a kind of using NiSe as efficient heterojunction photocatalyst of auxiliary agent and its preparation method and application | |
CN110164699B (en) | Iron-doped nickel oxide and application thereof in photocatalytic fuel cell | |
CN101789298A (en) | Preparation method of Cu2O/NiFe2O4 magnetic composite | |
CN109761276A (en) | A kind of stratiform ammonium vanadate electrode material and its preparation method and application | |
CN111420664A (en) | Preparation method of flaky cuprous oxide/cobaltous oxide nanocomposite and application of flaky cuprous oxide/cobaltous oxide nanocomposite in catalyzing ammonia borane hydrolysis hydrogen production | |
CN103936082B (en) | A kind of synthetic method of cobalt acid samarium nano-powder | |
CN105396605A (en) | Preparation method of silicate clay/copper/carbon nitride composite material | |
CN101891236A (en) | Method for synthesizing monodisperse samarium-doped rare earth cerium oxide nanocrystal | |
CN109794261A (en) | A kind of one-step method prepares indium sulfide/hydroxyl samarium oxide composite photo-catalyst method | |
CN108273522B (en) | A kind of Z-type semiconductor light-catalyst and its preparation method and application with trapezium structure | |
CN108187686A (en) | A kind of CuCrO2The sol-gel process for preparing of powder | |
CN111482175B (en) | Preparation method of copper/cuprous oxide heterojunction nanosheet catalyst | |
CN103332740A (en) | Preparation method of monoclinic phase ditetrahedron bismuth vanadate crystal | |
CN103601157B (en) | A kind of method that ethanediamine auxiliary polyhydric alcohol based sols synthesis Cu-In-Al-Se is nanocrystalline |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |