CN108069390A - The method that zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution prepares hydrogen - Google Patents

The method that zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution prepares hydrogen Download PDF

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Publication number
CN108069390A
CN108069390A CN201711310821.5A CN201711310821A CN108069390A CN 108069390 A CN108069390 A CN 108069390A CN 201711310821 A CN201711310821 A CN 201711310821A CN 108069390 A CN108069390 A CN 108069390A
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CN
China
Prior art keywords
photochemical catalyst
lactic acid
zinc sulphide
acid aqueous
aqueous solution
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Pending
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CN201711310821.5A
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Chinese (zh)
Inventor
孙剑辉
铁璐娜
禹崇菲
谭露
杨丝雨
陈慧
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Henan Normal University
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Henan Normal University
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Priority to CN201711310821.5A priority Critical patent/CN108069390A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042Decomposition of water
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04Sulfides
    • B01J35/39
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/08Sulfides
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention discloses a kind of methods that zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution prepares hydrogen, it weighs 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions is placed in the 100mL quartz containers of top light-permeable, by magnetic stirring apparatus zinc sulphide photochemical catalyst is made to be dispersed in reaction solution, it smears vacuum grease quartz container is connected on reaction unit, whole system first vacuumizes while is passed through condensed water maintenance system constant temperature before reaction, and zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution persistently generates hydrogen under Xe light irradiations.Zinc sulphide photochemical catalyst used in the present invention has preferable Photocatalyzed Hydrogen Production performance, photocatalysis lactic acid aqueous solution production hydrogen is continuous under 300W Xe light irradiations and stablizes, and 789.39 μm of olg are up to by the way that specific zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution is selected to react 5h hydrogen outputs‑1·h‑1

