CN104289234A - Preparation and application of efficient hydrogen production photo-catalyst MoS2-SrZrO3 - Google Patents

Preparation and application of efficient hydrogen production photo-catalyst MoS2-SrZrO3 Download PDF

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CN104289234A
CN104289234A CN201410539455.0A CN201410539455A CN104289234A CN 104289234 A CN104289234 A CN 104289234A CN 201410539455 A CN201410539455 A CN 201410539455A CN 104289234 A CN104289234 A CN 104289234A
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catalyst
srzro
solution
mos
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CN104289234B (en
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周建成
田庆文
刘佳慧
王猛
李乃旭
邓金全
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Southeast University
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Southeast University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention relates to preparation and application of a hydrogen production photo-catalyst MoS2-SrZrO3, aiming at solving the problems of low hydrogen production rate under ultraviolet light, instability and wide light response range of the catalyst. The catalyst is a heterojunction catalyst formed by MoS2 and SrZrO3. A preparation method of the catalyst comprises the following steps: adding SrOC12.8H2O and Sr(NO3)3 into a KOH solution, fully dissolving SrOC12.8H2O and Sr(NO3)3, putting the solution in a hydrothermal kettle for heating, washing and drying a product to obtain SrZrO3, then adding SrZrO3 a Na2MoO4.2H2O and CH3CSNH2 solution, ultrasonically stirring the solution, putting the solution in the hydrothermal kettle for heating, washing and drying the product to obtain the catalyst. The catalyst prepared by the method is environmentally friendly, and is high in hydrogen production rate which reaches 5.96mmol/L under ultraviolet light with wavelength being 365nm, and is long in service life, low in cost and suitable for large-scale production.

