CN107497486A - A kind of catalyst preparation of metal organogel supporting Pt and its application on photocatalysis hydrogen production - Google Patents
A kind of catalyst preparation of metal organogel supporting Pt and its application on photocatalysis hydrogen production Download PDFInfo
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- CN107497486A CN107497486A CN201710661498.XA CN201710661498A CN107497486A CN 107497486 A CN107497486 A CN 107497486A CN 201710661498 A CN201710661498 A CN 201710661498A CN 107497486 A CN107497486 A CN 107497486A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 42
- 239000002184 metal Substances 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 17
- 239000001257 hydrogen Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000007146 photocatalysis Methods 0.000 title abstract description 10
- 230000001699 photocatalysis Effects 0.000 title abstract description 10
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 57
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 11
- 159000000013 aluminium salts Chemical class 0.000 claims abstract description 5
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000006303 photolysis reaction Methods 0.000 claims abstract 2
- 230000015843 photosynthesis, light reaction Effects 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000013291 MIL-100 Substances 0.000 claims description 12
- 239000000499 gel Substances 0.000 claims description 11
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- -1 aluminum ions Chemical class 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000011240 wet gel Substances 0.000 claims description 6
- 230000036571 hydration Effects 0.000 claims description 4
- 238000006703 hydration reaction Methods 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims description 3
- SWCIQHXIXUMHKA-UHFFFAOYSA-N aluminum;trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SWCIQHXIXUMHKA-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 230000035484 reaction time Effects 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000003599 detergent Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 14
- 125000005909 ethyl alcohol group Chemical group 0.000 description 12
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 230000002186 photoactivation Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 150000003639 trimesic acids Chemical class 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 230000001235 sensitizing effect Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- AYKOTYRPPUMHMT-UHFFFAOYSA-N silver;hydrate Chemical compound O.[Ag] AYKOTYRPPUMHMT-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
-
- 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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
- B01J31/2239—Bridging ligands, e.g. OAc in Cr2(OAc)4, Pt4(OAc)8 or dicarboxylate ligands
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/60—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
-
- 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
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/30—Complexes comprising metals of Group III (IIIA or IIIB) as the central metal
- B01J2531/31—Aluminium
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Dispersion Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to photocatalysis hydrogen production field, more particularly to a kind of method for preparing catalyst of the metal organogel supporting Pt based on MIL 100 (Al), including(1)Metal organogel is prepared as raw material using aluminium salt and trimesic acid;(2)The solution containing platinum ion is prepared, obtains solution A;(3)Solution A is slowly injected into metal organic gel materials, then lucifuge stands a period of time;(4)By the organic metal gel detergent after load, the catalyst of metal organogel supporting Pt is drying to obtain;(5)The catalyst of metal organogel supporting Pt is reacted for photolysis water hydrogen.Catalyst preparation of the present invention is simple, catalyst service life length, has big specific surface area, can effectively reduce reaction activity, can dramatically speed up light-catalyzed reaction process.
Description
Technical field
The invention belongs to photocatalysis hydrogen production field, technology is related to metal organogel, and particularly one kind is based on MIL-100
(Al) metal organogel(MOG)The preparation method of supporting Pt and its application in terms of photocatalysis hydrogen production.
Background technology
Under the background that science and technology develops rapidly with industrialized level, the mankind were also just former for the degree of dependence of the energy
The speed not having increases.Undue use fossil energy, not only consumes the only surplus resource of the earth, the thing followed also has
Problem of environmental pollution, the serious life for having had influence on people of these problems.Nowadays, want solution and concern whole mankind's existence
With the ultimate problem of development, unique approach is exactly to find new reproducible clean energy resource, and solar energy become one
It now appear that optimal selection.
By the utilization to luminous energy, chemical energy, especially Hydrogen Energy are converted light energy into, can solve above-mentioned ask well
Topic.The method for making it have photocatalysis performance to Photocatalyst and with the means of dye sensitization by using MOGs materials,
The new photochemical catalyst applied to photocatalysis hydrogen production field is prepared, more efficient photochemical catalyst is desirably to obtain, effectively carries
Rise the catalyst activity of photocatalysis hydrogen production reaction.
Metal organogel(MOG)It is that metallo-organic compound particle is acted on by Van der Waals force, intermolecular force etc.