Description

The method that zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution prepares hydrogen
Technical field
The invention belongs to Photocatalyzed Hydrogen Production technical fields, and in particular to a kind of zinc sulphide photochemical catalyst photocatalysis lactic acid is water-soluble The method that liquid prepares hydrogen.
Background technology
With the development of modern industry, the non-renewable fossil energy such as coal is used by a large amount of burnings, does not only result in the earth Upper energy shortage and burning causes serious environmental problem, greenhouse effects can be formed by such as generating carbon dioxide, generate nitrogen oxygen Compound and oxysulfide can bring acid rain etc..Since entry into 21 century, the world is increasing to the demand of the energy, finds a kind of energy Mass production and environment amenable fossil fuel alternative energy source have become extremely urgent thing, and develop such as the sun The new energy such as energy, wind energy, nuclear energy, geothermal energy, ocean energy are then the preferable means of a kind of future for tackling current energy crisis.Its The advantages that middle Hydrogen Energy is generated with contamination-free after its clean, renewable, burning is favored be subject to researcher, is expected to become The energy of new generation is effectively to alleviate huge Pressure on Energy.It is that one kind can reduce hydrogen manufacturing cost, meet by photolysis water hydrogen Not only developed the economy but also a kind of method of environmental protection theory, it is only necessary under the irradiation of luminous energy and the catalytic action of catalysis material With regard to that can be Hydrogen Energy by the great Water Resource Transformation of reserves in nature, while any pollutant will not be generated, it is catalyzed to urge Agent can be used with repetitive cycling, be undoubtedly a kind of inexpensive, green, efficient possible technique.
The content of the invention
The technical problem to be solved by the present invention is to provide the zinc sulphide light that a kind of technical process is simple and hydrogen generation efficiency is higher The method that catalyst photocatalysis lactic acid aqueous solution prepares hydrogen.
The present invention adopts the following technical scheme that zinc sulphide photochemical catalyst photocatalysis lactic acid is water-soluble to solve above-mentioned technical problem The method that liquid prepares hydrogen, it is characterised in that concretely comprise the following steps:Weigh 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions It is placed in the 100mL quartz containers of top light-permeable, by magnetic stirring apparatus zinc sulphide photochemical catalyst is made to be dispersed in reaction In liquid, smear vacuum grease and quartz container is connected on reaction unit, whole system first vacuumizes while is passed through condensation before reaction Water maintenance system constant temperature, zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution persistently generates hydrogen under Xe light irradiations, instead 5h hydrogen outputs is answered to reach 789.39 μm of olg-1·h-1, the specific preparation process of the zinc sulphide photochemical catalyst is:It weighs 0.7513g thioacetamides add in the mixed solution of the prepared absolute ethyl alcohols of 50mL and glycerine, magnetic in the beaker of 80mL Power is stirred to solution and clarified, and adds 1.3630g zinc chloride, continues that mixed liquor is transferred to 100mL polytetrafluoroethyl-nes after stirring 10min 10h is reacted in 180 DEG C in alkene reaction kettle, cooled to room temperature after the completion of reaction is separated by filtration, and is alternately cleaned with water and ethyl alcohol It is 3 times, then dry for 24 hours up to zinc sulphide photochemical catalyst in 60 DEG C.
Further preferably, deionized water and the volume ratio of lactic acid are 3 in the lactic acid aqueous solution:1.
Zinc sulphide photochemical catalyst used in the present invention has preferable Photocatalyzed Hydrogen Production performance, under 300W Xe light irradiations Photocatalysis lactic acid aqueous solution production hydrogen is continuous and stablizes, by selecting specific zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution anti- 5h hydrogen outputs is answered to be up to 789.39 μm of olg-1·h-1
Description of the drawings
Fig. 1 is the transmission electron microscope picture of zinc sulphide photochemical catalyst made from embodiment 3;
Fig. 2 is that the production curve that zinc sulphide photochemical catalyst photocatalysis lactic acid solution prepares hydrogen is made in different embodiments.
Specific embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair Bright scope.
Embodiment 1
0.1879g thioacetamides are weighed in the beaker of 80mL, add in the mixed of the prepared absolute ethyl alcohols of 50mL and glycerine Solution is closed, and magnetic agitation to solution is clarified, and adds 1.3630g zinc chloride, continues mixed liquor to be transferred to after stirring 10min 10h is reacted in 180 DEG C in 100mL ptfe autoclaves, cooled to room temperature after the completion of reaction is separated by filtration, uses water With ethyl alcohol alternately cleaning 3 times, zinc sulphide photochemical catalyst is then obtained for 24 hours in 60 DEG C of dryings.
Weigh 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions(The volume ratio of wherein deionized water and lactic acid is 3:1)It is placed in the 100mL quartz containers of top light-permeable, is dispersed in zinc sulphide photochemical catalyst by magnetic stirring apparatus In reaction solution, smear vacuum grease and quartz container is connected on reaction unit, whole system is first vacuumized while is passed through before reaction Condensed water maintenance system constant temperature, zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution persistently generates hydrogen under Xe light irradiations Gas carries out on-line analysis by the TCD detectors of gas chromatograph, reacts 5h hydrogen outputs up to 355.53 μm of olg-1·h-1
