CN116444806A - Nickel-sulfur coordination polymer and preparation and application thereof - Google Patents
Nickel-sulfur coordination polymer and preparation and application thereof Download PDFInfo
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- 239000013256 coordination polymer Substances 0.000 title claims abstract description 23
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 23
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 23
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000006722 reduction reaction Methods 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 8
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 8
- 239000001294 propane Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- WHMDPDGBKYUEMW-UHFFFAOYSA-N pyridine-2-thiol Chemical compound SC1=CC=CC=N1 WHMDPDGBKYUEMW-UHFFFAOYSA-N 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 238000001308 synthesis method Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 2
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 5
- 235000019253 formic acid Nutrition 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 239000003504 photosensitizing agent Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000003446 ligand Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- 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
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1815—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine with more than one complexing nitrogen atom, e.g. bipyridyl, 2-aminopyridine
-
- 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
- B01J31/226—Sulfur, e.g. thiocarbamates
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
-
- 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
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/60—Reduction reactions, e.g. hydrogenation
- B01J2231/62—Reductions in general of inorganic substrates, e.g. formal hydrogenation, e.g. of N2
-
- 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
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/847—Nickel
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a nickel-sulfur coordination polymer and preparation and application thereof. The nickel-sulfur coordination polymer is prepared by adopting a hydrothermal method, and the chemical formula of the nickel-sulfur coordination polymer is [ Ni (1, 3-biim) (PySH) 2 ] n Is an orthorhombic system, and the space group isP 2 1 2 1 2 1 Unit cell parametersa=9.8295(3),b=13.1086(4),c=16.2948(6),α=90°,β=90°,γUnit cell volume =90°, z=8V=2099.60(12). The coordination polymer material shows good CO under the irradiation of visible light 2 Reduction performance.
Description
Technical Field
The invention belongs to the field of coordination polymer materials, and in particular relates to a nickel-sulfur coordination polymer and preparation thereof and application thereof in photocatalysis of CO 2 Use in reduction reactions.
Background
The main energy sources in the world still mainly adopt fossil energy sources, and the energy source structure inevitably brings about energy source shortage and CO while promoting the social development 2 Greenhouse effect caused by emission and the like. Solar energy is used as a renewable energy source, is green and clean, is widely distributed, and is one of the most potential methods for coping with the current dilemma, namely, converting solar energy into electric energy or chemical energy. CO is produced by artificial photocatalysis reaction by utilizing solar energy 2 Is reduced to CO, HCOOH, CH 4 Etc., not only can reduce CO 2 And the generated carbon-based product can be used as fuel, so that the energy crisis and the environmental problem are effectively relieved, and the recycling of resources is realized. Thus, photocatalytic CO 2 Reduction is receiving increasing attention. However, although photocatalytic CO has been in recent years 2 Great progress has been made in the field of reduction, but there is still a problem of low catalytic efficiency. Thus, the development of a highly active catalyst is photocatalytic CO 2 The key of the reduction.
The coordination polymer material has easily-controlled structure and functionThe method is characterized in that the catalytic activity of the material can be improved by regulating and controlling the metal center or the ligand structure, so that the method is a potential photocatalyst. Based on the method, the nickel-sulfur coordination polymer is synthesized in one step through simple hydrothermal reaction, the raw materials are low in price, the synthesis method is simple, pure crystals can be obtained through simple cleaning, and the pure crystals can be applied to a photocatalysis system taking water as a solvent and participating in an inexpensive organic photosensitizer, so that CO can be obtained 2 Reduced to HCOOH and exhibits good catalytic activity and selectivity.
Disclosure of Invention
The invention aims to provide a nickel-sulfur coordination polymer, a preparation method thereof and application thereof in photocatalysis.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a nickel-sulfur coordination polymer has a chemical formula of [ Ni (1, 3-biim) (PySH) 2 ] n Is an orthorhombic system, and the space group isP2 1 2 1 2 1 Unit cell parametersa= 9.8295(3),b= 13.1086(4)/>,c= 16.2948(6)/>,α= 90°,β= 90°,γUnit cell volume =90°, z=8V= 2099.60(12)/>The method comprises the steps of carrying out a first treatment on the surface of the Wherein, 1,3-biim is 1, 3-bis (1-imidazole) propane, and n is a positive integer.
The synthesis method of the nickel-sulfur coordination polymer comprises the steps of adding 2-mercaptopyridine, 1, 3-bis (1-imidazole) propane, a nickel source and an alkali source into deionized water, stirring, sealing and carrying out hydrothermal reaction; and after the reaction is finished, washing with deionized water and ethanol to obtain a blue target crystal.
Further, the molar ratio of the 2-mercaptopyridine, the 1, 3-bis (1-imidazole) propane, the nickel source and the alkali source is (0.9-1.0): 0.45-0.50): 0.9-1.0.
Further, the nickel source is NiCl 2 •6H 2 O. The alkali source is potassium hydroxide.
Further, the hydrothermal reaction is to heat from room temperature to 180 ℃ at a heating rate of 37.5 ℃/h, cool from 180 ℃ to 150 ℃ at a heating rate of 0.625 ℃/h, and finally cool from 150 ℃ to room temperature at a heating rate of 2.5 ℃/h.
The nickel-sulfur coordination polymer can be used in the field of photocatalysis reaction, and specifically can catalyze CO under the combined action of a photosensitizer and a sacrificial agent under the irradiation of visible light 2 Reduced to HCOOH.
