CN108927178A - A kind of In-situ sulphiding method of metal-organic framework material prepares the method and application of NiS/CdS composite catalyst - Google Patents
A kind of In-situ sulphiding method of metal-organic framework material prepares the method and application of NiS/CdS composite catalyst Download PDFInfo
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- CN108927178A CN108927178A CN201810644552.4A CN201810644552A CN108927178A CN 108927178 A CN108927178 A CN 108927178A CN 201810644552 A CN201810644552 A CN 201810644552A CN 108927178 A CN108927178 A CN 108927178A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1052—Nickel or cobalt catalysts
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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 present invention relates to a kind of NiS/CdS nanocomposites and preparation method thereof and the application in photocatalysis Decomposition aquatic products hydrogen, belong to technical field of new energy material preparation.The material decomposes the ability that water prepares hydrogen with excellent visible light catalytic in the case where non precious metal.The present invention passes through solvent thermal process first and prepares Nano cadmium sulphide, then Nano cadmium sulphide is wrapped in its internal gutter and load on the surface using when porous Ni-base metal-organic framework material in-situ preparation, it then is sulphur source using vulcanized sodium, In-situ sulphiding method prepares NiS/CdS composite material under thermal and hydric environment.Method for preparing catalyst of the present invention is simple, catalyst long service life, has 524μThe Photocatalyzed Hydrogen Production performance of mol/g, and the product of this method has yield big, with high purity, without post-processing, device therefor and simple process, synthesis condition are controllable, cost is relatively low, product yield is high.
Description
Technical field
The invention belongs to photolysis water hydrogen fields in new energy materials, and particular technique, which relates to the use of nano material and metal, to be had
The preparation method and applications of machine frame derivative In-situ reaction catalyst.
Background technique
In science and technology under the background of industrialized level rapid development, the mankind were also just former for the degree of dependence of the energy
The speed not having increases.Excessive use fossil energy not only consumes the resource that the earth only remains, and following there are also rings
Border pollution problem, these problems are serious to have influenced people's lives.Nowadays, to solve concerning the whole mankind existence with
The ultimate problem of development, unique approach are exactly to find new reproducible clean energy resource, and solar energy has become one existing
In optimal selection.
Being converted into chemical energy especially Hydrogen Energy using solar energy becomes the hot topic of field of renewable energy research, early in
In the early 1970s, Japanese Scientists Fujishima and Honda have found that photodissociation aquatic products hydrogen can occur for titanium dioxide electrodes
Phenomenon.In numerous optical response semiconductor materials, cadmium sulfide (CdS) as representative sulfide semiconductor material with its compared with
Narrow band gap (2.4eV) becomes good visible light-responded semiconductor material in photocatalysis field.However, cadmium sulfide is urged as light
Changing material, there is the low oxidability with photohole when being illuminated by the light of hydrogen-producing speed can arrive the negative sulfidion on its surface by force
It aoxidizes and photoetch occurs and limits the efficiency of its photochemical catalyzing.The catalyst of function admirable is often in light-catalyzed reaction
It needs that there is good light induced electron, photohole separative efficiency and high photo-generated carrier migration rate.Co-catalyst load
Important function is played to CdS photocatalysis Decomposition aquatic products hydrogen, since co-catalyst can not only accelerate light induced electron and hole
The rate of departure can also substantially reduce production Hydrogen over potential, so co-catalyst load strategy is improving CdS photochemical catalyzing
It is very necessary in hydrogen manufacturing.In the most of work reported at present, people often make in its area load noble metal such as Pt, Pd etc.
It is surface modified for co-catalyst, this measure can improve its photocatalysis performance to a certain extent really.Noble metal it is rare
Property and expensive property make it in practical application area by very big restriction.