Power is self-assembly of irregular tridimensional network in space.It has big specific surface area and synthesis is simple, as urging
There is very big potential application in terms of the carrier of agent.
The content of the invention
It is an object of the invention to prepare a kind of metal organogel for being based on MIL-100 (Al)(MOG)Supporting Pt is urged
Agent, use it for photocatalysis hydrogen production.This catalyst preparation is simple, can effectively improve photocatalysis hydrogen production speed, and is one
Kind different-phase catalyst, separated and recovered after catalysis simple.
The method for preparing catalyst of metal organogel supporting Pt of the one kind based on MIL-100 (Al), can be as follows
Carry out.
(1)By trimesic acid dissolving in a solvent, the solution containing trimesic acid is prepared.
(2)Aluminium salt dissolves in a solvent, and preparation contains aluminum ions solution.
(3)By step(1)The solution of gained pours into step(2)In the solution of gained, stirring at room temperature makes it for a period of time
It is sufficiently mixed, is then transferred in reactor, a period of time is reacted under high temperature, you can obtains wet solidifying based on MIL-100 (Al)
Glue, then wet gel is washed three times with ethanol.
(4)Six hydration platinum acid chloride solutions are prepared, obtain solution A.
(5)Solution A is slowly injected into step(3)In wet gel after washing three times, lucifuge is stood.
(6)By step(5)Obtained wet gel washing, dries the catalyst that can obtain xerogel supporting Pt.
(7)Sensitising agent is dissolved in water, prepares the solution containing sensitising agent.
(8)Take triethanolamine to be added in the light reaction container of the solution prepared equipped with step 7, add step(6)
In the obtained catalyst of xerogel supporting Pt.
(9)Photoactivation analysis system records the process of catalytic reaction.
Further, step of the present invention(1)And step(2)In used solvent be ethanol.
Further, step of the present invention(2)In aluminium salt be ANN aluminium nitrate nonahydrate.
Further, step of the present invention(3)In, the mol ratio of aluminium ion and trimesic acid is 1.5 ~ 2:1.
Further, step of the present invention(3)In high temperature be 140 DEG C, the time be 6 hours.
Further, step of the present invention(4)The middle solvent prepared used in six nitric hydrate silver solution is absolute ethyl alcohol,
The dosage of six hydration chloroplatinic acids(Quality)For the 4/100 of xerogel.
Further, step of the present invention(5)In lucifuge time of repose be 36-48 hours.
Further, step of the present invention(6)Middle drying condition is lower 80 DEG C of vacuum.
Further, step of the present invention(7)Middle sensitising agent is that rhodamine B dosage is the ppm of 100 ppm ~ 250.Enter one
Step ground, step of the present invention(8)Middle triethanolamine volume fraction is 10%.
Research finds, Pt beaded catalysts of receiving have an extensive prospects for commercial application, Pt nano particle due to its high surface from
Decline catalytic activity by that agglomeration easily can occur in the reaction, so before supported Pt catalysts are with more application
Scape.Metal organogel is a kind of porous material, have higher specific surface area and can modulation pore passage structure.
The catalyst of metal organogel supporting Pt prepared by the present invention, the active site of metal organogel and compared with
High specific surface area, the degree of scatter of active component Pt nano particle can be improved and avoid it from reuniting so that the metal of preparation has
The catalyst of machine gel supporting Pt is that usage amount seldom can also have superior catalytic performance during the course of the reaction.
Brief description of the drawings
Fig. 1 is wet gel figure before embodiment 2 loads(A)And the catalyst pictorial diagram dried after load(B).
Fig. 2 is the front and rear XRD of the metal organogel of embodiment 2 load.
Fig. 3 is the TEM figures after metal organogel supporting Pt made from the embodiment of the present invention 2.
Fig. 4 is the catalyst of metal organogel supporting Pt made from the embodiment of the present invention 2 under different rhodamine B concentration
Hydrogen-producing speed.
Embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
0.4856g ANN aluminium nitrate nonahydrates [Al (NO are weighed first3)3·9H2O] it is fully dissolved in 8mL absolute ethyl alcohols;Weigh
0.2101g trimesic acids are dissolved in 8mL absolute ethyl alcohols;Both of which ultrasound is to being completely dissolved, after then former solution is poured into
In person's solution, mixed solution is stirred at room temperature on magnetic stirring apparatus to 5 minutes to well mixed.Then mixed solution is transferred to
In 30mL reactors, 140 DEG C of insulation 6h in air dry oven are put into, are cooled down, washing, it is possible to obtain metal organogel.Connect
Weigh 0.0121g six be hydrated chloroplatinic acid be dissolved completely in 15mL absolute ethyl alcohols, obtain platinum acid chloride solution.By platinum acid chloride solution
It is slowly injected into the beaker equipped with gel, its lucifuge is then stood into 36h, washed three times with absolute ethyl alcohol, you can loaded
There is Pt metal organogel.The metal organogel for being loaded with Pt of above-mentioned gained is dried in vacuo 12h at 80 DEG C
Obtain the catalyst of metal organogel supporting Pt.Compound concentration is 100 ppm rhodamine B solution, takes above-mentioned solution 72mL
Into light reaction container, 8mL triethanolamine is added, photoactivation analysis system records the process of catalytic reaction.Produce hydrogen speed
Rate is 139.64 μm of olg-1h-1。
Embodiment 2
0.4856g ANN aluminium nitrate nonahydrates [Al (NO are weighed first3)3·9H2O] it is fully dissolved in 8mL absolute ethyl alcohols;Weigh
0.2101g trimesic acids are dissolved in 8mL absolute ethyl alcohols;Both of which ultrasound is to being completely dissolved, after then former solution is poured into
In person's solution, mixed solution is stirred at room temperature on magnetic stirring apparatus to 5 minutes to well mixed.Then mixed solution is transferred to
In 30mL reactors, 140 DEG C of insulation 6h in air dry oven are put into, are cooled down, washing, it is possible to obtain metal organogel.Connect
Weigh 0.0121g six be hydrated chloroplatinic acid be dissolved completely in 15mL absolute ethyl alcohols, obtain platinum acid chloride solution.By platinum acid chloride solution
It is slowly injected into the beaker equipped with gel, its lucifuge is then stood into 36h, washed three times with absolute ethyl alcohol, you can loaded
There is Pt metal organogel.The metal organogel for being loaded with Pt of above-mentioned gained is dried in vacuo 12h at 80 DEG C
Obtain the catalyst of metal organogel supporting Pt.Compound concentration is 150 ppm rhodamine B solution, takes above-mentioned solution 72mL
Into light reaction container, 8mL triethanolamine is added, photoactivation analysis system records the process of catalytic reaction.Produce hydrogen speed
Rate is 340.63 μm of olg-1h-1。
Embodiment 3
0.4856g ANN aluminium nitrate nonahydrates [Al (NO are weighed first3)3·9H2O] it is fully dissolved in 8mL absolute ethyl alcohols;Weigh
0.2101g trimesic acids are dissolved in 8mL absolute ethyl alcohols;Both of which ultrasound is to being completely dissolved, after then former solution is poured into
In person's solution, mixed solution is stirred at room temperature on magnetic stirring apparatus to 5 minutes to well mixed.Then mixed solution is transferred to
In 30mL reactors, 140 DEG C of insulation 6h in air dry oven are put into, are cooled down, washing, it is possible to obtain metal organogel.Connect
Weigh 0.0121g six be hydrated chloroplatinic acid be dissolved completely in 15mL absolute ethyl alcohols, obtain platinum acid chloride solution.By platinum acid chloride solution
It is slowly injected into the beaker equipped with gel, its lucifuge is then stood into 36h, washed three times with absolute ethyl alcohol, you can loaded
There is Pt metal organogel.The metal organogel for being loaded with Pt of above-mentioned gained is dried in vacuo 12h at 80 DEG C
Obtain the catalyst of metal organogel supporting Pt.Compound concentration is 200 ppm rhodamine B solution, takes above-mentioned solution 72mL
Into light reaction container, 8mL triethanolamine is added, photoactivation analysis system records the process of catalytic reaction.Produce hydrogen speed
Rate is 283.42 μm of olg-1h-1。
Embodiment 4
0.4856g ANN aluminium nitrate nonahydrates [Al (NO are weighed first3)3·9H2O] it is fully dissolved in 8mL absolute ethyl alcohols;Weigh