Embodiment 2
0.3757g thioacetamides are weighed in the beaker of 80mL, add in the mixed of the prepared absolute ethyl alcohols of 50mL and glycerine Solution is closed, and magnetic agitation to solution is clarified, and adds 1.3630g zinc chloride, continues mixed liquor to be transferred to after stirring 10min 10h is reacted in 180 DEG C in 100mL ptfe autoclaves, cooled to room temperature after the completion of reaction is separated by filtration, uses water With ethyl alcohol alternately cleaning 3 times, zinc sulphide photochemical catalyst is then obtained for 24 hours in 60 DEG C of dryings.
Weigh 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions(The volume ratio of wherein deionized water and lactic acid is 3:1)It is placed in the 100mL quartz containers of top light-permeable, is dispersed in zinc sulphide photochemical catalyst by magnetic stirring apparatus In reaction solution, smear vacuum grease and quartz container is connected on reaction unit, whole system is first vacuumized while is passed through before reaction Condensed water maintenance system constant temperature, zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution persistently generates hydrogen under Xe light irradiations Gas carries out on-line analysis by the TCD detectors of gas chromatograph, reacts 5h hydrogen outputs up to 556.49 μm of olg-1·h-1
Embodiment 3
0.7513g thioacetamides are weighed in the beaker of 80mL, add in the mixed of the prepared absolute ethyl alcohols of 50mL and glycerine Solution is closed, and magnetic agitation to solution is clarified, and adds 1.3630g zinc chloride, continues mixed liquor to be transferred to after stirring 10min 10h is reacted in 180 DEG C in 100mL ptfe autoclaves, cooled to room temperature after the completion of reaction is separated by filtration, uses water With ethyl alcohol alternately cleaning 3 times, zinc sulphide photochemical catalyst is then obtained for 24 hours in 60 DEG C of dryings.
Weigh 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions(The volume ratio of wherein deionized water and lactic acid is 3:1)It is placed in the 100mL quartz containers of top light-permeable, is dispersed in zinc sulphide photochemical catalyst by magnetic stirring apparatus In reaction solution, smear vacuum grease and quartz container is connected on reaction unit, whole system is first vacuumized while is passed through before reaction Condensed water maintenance system constant temperature, zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution persistently generates hydrogen under Xe light irradiations Gas carries out on-line analysis by the TCD detectors of gas chromatograph, reacts 5h hydrogen outputs up to 789.39 μm of olg-1·h-1
Embodiment 4
1.1271g thioacetamides are weighed in the beaker of 80mL, add in the mixed of the prepared absolute ethyl alcohols of 50mL and glycerine Solution is closed, and magnetic agitation to solution is clarified, and adds 1.3630g zinc chloride, continues mixed liquor to be transferred to after stirring 10min 10h is reacted in 180 DEG C in 100mL ptfe autoclaves, cooled to room temperature after the completion of reaction is separated by filtration, uses water With ethyl alcohol alternately cleaning 3 times, zinc sulphide photochemical catalyst is then obtained for 24 hours in 60 DEG C of dryings.
Weigh 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions(The volume ratio of wherein deionized water and lactic acid is 3:1)It is placed in the 100mL quartz containers of top light-permeable, is dispersed in zinc sulphide photochemical catalyst by magnetic stirring apparatus In reaction solution, smear vacuum grease and quartz container is connected on reaction unit, whole system is first vacuumized while is passed through before reaction Condensed water maintenance system constant temperature, zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution persistently generates hydrogen under Xe light irradiations Gas carries out on-line analysis by the TCD detectors of gas chromatograph, reacts 5h hydrogen outputs up to 252.59 μm of olg-1·h-1
Embodiment 5
1.5028g thioacetamides are weighed in the beaker of 80mL, add in the mixed of the prepared absolute ethyl alcohols of 50mL and glycerine Solution is closed, and magnetic agitation to solution is clarified, and adds 1.3630g zinc chloride, continues mixed liquor to be transferred to after stirring 10min 10h is reacted in 180 DEG C in 100mL ptfe autoclaves, cooled to room temperature after the completion of reaction is separated by filtration, uses water With ethyl alcohol alternately cleaning 3 times, zinc sulphide photochemical catalyst is then obtained for 24 hours in 60 DEG C of dryings.
Weigh 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions(The volume ratio of wherein deionized water and lactic acid is 3:1)It is placed in the 100mL quartz containers of top light-permeable, is dispersed in zinc sulphide photochemical catalyst by magnetic stirring apparatus In reaction solution, smear vacuum grease and quartz container is connected on reaction unit, whole system is first vacuumized while is passed through before reaction Condensed water maintenance system constant temperature, zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution persistently generates hydrogen under Xe light irradiations Gas carries out on-line analysis by the TCD detectors of gas chromatograph, reacts 5h hydrogen outputs up to 179.98 μm of olg-1·h-1
Basic principle, main features and advantages embodiment above describes the present invention, the technical staff of the industry should Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, these changes and improvements are each fallen within In the scope of protection of the invention.