Herein for above-mentioned state of the art, by utilizing nickel based metal organic framework materials in-stiu coating cadmium sulfide,
It then is sulphur source using vulcanized sodium, In-situ sulphiding method prepares NiS/CdS catalytic composite material under thermal and hydric environment.Experiment
As a result, it has been found that the NiS/CdS composite catalyst that this synthetic strategy is constructed has higher photocatalysis efficiency.
Summary of the invention
It is an object of the invention to prepare a kind of material using metal organic frame derivative composite sulfur cadmium, used
In photocatalysis hydrogen production system.This catalyst preparation is simple, can effectively improve photocatalytic water rate, and is a kind of heterocatalysis
Agent.
A kind of preparation method and applications using metal organic frame derivative composite sulfur cadmium, can as follows into
Row:
(1) inorganic cadmium salt and thiocarbamide are dissolved in ethylenediamine solvent, are washed after the reaction was completed, be dried to obtain 1-dimention nano
Rodlike CdS；
(2) by nano bar-shape CdS, 2,5- bis- (3,5- dicarboxyphenyi) benzoic acid prepared in (1) step, six water chlorinations
Nickel, mixed solvent wash after solvent thermal reaction in ptfe autoclave, are dried to obtain nickel based metal organic frame material
Material；
(3) the resulting nickel based metal organic framework materials of step (2) are placed in the reaction kettle equipped with sodium sulfide solution,
It reacts 6 hours, washs at 100-180 DEG C, it is dry to arrive NiS/CdS composite catalyst.
Inorganic cadmium salt described in the step (1) includes cadmium nitrate, cadmium acetate, any one in caddy,
In, the molar ratio of inorganic cadmium salt and thiocarbamide is 1:2~1:4.
Six water nickel chlorides used in materials synthesis and 2,5- bis- (3,5- dicarboxyphenyi) benzoic acid mole in the step (2)
Than for 2:0.5-1.2；
The mixed solvent includes n,N-Dimethylformamide, deionized water, six ring of Isosorbide-5-Nitrae-oxygen, N, N- dimethyl formyl
Amine, deionized water, the volume ratio of six ring of Isosorbide-5-Nitrae-oxygen are 2:0.5-1.5:0.5-1.5.
Six water nickel chlorides used in materials synthesis and (the 3,5- dicarboxyl benzene of 2,5- bis- in the further preferably described step (2)
Base) benzoic acid molar ratio be 2:1；Mixed solvent includes n,N-Dimethylformamide, deionized water, six ring of Isosorbide-5-Nitrae-oxygen, N, N- bis-
Methylformamide, deionized water, the volume ratio of six ring of Isosorbide-5-Nitrae-oxygen are 2:1:1.
The condition of solvent thermal reaction is 80-120 DEG C in step (2), and the reaction time is 65-80 hours, and drying condition is true
It is dry at 75-80 DEG C under empty condition.Further preferably the condition of solvent thermal reaction is 100 DEG C, and the reaction time is 72 hours,
Drying condition is dry at 80 DEG C under vacuum condition.
The temperature vulcanized in the step (3) can be in 100-180 DEG C of interval range.
The NiS/CdS composite catalyst that the preparation method of the NiS/CdS composite catalyst is prepared is cubic crystal
The crystalline material of system, space group P-1, cell parameter are as follows: α=90 °, β
=90 °, γ=90 °
The NiS/CdS that the preparation method of the NiS/CdS composite catalyst is prepared technical solution of the present invention
Composite catalyst produces the application on hydrogen in visible light photocatalysis.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the CdS nanometer material synthesized in embodiment 4.
The XRD comparison diagram for the CdS and NiS/CdS material that Fig. 2 is standard NiS, embodiment 4 synthesizes.
Fig. 3 is the high-resolution-ration transmission electric-lens photo of the NiS/CdS catalyst synthesized in embodiment 4.(left side is CdS's
(103) lattice fringe of crystal face, the right are the lattice fringe of (102) crystal face of NiS)
Fig. 4 is the relational graph of the NiS/CdS catalyst light application time and hydrogen output that synthesize in embodiment 4.
