AU2021107286A4 - A KIND OF Pr-DOPED TITANIUM-OXO CLUSTER AND SYNTHESIS METHOD - Google Patents
A KIND OF Pr-DOPED TITANIUM-OXO CLUSTER AND SYNTHESIS METHOD Download PDFInfo
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- AU2021107286A4 AU2021107286A4 AU2021107286A AU2021107286A AU2021107286A4 AU 2021107286 A4 AU2021107286 A4 AU 2021107286A4 AU 2021107286 A AU2021107286 A AU 2021107286A AU 2021107286 A AU2021107286 A AU 2021107286A AU 2021107286 A4 AU2021107286 A4 AU 2021107286A4
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- doped titanium
- oxo cluster
- titanium
- oxo
- cluster
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- 238000001308 synthesis method Methods 0.000 title abstract description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 42
- 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 description 20
- NOXQKISUYACYGB-LNTINUHCSA-K (z)-4-oxopent-2-en-2-olate;praseodymium(3+) Chemical compound [Pr+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O NOXQKISUYACYGB-LNTINUHCSA-K 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims 4
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 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
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
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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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table 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
- 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
-
- 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
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0202—Polynuclearity
- B01J2531/0205—Bi- or polynuclear complexes, i.e. comprising two or more metal coordination centres, without metal-metal bonds, e.g. Cp(Lx)Zr-imidazole-Zr(Lx)Cp
-
- 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
- B01J2531/0216—Bi- or polynuclear complexes, i.e. comprising two or more metal coordination centres, without metal-metal bonds, e.g. Cp(Lx)Zr-imidazole-Zr(Lx)Cp
-
- 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
- B01J2531/38—Lanthanides other than lanthanum
-
- 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
- B01J2531/40—Complexes comprising metals of Group IV (IVA or IVB) as the central metal
- B01J2531/46—Titanium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the technical field of crystal material preparation, and specifically
involves a Pr-doped titanium-oxo cluster material and the corresponding synthesis method. Its
molecular formula of Pr-doped titanium-oxo cluster is Ti4Pr(p3 -0)3(OPr)2(OOCPh)12-(CH 3CN) 3,
in which OOCPh represents benzoate, OPr represents isopropanol group, and 3-0 represents
the three-bridged 0 atom. Furthermore, the Pr-doped titanium-oxo cluster crystallizes in the
triclinic system, space group of P-1, and the unit cell parameters are as followed: a=13.3779(4)
A, b=13.8571(4) A, c=23.9590(7) A, a=85.5795(17)°, P=82.9024(17)°, y=81.1510(16)°. Besides,
the obtained Pr-doped titanium-oxo cluster material has the excellent photocatalytic activity and
exhibits an extensive application prospect in the field of photocatalysis.
Description
A KIND OF Pr-DOPED TITANIUM-OXO CLUSTER AND SYNTHESIS METHOD
Field of the Invention
The invention belongs to the technical field of crystal material preparation, and specifically
involves a Pr-doped titanium-oxo cluster material and the corresponding synthesis method.
Background of the Invention
The energy crisis and environmental pollution are two serious challenges facing mankind.
Hence, it is imperative to develop clean and low carbon new energy such as solar energy. The
photocatalysis technology can directly convert solar energy into the chemical energy. The key of
this technology is the synthesis of stable and efficient photocatalysts. The nano-titanium dioxide
(TiO2) has been regarded as one of the most potential photocatalysts due to its low cost, high
efficiency and environmental friendliness. However, TiO 2 nanomaterial also has many
shortcomings that cannot be ignored, including unclear structural information, uneven particle
size and ambiguous inorganic-organic interface. Thus, these factors greatly hinder the in-depth
investigation of such photocatalyst.
In recent years, the crystalline titanium-oxo clusters have attracted much attention as the
molecular model compounds of TiO2 nanomaterial. However, there are fewer reports of
titanium-oxo clusters compared with other metal-oxo clusters, because of the high reactivity and
easy hydrolysis of the titanium source. Even the reported titanium-oxo clusters generally have
weak visible light absorption and wide band gaps, which severely limit their practical
photocatalytic application. The metal dopant can regulate the electronic structure and reduce the
band gap by introducing additional energy levels, thereby enhancing the photocatalytic activity
of titanium-oxo cluster. Therefore, the development of metal-doped titanium-oxo cluster
materials has the good economic and social benefits.
