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
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- 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
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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.
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