Specific embodiment
The present invention is further illustrated below with reference to embodiment, but the scope of protection of present invention is not limited to implement
The range of example statement, the raw material of the invention are commercially available.
Embodiment 1
(1) weigh four water cadmium nitrates: the addition that the ratio between amount of thiocarbamide substance is 1:2 is equipped in the beaker of 40mL ethylenediamine,
Magnetic agitation 30 minutes.Then acquired solution is transferred in the band polytetrafluoroethyllining lining reaction kettle of 50mL and is heated in 160 DEG C
Insulation reaction 24 hours.Resulting cadmium sulfide powder filter after reacting, is placed on three times with deionized water and ethanol washing
80 DEG C drying 24 hours, can be obtained cadmium sulfide raw material in vacuum oven.As shown in Figure 1, the CdS material microscopic appearance of synthesis
To be rodlike, by scanning electron microscope it can be concluded that the nanoscale of one-dimensional rod-like is about 30-50nm.
(2) the cadmium sulfide raw material 4mg prepared in above-mentioned steps (1), 2,5- bis- (3,5- dicarboxyphenyi) benzoic acid are weighed
20mg, six water nickel chloride 10mg are placed in 10mL vial, are then added N into bottle, N- dimethylformamide, deionized water,
Isosorbide-5-Nitrae-dioxane (total 6mL, volume ratio 2:1:1), bottle is placed in react 72 hours in 100 DEG C of baking oven obtains yellow green
Product, and disposably prepare 20 parts it is spare.Gained yellow green product is filtered, after being washed three times with deionized water and dehydrated alcohol
80 DEG C of dryings 24 hours are placed in a vacuum drying oven, the presoma of composite catalyst can be obtained.
(3) the nine water vulcanized sodium for weighing 1.20g, which are dissolved in 50mL deionized water, obtains sodium sulfide solution.Weigh above-mentioned step
Suddenly the presoma 420mg of yellow green composite catalyst obtained by (2) is added in sodium sulfide solution, and above-mentioned solution is transferred to
It is reacted 6 hours in reaction kettle of the 50mL with polytetrafluoroethyllining lining in 100 DEG C of heating.Gained black particle object is filtered, is spent
Ionized water and dehydrated alcohol washing postposition 80 DEG C drying 24 hours in a vacuum drying oven three times, it is compound to can be obtained NiS/CdS
Catalyst material.
Embodiment 2
The nine water vulcanized sodium for weighing 1.20g, which are dissolved in 50mL deionized water, obtains sodium sulfide solution.It weighs in embodiment 1
The presoma 420mg of yellow green composite catalyst obtained by step (2) is added in sodium sulfide solution, and above-mentioned solution is transferred to
It is reacted 6 hours in reaction kettle of the 50mL with polytetrafluoroethyllining lining in 120 DEG C of heating.Gained black particle object is filtered, is spent
Ionized water and dehydrated alcohol washing postposition 80 DEG C drying 24 hours in a vacuum drying oven three times, it is compound to can be obtained NiS/CdS
Catalyst material.
Embodiment 3
The nine water vulcanized sodium for weighing 1.20g, which are dissolved in 50mL deionized water, obtains sodium sulfide solution.It weighs in embodiment 1
The presoma 420mg of yellow green composite catalyst obtained by step (2) is added in sodium sulfide solution, and above-mentioned solution is transferred to
It is reacted 6 hours in reaction kettle of the 50mL with polytetrafluoroethyllining lining in 140 DEG C of heating.Gained black particle object is filtered, is spent
Ionized water and dehydrated alcohol washing postposition 80 DEG C drying 24 hours in a vacuum drying oven three times, it is compound to can be obtained NiS/CdS
Catalyst material.