Summary of the Invention
In order to overcome the defects of the prior art, the invention provides a Pr-doped
titanium-oxo cluster, which has the precise structural information, excellent photocatalytic
activity and a broad application prospect in the field of photocatalysis.
Another object of the invention is to provide a facile method for synthesizing the Pr-doped
titanium-oxo cluster with the high yield and crystallinity.
In order to achieve the above purposes, the Pr-doped titanium-oxo cluster can be
synthesized by the following steps:
1) add the praseodymium acetylacetonate, benzoate and acetonitrile to a Teflon-lined
stainless-steel autoclave, followed by stirring for 0.3~0.7 h;
2) add the titanium isopropoxide into the above solution, subsequently react in a preheated
oven (80~120 °C) for 48~96 h, then cool down by air to 25 °C;
3) obtain the crystals of Pr-doped titanium-oxo cluster after separated and washed with the
acetonitrile for three times.
Z0 Preferably, the molecular formula of Pr-doped titanium-oxo cluster is
Ti 4Pr(p 3-0)3(O'Pr) 2 (OOCPh)12(CH 3CN) 3, in which OOCPh represents benzoate, O'Pr represents
isopropanol group, and 3-0 represents the three-bridged 0 atom.
Preferably, the crystal structure of Pr-doped titanium-oxo cluster crystallizes in the triclinic
system, space group of P-1, and the unit cell parameters are as follows: a=13.3779(4) A, b=13.8571(4) A, c=23.9590(7)X, a=85.5795(17), P=82.9024(17)0, y=81.1510(16)°.
Preferably, the ratio of titanium isopropoxide, praseodymium acetylacetonate, benzoate and
acetonitrile is: (0.05~0.15) mL: (0.01-0.03) g: 0.123 g: (4-6) mL.
Preferably, the cooling method of the Teflon-lined stainless-steel autoclave is naturally cooled.
Preferably, the obtained crystals of the Pr-doped titanium-oxo cluster are washed with acetonitrile for the three times.
Preferably, the Pr-doped titanium-oxo cluster can be applied in the field of photocatalysis.
Beneficial effects of the present disclosure
1) The Pr-doped titanium-oxo cluster has the precise structural information and excellent photocatalytic activity, and exhibits a broad application prospect in the field of photocatalysis. 2) The method for synthesizing the Pr-doped titanium-oxo cluster has the following advantages: the facile process and the product with high yield and crystallinity.
Brief Description of the Drawings
Fig. 1 is structure information of the Pr-doped titanium-oxo cluster obtained from the embodiment 2.
Fig. 2 is structure diagram of the Pr-doped titanium-oxo cluster obtained from the embodiment 2.
Detailed Description of the Embodiments
Unless otherwise specified, the technologies used in the invention are well-known methods for the technicians in the relevant fields. In addition, the embodiments should be understood as illustrative rather than limiting the scope of the invention, and the essence and scope of the invention are only limited by the claims. Besides, the raw materials and reagents used in the invention are commercially available.
In order to make the objectives and advantages of the invention clearer, the invention will
be further described in detail combined with the following embodiments.
Embodiment 1
The Pr-doped titanium-oxo cluster can be synthesized by the following steps:
1) add 10 mg of praseodymium acetylacetonate, 123 mg of benzoate and 4 mL of acetonitrile
to a Teflon-lined stainless-steel autoclave, followed by stirring for 0.3 h;
2) add 50 pL of titanium isopropoxide into the above solution, subsequently react in a
preheated oven (80 °C) for 96 h, then cool down by air to 25 °C;
3) obtain the crystals of Pr-doped titanium-oxo cluster after separated and washed with the
acetonitrile for three times.
The yield of the Pr-doped titanium-oxo cluster is 65%, which is obtained based on the amount of
titanium isopropoxide.
Embodiment 2
The Pr-doped titanium-oxo cluster can be synthesized by the following steps:
1) add 20 mg of praseodymium acetylacetonate, 123 mg of benzoate and 5 mL of acetonitrile
to a Teflon-lined stainless-steel autoclave, followed by stirring for 0.5 h;
2) add 100 tL of titanium isopropoxide into the above solution, subsequently react in a
preheated oven (100 °C) for 72 h, then cool down by air to 25 °C;
3) obtain the crystals of Pr-doped titanium-oxo cluster after separated and washed with the
acetonitrile for three times.