Description

A kind of highly effective hydrogen yield photochemical catalyst MoS 2-SrZrO 3preparations and applicatio
Technical field
Under the present invention relates to ultraviolet light, hydrogen is prepared in hydrolysis, is specifically related to MoS 2-SrZrO 3the preparation of photochemical catalyst and application thereof.
Background technology
Society, the energy that the mankind mainly consume has oil, coal and natural gas etc., but these energy belong to non-renewable energy resources, and is faced with exhausted danger.Meanwhile, this energy also causes countries in the world gradually close attention to a series of environmental problem that the earth brings is consumed.Therefore, Environment and energy be the 21 century mankind face and need the great problem of solution badly, look for a kind of environmentally friendly and the sustainable development of the energy of economy to human society and environment all has far-reaching and great meaning.Hydrogen Energy have renewable, source is wide, can store, the advantage not available for all traditional energies such as clean, therefore, utilizing the reproducible energy to prepare hydrogen will be one of main direction of developing of future source of energy.
Consider the problem such as energy fossil fuel shortages and environment deterioration, it will be one of the most excellent approach solving the energy and environmental problem that photochemical catalyzing prepares hydrogen.For a long time in 1972, the people such as the scientist Fujishima of Japan are at TiO 2electrode has found the phenomenon of photochemical catalyzing, has from then on opened the epoch of multiphase photocatalysis, due to photocatalysis hydrogen production main change solar energy into chemical energy, therefore the scientist of countries in the world studies the light-catalysed performance of different materials.The compound of perovskite, as SrZrO 3, SrTiO 3, BaZrO 3, CaTiO 3, there is unique physical property and chemical property, be widely studied in recent years.Chinese patent CN201210258924.2 describes the Ba of Ca-Ti ore type xsr 1-xfe 0.5co 0.5o 3-δphotochemical catalyst can effectively be degraded methyl orange solution.In document, (CrystEngComm, 2011,13,3842) report the SrZrO of Ca-Ti ore type 3the preparation process of nano-substance, but the raising of its application, light-catalysed performance and performance is not all introduced.
In order to solve the problem, therefore need design a kind of energy-efficient, hydrogen-producing speed is high, environmentally safe, relatively cheap photochemical catalyst.
Summary of the invention
Technical problem: the object of the invention is to solve that catalyst hydrogen-producing speed under ultraviolet light is low, poor stability and the problem such as optical range is narrow, provides a kind of photocatalysis MoS under ultraviolet light with highly effective hydrogen yield 2-SrZrO 3and application.
Technical scheme: a kind of highly effective hydrogen yield photochemical catalyst MoS of the present invention 2-SrZrO 3preparation method, wherein said photochemical catalyst MoS 2-SrZrO 3for MoS 2and SrZrO 3the hetero-junctions catalyst formed, its preparation method comprises the following steps:
1) zirconium oxychloride and strontium nitrate are joined according to mol ratio 1:1-3 in the solution of potassium hydroxide of 6-40mol/L, be uniformly mixed, solution is placed in water heating kettle, 1-72h is heated at 100-200 DEG C, after cooling by product through the washing of repeatedly deionization, pickling, vacuum drying, can obtain SrZrO 3powder;
2) by the SrZrO of preparation 3powder, sodium molybdate and thioacetamide are according to stoichiometric proportion, water-soluble with in ethanol, after stirring ultrasonic abundant mixing, be loaded in water heating kettle, at 160-240 DEG C, react 16-72h, naturally after cooling, product deionized water and ethanol are washed repeatedly, vacuum drying, can prepare MoS 2/ SrZrO 3photochemical catalyst.
Described MoS 2quality be the 0.001-30 of catalyst quality doubly, the mol ratio of sodium molybdate and thioacetamide is 1:3-8, and reaction temperature is 180-220 DEG C, and the reaction time is 24-54h.
The photochemical catalyst MoS of highly effective hydrogen yield of the present invention 2/ SrZrO 3be applied as: this hetero-junctions catalyst produces hydrogen under ultraviolet light.
Preferably, described step 1) described in basic zirconium chloride and the mol ratio of strontium nitrate be 1:1-2, the concentration of potassium hydroxide is 8-30mol/L, and reaction temperature is 140-220 DEG C, and the reaction time is 12-36h.
Described step 2) described in MoS 2quality be the 0.001-30 of catalyst quality doubly, the mol ratio of sodium molybdate and thioacetamide is 1:3-8, and reaction temperature is 180-220 DEG C, and the reaction time is 12-54h.
Beneficial effect: the present invention compared with prior art, has the following advantages:
1. the cheaper starting materials of the inventive method, reaction condition is gentle, production cost is low, environmental protection, is applicable to large-scale production, can effective alleviating energy crisis;
2. the hydrogen-producing speed of the novel photochemical catalyst prepared by the present invention is high, and catalyst activity is high and the life-span is long, effectively can substitute noble metal catalyst;
3. the MoS for preparing of the present invention 2-SrZrO 3photochemical catalyst belongs to hetero-junctions category, can make SrZrO 3electronics transfer to MoS fast and effectively 2, the combination of suppression and photohole, accelerates the generation of hydrogen.
Detailed description of the invention
Below by embodiment, technical solution of the present invention is described in further detail.
