CN107497490B - Preparation method of metal organic gel loaded CdS catalyst and application of catalyst in hydrogen production through photolysis of water - Google Patents

Preparation method of metal organic gel loaded CdS catalyst and application of catalyst in hydrogen production through photolysis of water Download PDF

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CN107497490B
CN107497490B CN201710662013.9A CN201710662013A CN107497490B CN 107497490 B CN107497490 B CN 107497490B CN 201710662013 A CN201710662013 A CN 201710662013A CN 107497490 B CN107497490 B CN 107497490B
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CN107497490A (en
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赵君
秦正生
李东升
董文文
吴亚盘
张其春
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China Three Gorges University CTGU
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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
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
    • 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
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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    • 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
    • C—CHEMISTRY; METALLURGY
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    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C01B2203/1082—Composition of support materials
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    • 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

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Abstract

The invention belongs to the field of photocatalytic hydrogen production, and particularly relates to a preparation method of a metal organic gel CdS-loaded catalyst based on MIL-100(Al), which comprises the following steps of (1) preparing metal organic gel by taking aluminum salt and trimesic acid as raw materials; (2) preparing a solution containing cadmium ions to obtain a solution A; (3) slowly injecting the solution A into the metal organogel material, and then reacting at a high temperature for a period of time; (4) washing the loaded organic metal gel, and drying to obtain the catalyst of the metal organic gel loaded with CdS; (5) the catalyst with metal organic gel loaded with CdS is used for hydrogen production reaction by photolysis of water. The catalyst of the invention has the advantages of simple preparation, long service life, large specific surface area, effective reduction of reaction activation energy and remarkable acceleration of the photocatalytic reaction process.