0.2101g trimesic acids are dissolved in 8mL absolute ethyl alcohols;Both of which ultrasound is to being completely dissolved, after then former solution is poured into
In person's solution, mixed solution is stirred at room temperature on magnetic stirring apparatus to 5 minutes to well mixed.Then mixed solution is transferred to
In 30mL reactors, 140 DEG C of insulation 6h in air dry oven are put into, are cooled down, washing, it is possible to obtain metal organogel.Connect
Weigh 0.0121g six be hydrated chloroplatinic acid be dissolved completely in 15mL absolute ethyl alcohols, obtain platinum acid chloride solution.By platinum acid chloride solution
It is slowly injected into the beaker equipped with gel, its lucifuge is then stood into 36h, washed three times with absolute ethyl alcohol, you can loaded
There is Pt metal organogel.The metal organogel for being loaded with Pt of above-mentioned gained is dried in vacuo 12h at 80 DEG C
Obtain the catalyst of metal organogel supporting Pt.Compound concentration is 250 ppm rhodamine B solution, takes above-mentioned solution 72mL
Into light reaction container, 8mL triethanolamine is added, photoactivation analysis system records the process of catalytic reaction.Produce hydrogen speed
Rate is 213.14 μm of olg-1h-1。
The preferred embodiment of the present invention is the foregoing is only, is not intended to limit the invention, for the technology of this area
For personnel, within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in
Within protection scope of the present invention.
Claims (6)
1. the method for preparing catalyst of organic metal gel supporting Pt of the one kind based on MIL-100 (Al), it is characterised in that by such as
Lower step is carried out:
(1)By trimesic acid dissolving in a solvent, the solution containing trimesic acid is prepared, by aluminium salt dissolving in a solvent, prepared
Contain aluminum ions solution;
(2)Solution containing trimesic acid is poured into containing in aluminum ions solution, stirring at room temperature makes it well mixed, then
It is transferred in reactor, after being reacted under high temperature, is washed with absolute ethyl alcohol and obtain the wet gel based on MIL-100 (Al);
(3)Six hydration platinum acid chloride solutions are prepared, are injected into the wet gel based on MIL-100 (Al), lucifuge stands 36-48 hours
After wash, at 80 DEG C, vacuum drying i.e. obtain the catalyst of xerogel supporting Pt.
2. the catalyst preparation side of the organic metal gel supporting Pt based on MIL-100 (Al) according to claims 1
Method, it is characterised in that:Step(1)Described in solvent be absolute ethyl alcohol, described aluminium salt is ANN aluminium nitrate nonahydrate.
3. the catalyst preparation side of the organic metal gel supporting Pt based on MIL-100 (Al) according to claims 1
Method, it is characterised in that:The step(2)The mol ratio of aluminium ion and trimesic acid is 1.5 ~ 2 in middle mixed solution:1;Equal benzene three
The molar concentration of acid solution is 0.1-0.3mmol/mL;The molar concentration of aluminium ion solution is 0.1-0.3mmol/mL.
4. the catalyst preparation side of the organic metal gel supporting Pt based on MIL-100 (Al) according to claims 1
Method, it is characterised in that:The step(2)In high temperature be 120-150 DEG C, the reaction time be 6 hours.
5. the catalyst preparation side of the organic metal gel supporting Pt based on MIL-100 (Al) according to claims 1
Method, it is characterised in that:The step(3)The middle solvent prepared used in six hydration chloroplatinic acids is absolute ethyl alcohol, and six are hydrated chloroplatinic acids
Quality be xerogel 4/100.
6. the organic metal gel supporting Pt based on MIL-100 (Al) being prepared described in claim any one of 1-6 is urged
Application of the agent on photolysis water hydrogen.
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CN103111262A (en) * | 2013-01-31 | 2013-05-22 | 北京大学 | Porous material of metal-organic framework and preparation method of material |
CN103240130A (en) * | 2013-05-21 | 2013-08-14 | 中国石油大学(北京) | TiO2 / MIL-101 composite catalyst for photocatalytic water splitting and preparation method and applications thereof |
CN106111198A (en) * | 2016-06-17 | 2016-11-16 | 三峡大学 | A kind of preparation method and applications of the catalyst of metal organic gel materials loaded Ag based on MIL 100 (Al) |
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