Embodiment 1: take 1.164gSr (NO 3) 3and 1.608gZrOCl 28H 2o is dissolved in the KOH solution of 12mol/L, and stirred at ambient temperature obtains white opacity suspension, is then transferred in water heating kettle, heats 24h, be cooled to room temperature at 200 DEG C, repeatedly washs, vacuum drying with deionized water, acetic acid,diluted, ethanol.Get the SrZrO of preparation 30.5g is dissolved in the deionized water of 20mL and the ethanol of 20mL, and pipettes 0.65mL0.005mol/LNa 2moO 42H 2o solution and 0.90mL0.025mol/LCH 3cSNH 2solution, after ultrasonic agitation 30min fully mixes, in transfer water heating kettle, is heated to 180 DEG C and maintains 48h.Be cooled to room temperature after reaction terminates, product is successively with deionized water and ethanol washing, and vacuum drying, obtains MoS 2/ SrZrO 3photochemical catalyst.By the SrZrO of 0.2g 3and MoS 2/ SrZrO 3catalyst joins the Na of 0.250mol/L 2sO 3with the Na of 0.350mol/L 2in S solution, pass into nitrogen 15min, the Hg light irradiation of 100w, records SrZrO by gas-chromatography 3and MoS 2/ SrZrO 3hydrogen-producing speed is respectively 1.95 and 4.51mmol/h.
Embodiment 2:
Take 1.387gSr (NO 3) 3and 1.608gZrOCl 28H 2o is dissolved in the KOH solution of 30mol/L, and stirred at ambient temperature obtains white opacity suspension, is then transferred in water heating kettle, heats 18h, be cooled to room temperature at 180 DEG C, repeatedly washs, vacuum drying with deionized water, acetic acid,diluted, ethanol.Get the SrZrO of preparation 30.5g is dissolved in the deionized water of 20mL and the ethanol of 20mL, and pipettes 2mL0.005mol/LNa 2moO 42H 2o solution and 4mL0.025mol/LCH 3cSNH 2solution, after ultrasonic agitation 30min fully mixes, in transfer water heating kettle, is heated to 200 DEG C and maintains 36h.Be cooled to room temperature after reaction terminates, product is successively with deionized water and ethanol washing, and vacuum drying, obtains MoS 2/ SrZrO 3photochemical catalyst.By 0.2gMoS 2/ SrZrO 3catalyst joins the Na of 0.250mol/L 2sO 3with the Na of 0.350mol/L 2in S solution, pass into nitrogen 15min, the Hg light irradiation of 100w, recording hydrogen-producing speed by gas-chromatography is 3.27mmol/h.
Embodiment 3:
Take 2.328gSr (NO 3) 3and 1.608gZrOCl 28H 2o is dissolved in the KOH solution of 20mol/L, and stirred at ambient temperature obtains white opacity suspension, is then transferred in water heating kettle, heats 28h, be cooled to room temperature at 200 DEG C, repeatedly washs, vacuum drying with deionized water, acetic acid,diluted, ethanol.Get the SrZrO of preparation 30.5g is dissolved in the deionized water of 20mL and the ethanol of 20mL, and pipettes 0.1mL0.005mol/LNa 2moO 42H 2o solution and 0.5mL0.025mol/LCH 3cSNH 2solution, after ultrasonic agitation 30min fully mixes, in transfer water heating kettle, is heated to 220 DEG C and maintains 15h.Be cooled to room temperature after reaction terminates, product is successively with deionized water and ethanol washing, and vacuum drying, obtains MoS 2/ SrZrO 3photochemical catalyst.By 0.2gMoS 2/ SrZrO 3catalyst joins the Na of 0.250mol/L 2sO 3with the Na of 0.350mol/L 2in S solution, pass into nitrogen 15min, the Hg light irradiation of 100w, recording hydrogen-producing speed by gas-chromatography is 5.96mmol/h.
Embodiment 4:
Take 1.752gSr (NO 3) 3and 1.608gZrOCl 28H 2o is dissolved in the KOH solution of 26mol/L, and stirred at ambient temperature obtains white opacity suspension, is then transferred in water heating kettle, heats 30h, be cooled to room temperature at 150 DEG C, repeatedly washs, vacuum drying with deionized water, acetic acid,diluted, ethanol.Get the SrZrO of preparation 30.5g is dissolved in the deionized water of 20mL and the ethanol of 20mL, and pipettes 1.3mL0.005mol/LNa 2moO 42H 2o solution and 2.1mL0.025mol/LCH 3cSNH 2solution, after ultrasonic agitation 30min fully mixes, in transfer water heating kettle, is heated to 210 DEG C and maintains 32h.Be cooled to room temperature after reaction terminates, product is successively with deionized water and ethanol washing, and vacuum drying, obtains MoS 2/ SrZrO 3photochemical catalyst.By 0.2gMoS 2/ SrZrO 3catalyst joins the Na of 0.250mol/L 2sO 3with the Na of 0.350mol/L 2in S solution, pass into nitrogen 15min, the Hg light irradiation of 100w, recording hydrogen-producing speed by gas-chromatography is 4.13mmol/h.
Embodiment 5:
Take 1.831gSr (NO 3) 3and 1.608gZrOCl 28H 2o is dissolved in the KOH solution of 12mol/L, and stirred at ambient temperature obtains white opacity suspension, is then transferred in water heating kettle, heats 20h, be cooled to room temperature at 190 DEG C, repeatedly washs, vacuum drying with deionized water, acetic acid,diluted, ethanol.Get the SrZrO of preparation 30.5g is dissolved in the deionized water of 20mL and the ethanol of 20mL, and pipettes 7mL0.005mol/LNa 2moO 42H 2o solution and 13mL0.025mol/LCH 3cSNH 2solution, after ultrasonic agitation 30min fully mixes, in transfer water heating kettle, is heated to 210 DEG C and maintains 54h.Be cooled to room temperature after reaction terminates, product is successively with deionized water and ethanol washing, and vacuum drying, obtains MoS 2/ SrZrO 3photochemical catalyst.By 0.2gMoS 2/ SrZrO 3catalyst joins the Na of 0.250mol/L 2sO 3with the Na of 0.350mol/L 2in S solution, pass into nitrogen 15min, the Hg light irradiation of 100w, recording hydrogen-producing speed by gas-chromatography is 3.57mmol/h.
Embodiment 6:
Take 1.350gSr (NO 3) 3and 1.608gZrOCl 28H 2o is dissolved in the KOH solution of 24mol/L, and stirred at ambient temperature obtains white opacity suspension, is then transferred in water heating kettle, heats 28h, be cooled to room temperature at 170 DEG C, repeatedly washs, vacuum drying with deionized water, acetic acid,diluted, ethanol.Get the SrZrO of preparation 30.5g is dissolved in the deionized water of 20mL and the ethanol of 20mL, and pipettes 1.4mL0.005mol/LNa 2moO 42H 2o solution and 2.0mL0.025mol/LCH 3cSNH 2solution, after ultrasonic agitation 30min fully mixes, in transfer water heating kettle, is heated to 190 DEG C and maintains 36h.Be cooled to room temperature after reaction terminates, product is successively with deionized water and ethanol washing, and vacuum drying, obtains MoS 2/ SrZrO 3photochemical catalyst.By 0.2gMoS 2/ SrZrO 3catalyst joins the Na of 0.250mol/L 2sO 3with the Na of 0.350mol/L 2in S solution, pass into nitrogen 15min, the Hg light irradiation of 100w, recording hydrogen-producing speed by gas-chromatography is 4.62mmol/h.