Description

Preparation method of metal organic gel loaded CdS catalyst and application of catalyst in hydrogen production through photolysis of water
Technical Field
The invention belongs to the field of hydrogen production by photolysis of water, and relates to a metal organic gel, in particular to a preparation method of Metal Organic Gel (MOG) loaded CdS based on MIL-100(Al) and application thereof in hydrogen production by photolysis of water.
Background
With the development of industry and economy, the world faces an important problem: energy is lost. The development of new clean energy capable of being recycled is urgent, and the solar energy is converted into chemical energy and effectively stored, so that the solar energy has wide research prospects. Hydrogen energy is a recognized clean energy source that is emerging as a low carbon and zero carbon energy source. The hydrogen has the advantages of high calorific value and no pollution after combustion, and is considered to replace fossil fuel to become a new energy source in the future. Scientists around the world are striving to solve the problems of reducing the cost of hydrogen production and achieving industrialization of hydrogen production. The method for producing hydrogen by decomposing water through sunlight catalysis is an important research direction, and the key point is to find a proper catalyst. Therefore, preparing a cheap and efficient catalyst is an important problem to be solved by chemists engaged in research on photocatalytic hydrogen production for many years.
The above problems can be solved well by converting light energy into chemical energy, particularly hydrogen energy, by utilizing the light energy. By using the method of modifying the photocatalyst by using MOGs materials, the novel photocatalyst applied to the field of photocatalytic hydrogen production is prepared, so that the photocatalyst with higher efficiency is obtained, and the catalyst activity of the photocatalytic hydrogen production reaction is effectively improved.
Metal Organic Gels (MOGs) are irregular three-dimensional networks formed by the self-assembly of metal organic compound particles in space by van der waals forces, intermolecular forces, and the like. It has large specific surface area and simple synthesis, and has great potential application as the carrier of catalyst.
Disclosure of Invention
The invention aims to prepare a Metal Organic Gel (MOG) CdS-loaded catalyst based on MIL-100(Al), and the catalyst is used for photocatalytic hydrogen production. The catalyst is simple to prepare, can effectively improve the rate of photolysis of water, is a heterogeneous catalyst, and is simple to separate and recycle after catalysis.
A preparation method of a MIL-100(Al) -based metal organic gel CdS-loaded catalyst can be carried out according to the following steps.
(1) Trimesic acid is dissolved in a solvent to prepare a solution containing trimesic acid.
(2) The aluminum salt is dissolved in a solvent to prepare a solution containing aluminum ions.
(3) And (3) pouring the solution obtained in the step (1) into the solution obtained in the step (2), stirring at room temperature for a period of time to fully mix the solution, then transferring the solution into a 30mL reaction kettle, reacting at high temperature for a period of time to obtain MIL-100(Al) -based wet gel, and washing the wet gel with ethanol for three times.
(4) Preparing cadmium acetate solution to obtain solution A.
(5) And (4) drying the wet gel washed for three times in the step (3) to obtain dry gel.
(6) And (3) adding the xerogel obtained in the step (5) into the cadmium acetate solution obtained in the step (4), transferring the solution into a 40mL reaction kettle, reacting at a high temperature for a period of time, and washing and drying after the reaction to obtain the catalyst of the xerogel negative CdS.
(7) Adding the catalyst obtained in the step (6) into water to prepare a reaction solution containing the catalyst.
(8) Adding lactic acid into a photoreaction vessel containing the reaction solution prepared in step 7.
(9) The progress of the catalytic reaction was recorded with a photocatalytic analysis system.
Further, the solvent used in step (1) and step (2) of the present invention is ethanol.
Further, the aluminum salt in step (2) of the present invention is aluminum nitrate nonahydrate.
Further, in the step (3), the molar ratio of aluminum ions to trimesic acid is 1.5-2: 1.
Further, the high temperature in the step (3) of the present invention is 140 ℃ for 6 hours.
Furthermore, the solvent used for preparing the cadmium acetate in the step (4) of the invention is dimethyl sulfoxide, and the dosage (mass) of the cadmium acetate is 32/100 of xerogel.
Further, the drying condition in the step (5) of the present invention is 80 ℃ under vacuum.
Further, the high-temperature reaction temperature in the step (6) of the present invention is 210 ℃.
Further, the volume fraction of lactic acid in the step (8) of the present invention is 10%.
Researches find that the nano CdS particle catalyst has wide industrial application prospect, and the nano CdS has high surface free energy, and is easy to agglomerate in the reaction to reduce the catalytic activity, so that the supported CdS catalyst has more application prospect. The metal organic gel is a porous material, and has a high specific surface area and a tunable pore channel structure.
According to the catalyst of the metal organogel loaded with the CdS, the metal organogel has active sites and a higher specific surface area, the dispersion degree of active component nano CdS particles can be improved, the agglomeration of the active component nano CdS particles can be avoided, and the prepared catalyst of the metal organogel loaded with the CdS can have excellent catalytic performance even if the dosage is small in the reaction process.
Drawings
FIG. 1 is a physical diagram of a sample of gel-loaded CdS of example 2.
Figure 2 is an XRD pattern of the metal organogel loaded CdS sample of example 2.
FIG. 3 is a TEM image of the metal organogel loaded with CdS prepared in example 2 of the present invention.
FIG. 4 shows the hydrogen production rate of the catalyst of metal organogel loaded with CdS prepared in example 2 of the present invention.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
0.4936g of aluminum nitrate nonahydrate [ Al (NO) were first weighed3)3·9H2O]All dissolved in 8mL of absolute ethyl alcohol; 0.2101g of trimesic acid is weighed and dissolved in 8mL of absolute ethyl alcohol; both were sonicated to dissolve completely, then the former solution was poured into the latter solution and the mixed solution was stirred on a magnetic stirrer at room temperature for 5 minutes until well mixed. And then transferring the mixed solution into a 30mL reaction kettle, putting the reaction kettle into an air-blowing drying oven, preserving the temperature for 6h at 140 ℃, cooling, washing and drying to obtain the xerogel. 0.0614g of cadmium acetate was then weighed and dissolved completely in 30mL of dimethyl sulfoxide to obtain a cadmium acetate solution. And adding the xerogel into a solution containing cadmium acetate, transferring the solution into a 40mL reaction kettle, and reacting for 12h at 210 ℃ to obtain the metal organogel loaded with CdS. The obtained CdS-loaded metal organic gel is vacuumized at 80 DEG CDrying for 12h to obtain the catalyst of the metal organic gel loaded CdS. 100mL of a lactic acid solution with a volume fraction of 10% was prepared. Adding the dried gel into a light reaction container, adding the prepared dried gel loaded CdS catalyst for light catalytic reaction, and recording the progress of the catalytic reaction by using a light catalytic analysis system. The hydrogen production rate is 5.08 mmoleg-1。
