CN109794261B - Method for preparing indium sulfide/hydroxyl samarium oxide composite photocatalyst by one-step method - Google Patents
Method for preparing indium sulfide/hydroxyl samarium oxide composite photocatalyst by one-step method Download PDFInfo
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Abstract
The invention discloses a method for preparing an indium sulfide/hydroxyl samarium oxide composite photocatalyst by a one-step method3)3·4.5H2Dissolving O in deionized water to form a solution, and then dissolving O in the deionized water according to the element molar ratio nIn:nsWeighing thioacetamide in a ratio of 1:3, adding the thioacetamide into the solution, and stirring to obtain a mixed solution A; then Sm (NO) was weighed out3)3·6H2O, in a molar ratio nIn:nSmAdding (0.4-0.7) to the mixed solution A, and stirring to obtain a mixed solution B; finally, carrying out homogeneous hydrothermal reaction on the mixed solution B, taking out a product after the reaction is finished, respectively centrifugally washing the product for a plurality of times by deionized water and absolute ethyl alcohol, and then drying the product to obtain In2S3/SmOOH composite photocatalyst. The method has the advantages of uniform heating, easy control, no other impure phase in the obtained product, high utilization rate, low cost of the used raw materials, easy obtainment of the target product, effective improvement of photocatalytic activity and stability, and capability of degrading pollutants in organic wastewater and relieving the problem of environmental pollution.
Description
Technical Field
The invention relates to a method for preparing an indium sulfide/hydroxyl samarium oxide composite photocatalyst by using samarium nitrate hexahydrate, indium nitrate and thioacetamide as raw materials through a one-step method.
Background
In the present day that industry and economy are increasingly developed, problems such as energy shortage and environmental pollution become more and more prominent, and the search for new materials for preparing clean energy and improving environmental problems is not slow. The composite material prepared by the invention aims to solve the problem of water pollution in the current society, and the material can degrade organic pollutants in water by converting light energy into chemical energy.
Indium sulfide is used as an excellent semiconductor material, is a crystal with a spinel structure, has the forbidden band width of 2.0eV, has better visible light response, and is a material with great development prospect for preparing visible light catalysts. At present, the methods for preparing indium sulfide mainly comprise: microwave hydrothermal method [ Pang, ZJ; zhang, ML; huang, L; synthesis of In2S3 thin film directly onto conductive substrates via PVP-assisted microwave irradiation method[J].MATERIALS LETTERS.2018:210:66-69]Sol-gel methods [ Wen, Xiao-Ju; niu, Cheng-Gang; zhang, Lei. Sol-gel derived In2S3 buffer layers for inverted organic photovoltaic cells[J].SOLAR ENERGY.2014,108:230-237]. The microwave hydrothermal method has the advantages of short reaction time, convenient operation and the like, but certain dangerousness exists in the reaction process; the sol-gel method has the defects that the sol and the gelation are not easy to control in the process of preparing the material, and the particle size of the prepared indium sulfide material is not uniform.
Oxyhydroxide is a relatively special oxide, which is a compound composed of hydroxide ions and a certain metal oxide, and can be regarded as an intermediate product for converting hydroxide into oxide, and currently, many oxyhydroxides such as iron oxyhydroxide (FeOOH) and nickel oxyhydroxide (NiOOH) are reported, and have good electrochemical properties, but samarium oxyhydroxide (SmOOH) is rarely reported. The existing method for preparing samarium oxyhydroxide mainly comprises the following steps: flux method [ Hiroaki, samata; masashi, Hanioka; tadashi, C; synthesis and magnetic properties OF SmOOH crystals [ J ]. JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS.2016,398:82-85 ]. However, the cosolvent method requires crystals to grow from a molten salt solvent at high temperature, and requires high energy and high cost.
Disclosure of Invention
The invention aims to provide a method for preparing an indium sulfide/samarium oxyhydroxide composite photocatalyst by a one-step method, which overcomes the defects in the prior art, is uniformly heated and easy to control, does not have other impure phases in the obtained product, has high utilization rate, uses low cost of raw materials, is easy to obtain a target product, effectively improves the photocatalytic activity and stability, can be used for degrading pollutants in organic wastewater and relieves the problem of environmental pollution.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing an indium sulfide/samarium oxyhydroxide composite photocatalyst by a one-step method comprises the following steps:
the method comprises the following steps: in (NO)3)3·4.5H2Dissolving O in deionized water to form a solution, and then dissolving O in the deionized water according to the element molar ratio nIn:nsWeighing thioacetamide in a ratio of 1:3, adding the thioacetamide into the solution, and stirring to obtain a mixed solution A;
step two: weighing Sm (NO)3)3·6H2O, in a molar ratio nIn:nSmAdding (0.4-0.7) to the mixed solution A, and stirring to obtain a mixed solution B;
step three: carrying out homogeneous hydrothermal reaction on the mixed solution B, taking out a product after the reaction is finished, respectively centrifugally washing the product for a plurality of times by deionized water and absolute ethyl alcohol, and drying the product to obtain In2S3/SmOOH composite photocatalyst.