Embodiment 4
The nine water vulcanized sodium for weighing 1.20g, which are dissolved in 50mL deionized water, obtains sodium sulfide solution.It weighs in embodiment 1
The presoma 420mg of yellow green composite catalyst obtained by step (2) is added in sodium sulfide solution, and above-mentioned solution is transferred to
It is reacted 6 hours in reaction kettle of the 50mL with polytetrafluoroethyllining lining in 160 DEG C of heating.Gained black particle object is filtered, is spent
Ionized water and dehydrated alcohol washing postposition 80 DEG C drying 24 hours in a vacuum drying oven three times, it is compound to can be obtained NiS/CdS
Catalyst material.As shown in Fig. 2, being CdS/NiS by the material that the standard card peak for comparing NiS and CdS can see synthesis
Composite material.As shown in Fig. 3, under high-resolution-ration transmission electric-lens, it can be seen that (102) crystal face of NiS and (103) of CdS are brilliant
Face, to more demonstrate the composition of material.
Embodiment 5
The nine water vulcanized sodium for weighing 1.20g, which are dissolved in 50mL deionized water, obtains sodium sulfide solution.It weighs in embodiment 1
The presoma 420mg of yellow green composite catalyst obtained by step (2) is added in sodium sulfide solution, and above-mentioned solution is transferred to
It is reacted 6 hours in reaction kettle of the 50mL with polytetrafluoroethyllining lining in 180 DEG C of heating.Gained black particle object is filtered, is spent
Ionized water and dehydrated alcohol washing postposition 80 DEG C drying 24 hours in a vacuum drying oven three times, it is compound to can be obtained NiS/CdS
Catalyst material.
Photocatalyzed Hydrogen Production performance test methods
Specific step is as follows: the composite catalyst sample for weighing 20mg is added to quartzy photolysis pond (band water-cooling jacket
Device), 8mL lactic acid is then added, 72mL deionized water stirs evenly.It is passed through nitrogen 30 minutes first before illumination test to remove
Oxygen in dereaction system, reaction temperature maintain 23 DEG C, after finally system being kept to vacuumize 30 minutes, in lasting stirring
Under the conditions of, light source, gaseous product (H are with the xenon lamp (300W) added with 420nm optical filter2) by the detection with gas chromatograph
Device TCD carries out on-line checking, every the primary production hydrogen activity data of hour acquisition.As shown in figure 4, the catalysis in embodiment 4
Agent has the Photocatalyzed Hydrogen Production performance of 524 μm of ol/g.
The above embodiments are only the preferred technical solution of the present invention, and are not construed as limitation of the invention, this Shen
Please in embodiment and embodiment in feature in the absence of conflict, can mutual any combination.It is any to be familiar with this technology
The variation that the technical staff in field can readily occur within the ideas and principles of the present invention, replacement and improvement should all be covered at this
In the protection scope of invention.
Claims (10)
1. a kind of method that the In-situ sulphiding method of metal-organic framework material prepares NiS/CdS composite catalyst, which is characterized in that benefit
The in-stiu coating CdS nanometer rods then step vulcanization reaction preparation in situ during hydrothermal growth with metal-organic framework material
NiS/CdS composite catalyst, specifically includes the following steps:
(1) inorganic cadmium salt and thiocarbamide are dissolved in ethylenediamine solvent, are washed after the reaction was completed, it is rodlike to be dried to obtain 1-dimention nano
CdS；
(2) by nano bar-shape CdS, 2,5- bis- (3,5- dicarboxyphenyi) benzoic acid prepared in (1) step, six water nickel chlorides,
Mixed solvent washs after solvent thermal reaction in ptfe autoclave, is dried to obtain nickel based metal organic framework materials；
(3) the resulting nickel based metal organic framework materials of step (2) are placed in the reaction kettle equipped with sodium sulfide solution, 100-
It reacts 6 hours, washs at 180 DEG C, it is dry to arrive NiS/CdS composite catalyst.