Claims (3)

1. a highly effective hydrogen yield photochemical catalyst MoS 2-SrZrO 3preparation method, it is characterized in that: described photochemical catalyst is MoS 2and SrZrO 3the hetero-junctions catalyst formed, its preparation method comprises the following steps:
1) zirconium oxychloride and strontium nitrate are joined according to mol ratio 1:1-3 in the solution of potassium hydroxide of 6-40mol/L, be uniformly mixed, solution is placed in water heating kettle, 1-72h is heated at 100-200 DEG C, after cooling by product through the washing of repeatedly deionization, pickling, vacuum drying, can obtain SrZrO 3powder;
2) by the SrZrO of preparation 3powder, sodium molybdate and thioacetamide are according to stoichiometric proportion, water-soluble with in ethanol, after stirring ultrasonic abundant mixing, be loaded in water heating kettle, at 160-240 DEG C, react 16-72h, naturally after cooling, product deionized water and ethanol are washed repeatedly, vacuum drying, can prepare MoS 2/ SrZrO 3photochemical catalyst.
2. the photochemical catalyst MoS of highly effective hydrogen yield according to claim 1 2-SrZrO 3preparation method, is characterized in that, described MoS 2quality be the 0.001-30 of catalyst quality doubly, the mol ratio of sodium molybdate and thioacetamide is 1:3-8, and reaction temperature is 180-220 DEG C, and the reaction time is 24-54h.
3. the photochemical catalyst MoS of a highly effective hydrogen yield as claimed in claim 1 2-SrZrO 3application, it is characterized in that: this hetero-junctions catalyst produces hydrogen under ultraviolet light.
CN201410539455.0A 2014-10-13 2014-10-13 A kind of highly effective hydrogen yield photocatalyst MoS2-SrZrO3Preparation and application Expired - Fee Related CN104289234B (en)

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CN105727999A (en) * 2016-01-25 2016-07-06 江苏大学 Method for preparing quaternary sulfide quantum dot based heterojunction efficient photocatalyst
CN111760566A (en) * 2020-07-07 2020-10-13 浙江大学 Calcium zirconate titanate micron particle, preparation method and application thereof
CN112811900A (en) * 2021-01-28 2021-05-18 苏州金宏气体股份有限公司 p-n-BaTiO3/NiO heterojunction piezoelectric ceramic, preparation method thereof and application thereof in self-powered high-efficiency hydrogen production
CN112876241A (en) * 2021-01-28 2021-06-01 苏州金宏气体股份有限公司 p-n-SrZrO3/NiO heterojunction piezoelectric ceramic, preparation method thereof and application thereof in self-powered high-efficiency hydrogen production
CN114100633A (en) * 2020-08-31 2022-03-01 中国石油化工股份有限公司 Catalyst for hydrogen production by visible light catalytic decomposition of hydrogen sulfide and preparation method thereof

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CN103071513A (en) * 2013-02-27 2013-05-01 福州大学 Hydrogen-production photocatalyst MoS2/ZnIn2S4 and preparation method thereof
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CN101979480A (en) * 2010-10-27 2011-02-23 合肥学院 Molybdenum disulfide nanosphere/titanium dioxide composite material and preparation method thereof
CN103028352A (en) * 2012-12-10 2013-04-10 江苏大学 Preparation method for synthesizing MoS2/Fe3O4 nano composite material
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105727999A (en) * 2016-01-25 2016-07-06 江苏大学 Method for preparing quaternary sulfide quantum dot based heterojunction efficient photocatalyst
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CN111760566A (en) * 2020-07-07 2020-10-13 浙江大学 Calcium zirconate titanate micron particle, preparation method and application thereof
CN114100633A (en) * 2020-08-31 2022-03-01 中国石油化工股份有限公司 Catalyst for hydrogen production by visible light catalytic decomposition of hydrogen sulfide and preparation method thereof
CN114100633B (en) * 2020-08-31 2023-10-20 中国石油化工股份有限公司 Catalyst for preparing hydrogen by catalyzing and decomposing hydrogen sulfide by visible light and preparation method thereof
CN112811900A (en) * 2021-01-28 2021-05-18 苏州金宏气体股份有限公司 p-n-BaTiO3/NiO heterojunction piezoelectric ceramic, preparation method thereof and application thereof in self-powered high-efficiency hydrogen production
CN112876241A (en) * 2021-01-28 2021-06-01 苏州金宏气体股份有限公司 p-n-SrZrO3/NiO heterojunction piezoelectric ceramic, preparation method thereof and application thereof in self-powered high-efficiency hydrogen production

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