Claims (2)

1. the method that zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution prepares hydrogen, it is characterised in that concretely comprise the following steps:It weighs 0.05g zinc sulphide photochemical catalyst and 80mL lactic acid aqueous solutions are placed in the 100mL quartz containers of top light-permeable, are stirred by magnetic force Mixing device makes zinc sulphide photochemical catalyst be dispersed in reaction solution, smears vacuum grease and quartz container is connected on reaction unit, Whole system first vacuumizes while is passed through condensed water maintenance system constant temperature before reaction, the zinc sulphide photocatalysis under Xe light irradiations Agent photocatalysis lactic acid aqueous solution persistently generates hydrogen, and reaction 5h hydrogen outputs reach 789.39 μm of olg-1·h-1, the vulcanization The specific preparation process of zinc photochemical catalyst is:0.7513g thioacetamides are weighed in the beaker of 80mL, 50mL is added in and prepares Absolute ethyl alcohol and glycerine mixed solution, magnetic agitation to solution clarify, add 1.3630g zinc chloride, continue to stir Mixed liquor is transferred in 100mL ptfe autoclaves after 10min and reacts 10h in 180 DEG C, is naturally cooled to after the completion of reaction Room temperature is separated by filtration, then dry for 24 hours up to zinc sulphide photochemical catalyst in 60 DEG C with water and ethyl alcohol alternately cleaning 3 times.
2. the method that zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution according to claim 1 prepares hydrogen, feature It is:Deionized water and the volume ratio of lactic acid are 3 in the lactic acid aqueous solution:1.
CN201711310821.5A 2017-12-11 2017-12-11 The method that zinc sulphide photochemical catalyst photocatalysis lactic acid aqueous solution prepares hydrogen Pending CN108069390A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114843563A (en) * 2022-02-24 2022-08-02 电子科技大学长三角研究院(湖州) Device for converting hydrogen produced by photocatalysis into electric energy and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102923760A (en) * 2012-12-02 2013-02-13 桂林理工大学 Ultrasonic/microwave synergistic constant-pressure solvothermal synthesis method of cubic-structure and hexagonal-structure nano ZnS semiconductor material
US20130224105A1 (en) * 2010-11-04 2013-08-29 Technical Institute of Physics and Chemistry of the Chinese Academy of Sciences Semiconductor photocatalyst for the photocatalytic reforming of biomass derivatives for hydrogen generation, and preparation and use thereof
CN103934005A (en) * 2014-04-30 2014-07-23 上海师范大学 Cuprous ion-doped zinc sulfide copper nanowire visible-light-driven photocatalyst as well as preparation method and application thereof
CN107349937A (en) * 2017-06-28 2017-11-17 西安交通大学 A kind of preparation method of graphene-based bimetallic sulfide nano composite photo-catalyst

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130224105A1 (en) * 2010-11-04 2013-08-29 Technical Institute of Physics and Chemistry of the Chinese Academy of Sciences Semiconductor photocatalyst for the photocatalytic reforming of biomass derivatives for hydrogen generation, and preparation and use thereof
CN102923760A (en) * 2012-12-02 2013-02-13 桂林理工大学 Ultrasonic/microwave synergistic constant-pressure solvothermal synthesis method of cubic-structure and hexagonal-structure nano ZnS semiconductor material
CN103934005A (en) * 2014-04-30 2014-07-23 上海师范大学 Cuprous ion-doped zinc sulfide copper nanowire visible-light-driven photocatalyst as well as preparation method and application thereof
CN107349937A (en) * 2017-06-28 2017-11-17 西安交通大学 A kind of preparation method of graphene-based bimetallic sulfide nano composite photo-catalyst

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114843563A (en) * 2022-02-24 2022-08-02 电子科技大学长三角研究院(湖州) Device for converting hydrogen produced by photocatalysis into electric energy and application thereof

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