Example 2
0.4936g of aluminum nitrate nonahydrate [ Al (NO) were first weighed3)3·9H2O]All dissolved in 8mL of absolute ethyl alcohol; 0.2101g of trimesic acid is weighed and dissolved in 8mL of absolute ethyl alcohol; both were sonicated to dissolve completely, then the former solution was poured into the latter solution and the mixed solution was stirred on a magnetic stirrer at room temperature for 5 minutes until well mixed. And then transferring the mixed solution into a 30mL reaction kettle, putting the reaction kettle into an air-blowing drying oven, preserving the temperature for 6h at 140 ℃, cooling, washing and drying to obtain the xerogel. 0.1228g of cadmium acetate was then weighed and dissolved completely in 30mL of dimethyl sulfoxide to obtain a cadmium acetate solution. And adding the xerogel into a solution containing cadmium acetate, transferring the solution into a 40mL reaction kettle, and reacting for 12h at 210 ℃ to obtain the metal organogel loaded with CdS. And (3) drying the obtained metal organogel loaded with the CdS at 80 ℃ for 12h in vacuum to obtain the catalyst of the metal organogel loaded with the CdS. 100mL of a lactic acid solution with a volume fraction of 10% was prepared. Adding the dried gel into a light reaction container, adding the prepared dried gel loaded CdS catalyst for light catalytic reaction, and recording the progress of the catalytic reaction by using a light catalytic analysis system. The hydrogen production rate is 14.51 mmoleg-1。
Example 3
0.4936g of aluminum nitrate nonahydrate [ Al (NO) were first weighed3)3·9H2O]All dissolved in 8mL of absolute ethyl alcohol; 0.2101g of trimesic acid is weighed and dissolved in 8mL of absolute ethyl alcohol; both were sonicated to dissolve completely, then the former solution was poured into the latter solution and the mixed solution was stirred on a magnetic stirrer at room temperature for 5 minutes until well mixed. And then transferring the mixed solution into a 30mL reaction kettle, putting the reaction kettle into an air-blowing drying oven, preserving the temperature for 6h at 140 ℃, cooling, washing and drying to obtain the xerogel. 0.0307g of acetic acid are weighed outCadmium is completely dissolved in 30mL of dimethyl sulfoxide to obtain a cadmium acetate solution. And adding the xerogel into a solution containing cadmium acetate, transferring the solution into a 40mL reaction kettle, and reacting for 12h at 210 ℃ to obtain the metal organogel loaded with CdS. And (3) drying the obtained metal organogel loaded with the CdS at 80 ℃ for 12h in vacuum to obtain the catalyst of the metal organogel loaded with the CdS. 100mL of a lactic acid solution with a volume fraction of 10% was prepared. Adding the dried gel into a light reaction container, adding the prepared dried gel loaded CdS catalyst for light catalytic reaction, and recording the progress of the catalytic reaction by using a light catalytic analysis system. The hydrogen production rate is 0.29 mmoleg-1。
Example 4
0.4936g of aluminum nitrate nonahydrate [ Al (NO) were first weighed3)3·9H2O]All dissolved in 8mL of absolute ethyl alcohol; 0.2101g of trimesic acid is weighed and dissolved in 8mL of absolute ethyl alcohol; both were sonicated to dissolve completely, then the former solution was poured into the latter solution and the mixed solution was stirred on a magnetic stirrer at room temperature for 5 minutes until well mixed. And then transferring the mixed solution into a 30mL reaction kettle, putting the reaction kettle into an air-blowing drying oven, preserving the temperature for 6h at 140 ℃, cooling, washing and drying to obtain the xerogel. 0.2456g of cadmium acetate was then weighed and dissolved completely in 30mL of dimethyl sulfoxide to obtain a cadmium acetate solution. And adding the xerogel into a solution containing cadmium acetate, transferring the solution into a 40mL reaction kettle, and reacting for 12h at 210 ℃ to obtain the metal organogel loaded with CdS. And (3) drying the obtained metal organogel loaded with the CdS at 80 ℃ for 12h in vacuum to obtain the catalyst of the metal organogel loaded with the CdS. 100mL of a lactic acid solution with a volume fraction of 10% was prepared. Adding the dried gel into a light reaction container, adding the prepared dried gel loaded CdS catalyst for light catalytic reaction, and recording the progress of the catalytic reaction by using a light catalytic analysis system. The hydrogen production rate is 11.78 mmoleg-1。
The above description is only a preferred example of the present invention, and should not be taken as limiting the invention, and any modifications, equivalents, improvements and the like made by those skilled in the art within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. A preparation method of a catalyst based on MIL-100(Al) organic metal gel loaded CdS for photolyzing water to produce hydrogen is characterized by comprising the following steps:
(1) dissolving trimesic acid in a solvent to prepare a solution containing trimesic acid, dissolving aluminum salt in the solvent to prepare a solution containing aluminum ions, pouring the solution containing trimesic acid into the solution containing aluminum ions, stirring at room temperature to uniformly mix the solution, transferring the solution into a reaction kettle, reacting at high temperature, and washing with absolute ethyl alcohol to obtain wet gel based on MIL-100 (Al);
(2) preparing a cadmium acetate solution, wherein a solvent for preparing the cadmium acetate is dimethyl sulfoxide, the mass of the cadmium acetate is 32/100 of xerogel, drying wet gel based on MIL-100(Al) to obtain xerogel, adding the xerogel into the cadmium acetate solution, then transferring into a reaction kettle, washing after high-temperature reaction at 200-250 ℃, and drying in vacuum at 80 ℃ to obtain the catalyst based on the organic metal gel loaded CdS of the MIL-100 (Al).
2. The method for preparing MIL-100(Al) -based organometallic gel CdS-supported catalyst according to claim 1, wherein: the solvent used in the step (1) is absolute ethyl alcohol; the aluminum salt is aluminum nitrate nonahydrate; the molar ratio of the aluminum ions to the trimesic acid is 1.5-2: 1; the molar concentration of the trimesic acid solution is 0.1-0.3 mmol/mL; the molar concentration of the aluminum ion solution is 0.1-0.3 mmol/mL.
3. The method for preparing MIL-100(Al) -based organometallic gel CdS-supported catalyst according to claim 1, wherein: the high temperature in the step (1) is 120-150 ℃, and the reaction time is 5-8 hours.
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