The yield of the Pr-doped titanium-oxo cluster is 75%, which is obtained based on the amount of
titanium isopropoxide.
Embodiment 3
The Pr-doped titanium-oxo cluster can be synthesized by the following steps:
1) add 30 mg of praseodymium acetylacetonate, 123 mg of benzoate and 6 mL of acetonitrile
to a Teflon-lined stainless-steel autoclave, followed by stirring for 0.7 h;
2) add 100 tL of titanium isopropoxide into the above solution, subsequently react in a
preheated oven (120 °C) for 48 h, then cool down by air to 25 °C;
3) obtain the crystals of Pr-doped titanium-oxo cluster after separated and washed with the
acetonitrile for three times.
The yield of the Pr-doped titanium-oxo cluster is 68%, which is obtained based on the amount of
titanium isopropoxide.
The molecular formula of the Pr-doped titanium-oxo cluster obtained from embodiments
1-3 is Ti4 Pr(t 3 -0)3 (O'Pr)2 (OOCPh)- 2 3 CN) 3 , in which OOCPh represents benzoate, .(CH OPr represents isopropanol group, and p3-0 represents the three-bridged 0 atom (Figs. 1 and 2).
Furthermore, the Pr-doped titanium-oxo cluster crystallizes in the triclinic system, space group of
P-1, and the unit cell parameters are as followed: a=13.3779(4)A, b=13.8571(4) A, c=23.9590(7)
A, a=85.5795(17)°, P=82.9024(17)°, y=81.1510(16)° (Fig. 1).
Claims (6)
1. A kind of Pr-doped titanium-oxo cluster, characterized in that the molecular formula of Pr-doped titanium-oxo cluster is Ti 4 Pr(p 3 -0)3 (OPr)2 (OOCPh) 12 (CH 3 CN) 3 , in which OOCPh
represents benzoate, O'Pr represents isopropanol group, and 3-0 represents the three-bridged 0 atom.
2. The Pr-doped titanium-oxo cluster mentioned in claim 1, characterized in that the Pr-doped titanium-oxo cluster crystallizes in the triclinic system, space group of P-1, and the unit cell parameters are as followed: a=13.3779(4) A, b=13.8571(4) A, c=23.9590(7) A, a=85.5795(17)°, P=82.9024(17)°, y=81.1510(16)°.
3. The Pr-doped titanium-oxo cluster mentioned in claim 1 or 2, characterized in that it can be obtained by the following synthetic method: 1) add the praseodymium acetylacetonate, benzoate and acetonitrile to a Teflon-lined stainless-steel autoclave, followed by stirring for 0.3~0.7 h; 2) add the titanium isopropoxide into the above solution, subsequently react in a preheated oven (80~120 C) for 48~96 h, then cool down by air to 25 °C; 3) obtain the crystals of Pr-doped titanium-oxo cluster after separated and washed with the acetonitrile for three times.
4. The synthetic method mentioned in claim 3, characterized in that the ratio of titanium isopropoxide, praseodymium acetylacetonate, benzoate and acetonitrile is: (0.05~0.15) mL: (0.01~0.03) g: 0.123 g: (4~6) mL.
5. The synthetic method mentioned in claim 3, characterized in that the cooling method of Teflon-lined stainless-steel autoclave is naturally cooled.
6. The synthetic method mentioned in claim 3, characterized in that the obtained crystals of Pr-doped titanium-oxo cluster are washed with acetonitrile for three times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021107286A AU2021107286A4 (en) | 2021-08-25 | 2021-08-25 | A KIND OF Pr-DOPED TITANIUM-OXO CLUSTER AND SYNTHESIS METHOD |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021107286A AU2021107286A4 (en) | 2021-08-25 | 2021-08-25 | A KIND OF Pr-DOPED TITANIUM-OXO CLUSTER AND SYNTHESIS METHOD |
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| Publication Number | Publication Date |
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| AU2021107286A4 true AU2021107286A4 (en) | 2021-12-09 |
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| AU2021107286A Ceased AU2021107286A4 (en) | 2021-08-25 | 2021-08-25 | A KIND OF Pr-DOPED TITANIUM-OXO CLUSTER AND SYNTHESIS METHOD |
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2021
- 2021-08-25 AU AU2021107286A patent/AU2021107286A4/en not_active Ceased
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