CN111574552B - Titanium oxide cluster-based coordination polymer and synthesis method and application thereof - Google Patents
Titanium oxide cluster-based coordination polymer and synthesis method and application thereof Download PDFInfo
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- 239000013256 coordination polymer Substances 0.000 title claims abstract description 42
- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 42
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 39
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000001308 synthesis method Methods 0.000 title claims abstract description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 19
- TWBYWOBDOCUKOW-UHFFFAOYSA-N isonicotinic acid Chemical compound OC(=O)C1=CC=NC=C1 TWBYWOBDOCUKOW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003446 ligand Substances 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/28—Titanium compounds
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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]
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- 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
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- 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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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/10—Complexes comprising metals of Group I (IA or IB) as the central metal
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
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Abstract
The invention belongs to the technical field of crystal material preparation, and particularly relates to a titanium oxide cluster-based coordination polymer, and a synthesis method and application thereof. The molecular formula of the titanium oxide cluster-based coordination polymer is Ti 3 O 12 C 30 N 3 H 47 And (4) CuBr. The specific synthesis steps are as follows: adding isopropyl titanate, cuprous bromide, an isonicotinic acid ligand and an acetonitrile solvent into a reaction kettle, stirring for 0.5-1.5 h at room temperature, reacting for 48-96h at 80-120 ℃, cooling to 25 ℃, precipitating blocky crystals in a system, separating, washing and drying to obtain the titanium oxide cluster-based coordination polymer. The titanium oxide cluster-based coordination polymer material prepared by the method has high stability and high catalytic activity, and shows good photocatalytic activity in a hydrogen production test by water splitting.
Description
Technical Field
The invention belongs to the technical field of preparation of crystal materials, and particularly relates to a titanium oxide cluster-based coordination polymer and a synthesis method and application thereof.
Background
Energy crisis and environmental pollution are two major challenges currently facing mankind, and the development of clean low-carbon new energy such as solar energy is imperative. The photocatalysis technology can directly convert solar energy into chemical energy, and the core of the technology is the synthesis of a stable and efficient photocatalyst. Nano titanium dioxide (TiO) 2 ) The material is considered as one of the most potential photocatalysts due to its characteristics of low cost, high efficiency and environmental friendliness. However, such TiO compounds 2 The material also has some non-negligible defects, such as wider energy band gap, faster recombination rate of photogenerated electron-hole pairs, shorter service life of photogenerated carriers and the like, which seriously limit the practical application of the material in the field of photocatalysis.
In recent years, titanium oxide cluster based coordination polymers have become one of the most attractive coordination polymers due to their wide application prospects in photocatalysis and optoelectronics. However, the development of titanium oxide cluster-based coordination polymers is still in the initial stage, and the reason is presumed to be as follows: (1) The high reactivity and easy hydrolysis of the titanium source lead to low crystallinity of the product and even difficult crystallization; (2) The higher charge/radius ratio (Z/r) of Ti (IV) causes the association/dissociation process reversibility of coordination bonds between titanium nodes and ligands to obstruct the formation of a high-crystallinity network structure. In order to make better use of solar energy, development of a novel titanium oxide cluster-based coordination polymer material which is highly efficient and stable has become an important research topic.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the titanium-oxygen-cluster-based coordination polymer, and the titanium-oxygen-cluster-based coordination polymer material has high stability and high catalytic activity, and has wide application prospects in the aspects of hydrogen production by photocracking water and the like.
The invention also aims to provide a synthesis method of the titanium oxide cluster-based coordination polymer, which has the characteristics of simple process, pure product, high yield, good crystallinity and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
a titanium oxide cluster-based coordination polymer, wherein the molecular formula of the titanium oxide cluster-based coordination polymer is Ti 3 O 12 C 30 N 3 H 47 CuBr。
Further, the crystal structure of the titanium oxide cluster-based coordination polymer is as follows: the crystal belongs to monoclinic system and has space group ofC2/cThe unit cell parameters are a =17.3730 a, b =19.2330 a, c =18.5000 a, α =90 °, β =109 °, γ =90 °.