Further, In step one, 1.145g of In (NO) is added to 30mL of deionized water3)3·4.5H2O。
Further, the stirring time in the first step and the second step is 60 min.
Further, in the third step, the homogeneous hydrothermal reaction of the mixed solution B is specifically: and transferring the mixed solution B into a homogeneous hydrothermal kettle, and putting the homogeneous hydrothermal kettle into a homogeneous reactor, wherein the filling ratio is controlled to be 40-60%, the reaction temperature is controlled to be 160-180 ℃, and the reaction time is controlled to be 10-16 h.
Further, the drying in the third step is vacuum drying.
Further, in the third step, the drying temperature is 60 ℃, and the drying time is 5 hours.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention uses indium nitrate (In (NO)3)3·4.5H2O), thioacetamide (CH)3CSNH2) Samarium nitrate hexahydrate (Sm (NO)3·6H2O) as raw material, adopting homogeneous hydrothermal method, In pure phase2S3Compounding small amount of SmOOH material on the nanosphere, and synthesizing In one step2S3/SmOOH photocatalytic material. The method has the advantages of uniform heating, easy control, no other impure phase In the obtained product, high utilization rate, low cost of the used raw materials, easy obtainment of a target product, effective improvement of photocatalytic activity and stability, and capability of degrading pollutants In organic wastewater and relieving the problem of environmental pollution to obtain In2S3The photocatalysis performance of the SmOOH composite photocatalyst is higher than that of pure In2S3SmOOH material. Methyl Orange (MO) is used as a degradation product, and when the visible light irradiates for 150min, the degradation efficiency reaches over 90 percent.
Drawings
FIG. 1 is In prepared In example 32S3XRD pattern of SmOOH composite photocatalyst;
FIG. 2 is In2S3Degradation map of degraded MO;
FIG. 3 is In2S3And In prepared In example 32S3Degradation rate profile of degraded MO/SmOOH.
Detailed Description
Embodiments of the invention are described in further detail below:
a method for preparing an indium sulfide/samarium oxyhydroxide composite photocatalyst by a one-step method comprises the following steps:
(1) 1.145g of In (NO)3)3·4.5H2O, dissolved in 30ml of deionized water according to the element molar ratio nIn:nsQuantitative thioacetamide was weighed in a ratio of 1:3, slowly added to the above solution, and continuously stirred for 60min to obtain a mixed solution a.
(2) Then, a predetermined amount of Sm (NO) was weighed3)3·6H2O, in a molar ratio nIn:nSmSlowly adding the mixture into the mixed solution A at a ratio of 1: 0.4-0.7, and stirring for 60min to obtain a mixed solution B.
(3) And transferring the mixed solution B into a homogeneous hydrothermal kettle, putting the homogeneous hydrothermal kettle into a homogeneous reactor, controlling the filling ratio to be 40-60%, controlling the reaction temperature to be 160-180 ℃, and reacting for 10-16 h.
(4) After the reaction is finished, taking out the product, respectively centrifugally washing the product for 4-6 times by using deionized water and absolute ethyl alcohol, and drying the product for 5 hours to obtain In2S3/SmOOH composite photocatalyst.
The present invention is described in further detail below with reference to examples:
example 1
(1) 1.145g of In (NO)3)3·4.5H2O, dissolved in 30ml of deionized water according to the element molar ratio nIn:nsQuantitative thioacetamide was weighed in a ratio of 1:3, slowly added to the above solution, and continuously stirred for 60min to obtain a mixed solution a.
(2) Then, a predetermined amount of Sm (NO) was weighed3)3·6H2O, in a molar ratio nIn:nSmSlowly adding the mixture A at a ratio of 1:0.4, and stirring for 60min to obtain a mixed solution B.
(3) And transferring the mixed solution B into a homogeneous hydrothermal kettle, putting the homogeneous hydrothermal kettle into a homogeneous reactor, controlling the filling ratio to be 40 percent, controlling the reaction temperature to be 160 ℃, and reacting for 10 hours.
(4) After the reaction is finished, taking out the reactant, respectively centrifugally washing the reactant for 4 times by deionized water and absolute ethyl alcohol, and drying the reactant for 5 hours In vacuum at the temperature of 60 ℃ to obtain In2S3/SmOOH composite photocatalyst.
Example 2
(1) 1.145g of In (NO)3)3·4.5H2O, dissolved in 30ml of deionized water according to the element molar ratio nIn:nsQuantitative thioacetamide was weighed in a ratio of 1:3, slowly added to the above solution, and continuously stirred for 60min to obtain a mixed solution a.