The beneficial effects of this application are:
the invention prepares the nickel-sulfur coordination polymer [ Ni (1, 3-biim) (PySH) by a simple method 2 ] n . Under the combined action of the cheap photosensitizer and the sacrificial agent, the metal organic coordination polymer material can show good CO catalysis under the irradiation of visible light 2 Reduction performance and selectivity.
Drawings
FIG. 1 is a diagram of a nickel sulfur coordination polymer [ Ni (1, 3-biim) (PySH) of the present invention 2 ] n Is a schematic diagram of the structural element of (a). As can be seen, the crystal is not extended by N atoms at both ends of the 1, 3-bis (1-imidazole) propane ligand coordinated to Ni.
FIG. 2 is a diagram of a nickel sulfur coordination polymer [ Ni (1, 3-biim) (PySH) of the present invention 2 ] n Is an X-ray powder diffraction pattern of (c). Wherein a is a diffraction pattern obtained by fitting the analyzed crystal structure; b is a spectrum obtained by grinding the sample and then performing X-ray powder diffraction.
FIG. 3 is a nickel sulfur coordination polymer [ Ni (1, 3-biim) (PySH) prepared in example 1 of the present invention 2 ] n Photocatalytic CO in the presence of photosensitizers and sacrificial agents 2 Reduction performance comparison graph.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1 Synthesis of [ Ni (1, 3-biim) (PySH) by hydrothermal method 2 ] n Crystal body
As shown in Table 1, 2-mercaptopyridine, 1, 3-bis (1-imidazole) propane and NiCl were weighed in a molar amount 2 •6H 2 O and potassium hydroxide are added into a hydrothermal reaction tank, then 10 mL deionized water is added, and the mixture is stirred and sealed and heated, wherein the hydrothermal reaction is carried out under the conditions that the temperature is increased from room temperature to 180 ℃ at the heating rate of 37.5 ℃/h, then the temperature is reduced from 180 ℃ to 150 ℃ at the speed of 0.625 ℃/h, and then the temperature is reduced from 150 ℃ to room temperature at the speed of 2.5 ℃/h. After the reaction is finished, the blue crystal is obtained by alternately washing with deionized water and ethanol.
TABLE 1 sample [ Ni (1, 3-biim) (PySH) 2 ] n Is the synthesis condition of (2)
EXAMPLE 2 photocatalytic CO 2 Reduction Performance study
Weighing an appropriate amount of [ Ni (1, 3-biim) (PySH) prepared in example 1 2 ] n Is used as a catalyst and added into a catalyst containing a photosensitizer Na 2 Fl (2 mM) and a sacrificial agent TEA (5%, v/v) in water, and the pH of the solution was adjusted to 10, then the solution was transferred to a reaction flask, and the reaction product was subjected to photocatalytic reaction at 30℃and then detected by gas chromatography and nuclear magnetism, and the result is shown in FIG. 3.
As can be seen from FIG. 3, [ Ni (1, 3-biim) (PySH) 2 ] n Can effectively carry out CO for catalyst 2 Reduction and high selectivity of the product. HCOOH yields up to 20.83 mu mol g -1 ·h -1 HCOOH selectivity reaches 96.0%, only trace CO and CH 4 And (3) generating.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (8)
1. A nickel-sulfur coordination polymer is characterized in that the chemical formula of the nickel-sulfur coordination polymer is [ Ni (1, 3-biim) (PySH) 2 ] n Is an orthorhombic system, and the space group isP 2 1 2 1 2 1 Unit cell parametersa = 9.8295(3) ,b = 13.1086(4)/>,c = 16.2948(6)/>,α = 90°,β = 90°,γUnit cell volume =90°, z=8V = 2099.60(12) />The method comprises the steps of carrying out a first treatment on the surface of the Wherein, 1,3-biim is 1, 3-bis (1-imidazole) propane, and n is a positive integer.
2. A method for synthesizing the nickel-sulfur coordination polymer according to claim 1, wherein the hydrothermal reaction is performed by adding 2-mercaptopyridine, 1, 3-bis (1-imidazole) propane, a nickel source and an alkali source into deionized water, stirring and sealing; and after the reaction is finished, washing with deionized water and ethanol to obtain a blue target crystal.
3. The synthesis method according to claim 2, wherein the molar ratio of the 2-mercaptopyridine, the 1, 3-bis (1-imidazole) propane, the nickel source and the alkali source is (0.9-1.0): (0.45-0.50): (0.9-1.0).
4. A method of synthesis according to claim 2 or claim 3, wherein the nickel source is NiCl 2 •6H 2 O。
5. A method of synthesis according to claim 2 or claim 3, wherein the source of alkalinity is potassium hydroxide.
6. The method of claim 2, wherein the hydrothermal reaction is performed by heating from room temperature to 180 ℃, cooling from 180 ℃ to 150 ℃, and cooling from 150 ℃ to room temperature.
7. The method of synthesis according to claim 6, wherein the rate of temperature increase is 37.5 ℃/h, the first rate of temperature decrease is 0.625 ℃/h and the second rate of temperature decrease is 2.5 ℃/h.
8. A nickel-sulfur coordination polymer as claimed in claim 1 for photocatalytic CO 2 Use in reduction reactions.
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