The synthesis method of the titanium oxide cluster-based coordination polymer adopts the following steps: adding isopropyl titanate, cuprous bromide, an isonicotinic acid ligand and an acetonitrile solvent into a reaction kettle, stirring for 0.5-1.5 h at room temperature, reacting for 48-96h at 80-120 ℃, cooling to 25 ℃, precipitating blocky crystals in a system, separating, washing and drying to obtain the titanium oxide cluster-based coordination polymer.
Further, the mass-to-volume ratio of the isopropyl titanate, the cuprous bromide, the isonicotinic acid ligand and the acetonitrile solvent is as follows: (0.1 to 0.2) mL: (0.15 to 0.20) g:0.1g: (4 to 6) mL. .
Further, the temperature is reduced by adopting a program temperature control mode, and the temperature reduction rate is controlled to be 3 to 10 ℃/h.
Further, the washing is carried out for three times by adopting isopropanol; the drying is natural drying.
The application of the titanium oxygen cluster-based coordination polymer material can be applied to hydrogen production by photocracking water.
Advantageous effects
The titanium oxide cluster-based coordination polymer material has high stability and high catalytic activity, and has wide application prospect in the aspect of hydrogen production by photocracking water.
The synthesis method of the titanium oxide cluster-based coordination polymer has the characteristics of simple process, pure product, high yield, good crystallinity and the like.
Drawings
FIG. 1 is a graph showing X-ray single crystal ray diffraction data of a titanium oxide cluster-based coordination polymer prepared in example 2;
FIG. 2 is a view showing the structure of the titanium oxide cluster-based coordination polymer prepared in example 2 along the a-axis direction (a) and along the c-axis direction (b));
FIG. 3 is a thermogravimetric analysis chart of the titanium oxide cluster-based coordination polymer prepared in example 2;
FIG. 4 is an X powder diffraction pattern of the titanium oxide cluster-based coordination polymer prepared in example 2;
FIG. 5 is a test chart of hydrogen production by photocracking water of the titanium oxide cluster-based coordination polymer prepared in example 2.
Detailed Description
The invention is described below by means of specific embodiments. Unless otherwise specified, all technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications can be made in the components and amounts of the materials used in these embodiments without departing from the spirit and scope of the invention. The raw materials and reagents used in the present invention are commercially available.
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples.
Example 1
A method for synthesizing a titanium oxide cluster-based coordination polymer comprises the following steps:
adding 100 muL of isopropyl titanate, 150mg of cuprous bromide, 100mg of isonicotinic acid ligand and 4mL of acetonitrile solvent into a reaction kettle, and stirring for 0.5h at room temperature; reacting for 48 hours at the temperature of 80 ℃, and cooling to 25 ℃ at the speed of 3 ℃/h by a program, so that blocky crystals are separated out from the system; the obtained crystals were separated, washed three times with an isopropyl alcohol solvent, and naturally dried to obtain the titanium oxide cluster-based coordination polymer with a yield of 80% based on the amount of isopropyl titanate.
Example 2
Adding 150 mu L of isopropyl titanate, 175mg of cuprous bromide, 100mg of isonicotinic acid ligand and 5mL of acetonitrile solvent into a reaction kettle, and stirring at room temperature for 1.0h; reacting for 72 hours at 120 ℃, and cooling to 25 ℃ at the speed of 6 ℃/h by a program, and separating out blocky crystals in the system; the obtained crystals were separated, washed three times with an isopropyl alcohol solvent, and naturally dried to obtain the titanium oxide cluster-based coordination polymer with a yield of 82% based on the amount of isopropyl titanate.