2. the preparation method of NiS/CdS composite catalyst according to claim 1, which is characterized in that described in step (1)
Inorganic cadmium salt include cadmium nitrate, cadmium acetate, any one in caddy, wherein the molar ratio of inorganic cadmium salt and thiocarbamide is
1:2~1:4.
3. according to the preparation method of NiS/CdS composite catalyst described in claims 1, which is characterized in that in the step (2)
Six water nickel chlorides used in materials synthesis and (3,5- dicarboxyphenyi) the benzoic acid molar ratio of 2,5- bis- are 2:0.5-1.2；
The mixed solvent includes n,N-Dimethylformamide, deionized water, six ring of Isosorbide-5-Nitrae-oxygen, n,N-Dimethylformamide,
Deionized water, the volume ratio of six ring of Isosorbide-5-Nitrae-oxygen are 2:0.5-1.5:0.5-1.5.
4. according to the preparation method of NiS/CdS composite catalyst described in claims 1, which is characterized in that in the step (2)
Six water nickel chlorides used in materials synthesis and (3,5- dicarboxyphenyi) the benzoic acid molar ratio of 2,5- bis- are 2:1；
The mixed solvent includes n,N-Dimethylformamide, deionized water, six ring of Isosorbide-5-Nitrae-oxygen, n,N-Dimethylformamide,
Deionized water, the volume ratio of six ring of Isosorbide-5-Nitrae-oxygen are 2:1:1.
5. according to the preparation method of NiS/CdS composite catalyst described in claims 1, which is characterized in that solvent in step (2)
The condition of thermal response is 80-120 DEG C, and the reaction time is 65-80 hours, and drying condition is to do at 75-80 DEG C under vacuum condition
It is dry.
6. according to the preparation method of NiS/CdS composite catalyst described in claims 1, which is characterized in that solvent in step (2)
The condition of thermal response is 100 DEG C, and the reaction time is 72 hours, and drying condition is dry at 80 DEG C under vacuum condition.
7. the preparation method of NiS/CdS composite catalyst according to claim 1, which is characterized in that vulcanization in step (3)
Temperature can be in 100-180 DEG C of interval range.
8. the NiS/CdS being prepared using the preparation method of the described in any item NiS/CdS composite catalysts of claim 1-7
Composite catalyst is the crystalline material of cubic system, space group P-1, cell parameter are as follows: α=90 °, β=90 °, γ=90 °
9. the NiS/CdS being prepared using the preparation method of the described in any item NiS/CdS composite catalysts of claim 1-7
Application of the composite catalyst on Photocatalyzed Hydrogen Production.
10. application as claimed in claim 9, the Photocatalyzed Hydrogen Production is that visible light photocatalysis produces hydrogen.
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| CN110090651A (en) * | 2019-05-29 | 2019-08-06 | 西安石油大学 | A kind of graphene-based sulfide heterojunction photocatalyst and its preparation method and application |
| CN110433866A (en) * | 2019-08-13 | 2019-11-12 | 云南大学 | A kind of Ni (OH)2Adulterate the composite photo-catalyst and the preparation method and application thereof of CdS |
| CN110586189A (en) * | 2019-08-13 | 2019-12-20 | 云南大学 | Composite photocatalyst of Ni doped CdS, preparation method and application thereof |
| CN111185199A (en) * | 2020-01-22 | 2020-05-22 | 天津理工大学 | Z-type heterojunction photocatalyst and preparation method and application thereof |
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| CN113634267A (en) * | 2021-08-27 | 2021-11-12 | 西安交通大学 | CdS/ZnS-NiS nanocluster photocatalyst and preparation method and application thereof |
| CN115193450A (en) * | 2022-08-16 | 2022-10-18 | 哈尔滨理工大学 | NiS quantum dot modified CdS/WO 3 Heterojunction photocatalyst and preparation method thereof |
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| CN115779932B (en) * | 2022-11-01 | 2024-04-02 | 陕西科技大学 | V-CdS/NiS 2 Preparation method of composite photocatalyst |
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