(2) Then, a predetermined amount of Sm (NO) was weighed3)3·6H2O, in a molar ratio nIn:nSmSlowly adding the mixture into the mixed solution A at a ratio of 1:0.5, and stirring for 60min to obtain a mixed solution B.
(3) And transferring the mixed solution B into a homogeneous hydrothermal kettle, putting the homogeneous hydrothermal kettle into a homogeneous reactor, controlling the filling ratio to be 50 percent, controlling the reaction temperature to be 170 ℃, and reacting for 12 hours.
(4) After the reaction is finished, taking out the reactant, respectively centrifugally washing the reactant for 5 times by deionized water and absolute ethyl alcohol, and drying the reactant for 5 hours In vacuum at the temperature of 60 ℃ to obtain In2S3/SmOOH composite photocatalyst.
Example 3
(1) 1.145g of In (NO)3)3·4.5H2O, dissolved in 30ml of deionized water according to the element molar ratio nIn:nsQuantitative thioacetamide was weighed in a ratio of 1:3, slowly added to the above solution, and continuously stirred for 60min to obtain a mixed solution a.
(2) Then, a predetermined amount of Sm (NO) was weighed3)3·6H2O, in a molar ratio nIn:nSmSlowly add the mixture a at a ratio of 1:0.7, and stir for 60min to obtain a mixture B.
(3) And transferring the mixed solution B into a homogeneous hydrothermal kettle, putting the homogeneous hydrothermal kettle into a homogeneous reactor, controlling the filling ratio to be 60 percent, controlling the reaction temperature to be 180 ℃, and reacting for 16 hours.
(4) After the reaction is finished, taking out the reactant, respectively centrifugally washing the reactant for 6 times by deionized water and absolute ethyl alcohol, and drying the reactant for 5 hours In vacuum at the temperature of 60 ℃ to obtain In2S3/SmOOH composite photocatalyst.
FIG. 1 shows In prepared In example 3 of the present invention2S3XRD pattern of/SmOOH composite photocatalystIt can be seen that the prepared samples correspond to the standard card PFD 32-0456 (indium sulfide) and PFD13-0618 (samarium oxyhydroxide), respectively, the main peak is clear, the phases are relatively pure, and FIG. 2 shows pure phase In2S3Degradation diagram, degradation rate 80.64% In 150 minutes, FIG. 3 is In prepared by example 3 of the present invention2S3The SmOOH has the degradation rate improved to 94.6 percent after 150 minutes, and the composite material prepared by the invention has obviously improved degradation efficiency compared with a pure phase material.
Claims (6)
1. A method for preparing an indium sulfide/samarium oxyhydroxide composite photocatalyst by a one-step method is characterized by comprising the following steps of:
the method comprises the following steps: in (NO)3)3·4.5H2Dissolving O in deionized water to form a solution, and then dissolving O in the deionized water according to the element molar ratio nIn:nsWeighing thioacetamide in a ratio of 1:3, adding the thioacetamide into the solution, and stirring to obtain a mixed solution A;
step two: weighing Sm (NO)3)3·6H2O, in a molar ratio nIn:nSmAdding (0.4-0.7) to the mixed solution A, and stirring to obtain a mixed solution B;
step three: carrying out homogeneous hydrothermal reaction on the mixed solution B, taking out a product after the reaction is finished, respectively centrifugally washing the product for a plurality of times by deionized water and absolute ethyl alcohol, and drying the product to obtain In2S3/SmOOH composite photocatalyst.
2. The method for preparing the indium sulfide/samarium hydroxide composite photocatalyst by the one-step method according to claim 1, wherein 1.145gIn (NO) is added into every 30mL of deionized water in the first step3)3·4.5H2O。
3. The method for preparing the indium sulfide/samarium oxyhydroxide composite photocatalyst by the one-step method according to claim 1, wherein the stirring time in the first step and the second step is 60 min.
4. The method for preparing the indium sulfide/samarium oxyhydroxide composite photocatalyst by the one-step method according to claim 1, wherein the step three comprises the following specific steps of performing a homogeneous hydrothermal reaction on the mixed solution B: and transferring the mixed solution B into a homogeneous hydrothermal kettle, and putting the homogeneous hydrothermal kettle into a homogeneous reactor, wherein the filling ratio is controlled to be 40-60%, the reaction temperature is controlled to be 160-180 ℃, and the reaction time is controlled to be 10-16 h.
5. The method for preparing the indium sulfide/samarium oxyhydroxide composite photocatalyst by the one-step method according to claim 1, wherein the drying in the third step is vacuum drying.
6. The method for preparing the indium sulfide/samarium oxyhydroxide composite photocatalyst according to claim 5, wherein the drying temperature in the third step is 60 ℃ and the drying time is 5 hours.
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