Example 3
Adding 200 mu L of isopropyl titanate, 200mg of cuprous bromide, 100mg of isonicotinic acid ligand and 6ml of acetonitrile solvent into a reaction kettle, and stirring for 1.5h at room temperature; reacting for 96 hours at the temperature of 100 ℃, and cooling to 25 ℃ at the speed of 10 ℃/h by a program, and separating out blocky crystals in the system; the obtained crystals were separated, washed three times with an isopropyl alcohol solvent, and naturally dried to obtain the titanium oxide cluster-based coordination polymer with a yield of 78% based on the amount of isopropyl titanate.
Examples 1 to 3 above Synthesis of titanium oxide Cluster based Complex Polymer having the molecular formula Ti 3 O 12 C 30 N 3 H 47 CuBr。
The crystal structure of the titanium oxide cluster-based coordination polymer is as follows: the crystal belongs to monoclinic system and has space group ofC2/cUnit cell parameters a =17.3730 a, b =19.2330 a, c =18.5000 a, α =90 °, β =109 °, γ =90 °.
The titanium oxide cluster-based coordination polymer prepared in example 2 is subjected to structural characterization by using an X-ray single crystal diffractometer, and the crystallographic structural parameters are shown in figure 1; FIG. 2 is a structural diagram; thermogravimetric analysis shows that the prepared compound has stable structure within 450 ℃ (FIG. 3); the X-ray powder diffraction pattern showed that the experimental test data was substantially consistent with the theoretical simulation data, indicating that the prepared compound was pure and highly crystalline (fig. 4).
The titanium-oxygen cluster-based coordination polymer material is used for producing hydrogen by photocatalytic water splitting. The test was carried out in a closed gas circulation system using a 300W Xe lamp as a light source and methanol as a sacrificial agent, 30mg of the prepared titanium oxide cluster-based coordination polymer was dispersed in 90mL of water, and HPtCl was added 4 The hydrogen production was monitored by on-line gas chromatography at 1H intervals, and the test results showed that H 2 The yield is 80.1 mu mol/g/h, which shows that the prepared material has good photocatalytic activity.
Claims (6)
1. The titanium-oxygen cluster-based coordination polymer is characterized in that the molecular formula of the titanium-oxygen cluster-based coordination polymer is Ti 3 O 12 C 30 N 3 H 47 CuBr, the crystal structure of the titanium-oxygen cluster-based coordination polymer is as follows: the crystal belongs to monoclinic system and has space group ofC2/cThe unit cell parameters are a =17.3730 a, b =19.2330 a, c =18.5000 a, α =90 °, β =109 °, γ =90 °.
2. A method for synthesizing a titanium oxide cluster-based coordination polymer according to claim 1, characterized by comprising the steps of: adding isopropyl titanate, cuprous bromide, isonicotinic acid ligand and acetonitrile solvent into a reaction kettle, stirring for 0.5 to 1.5 hours at room temperature, reacting for 48 to 96hours at 80 to 120 ℃, cooling to 25 ℃, separating out blocky crystals in the system, separating, washing and drying to obtain the titanium oxo-cluster-based coordination polymer.
3. The synthesis method according to claim 2, wherein the mass-to-volume ratio of the isopropyl titanate, the cuprous bromide, the isonicotinic acid ligand and the acetonitrile solvent is as follows: (0.1 to 0.2) mL: (0.15 to 0.20) g:0.1g: (4 to 6) mL.
4. The synthesis method according to claim 2, wherein the temperature reduction is carried out in a programmed temperature control manner, and the temperature reduction rate is controlled to be 3 to 10 ℃/h.
5. The synthesis method according to claim 2, characterized in that the washing is three times with isopropanol; the drying is natural drying.
6. Use of a titanium oxide cluster-based coordination polymer according to claim 1, wherein said titanium oxide cluster-based coordination polymer material is used for photocracking water to produce hydrogen.
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CN110330523A (en) * | 2019-06-27 | 2019-10-15 | 浙江工业大学 | A kind of titanyl cluster monomer of the formic acid of -3- containing thiophene and its preparation and application |
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A cluster-based mesoporous Ti-MOF with sodalite supercages;Chao Wang et al.;《Chemical Communications》;20171002;第11670-11673页 * |
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