Trivalent gold complex and application thereof to hydrogen manufacturing through photocatalytic reduction water

A gold complex and chemical technology, applied in the field of photocatalyst, can solve the problems of poor ability to absorb visible light and slow catalytic rate

Active Publication Date: 2016-06-08
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional semiconductor photocatalysts have the characteristics of poor ability to absorb visible light and slow catalytic rate.

Method used

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  • Trivalent gold complex and application thereof to hydrogen manufacturing through photocatalytic reduction water
  • Trivalent gold complex and application thereof to hydrogen manufacturing through photocatalytic reduction water
  • Trivalent gold complex and application thereof to hydrogen manufacturing through photocatalytic reduction water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 0.43mmol[Au(C^N^C)Cl] and 0.1ml phenylacetylene (molar ratio is 1:2) were dissolved in 20mg cuprous iodide, 35mL dichloromethane and 2mL triethylamine molar ratio: 1 :5460:14 in the mixed solution of composition, stirred at room temperature for 6h, after the reaction was finished, the solvent was spin-dried and carried out chromatographic separation in a silica gel column with a volume ratio of 2:1 n-hexane and dichloromethane as the eluent, The trivalent gold complex was obtained through the recrystallization process.

[0033] The trivalent gold complex is carried out nuclear magnetic resonance (H spectrogram sees figure 1 ), measured: 1 HNMR (DMSO, 500MHz): δ8.16 (1H, t, J = 8.0), 7.98 (2H, d, J = 8.0), 7.90 (4H, t, J = 6.0), 7.54 (2H, d, J = 7.3), 7.41(4H,m), 7.33(3H,m). Elemental analysis, calculated value: C 25 h 16 NAu: C, 56.94; H, 3.06; N, 2.66. Calculated: C, 56.66; H, 3.07; N, 2.67. ESI-MS (Methanol): Found: 1076.83 [2×M+Na] + . Calculated value: 527.37. ...

Embodiment 2

[0035] Dissolve 0.52mmol[Au(C^N^C)Cl] and 0.79ml3,6-di-tert-butyl-9-(4-ethynylphenyl)-9H-carbazole in a molar ratio of 2:3 in In the mixed solution that 20mg cuprous iodide, 35mL dichloromethane and 2mL triethylamine form, stir 8h at room temperature, after the reaction finishes, after the solvent is spin-dried, in the silica gel column, be that the volume ratio is 2:1 n-hexane and Dichloromethane is used as the eluent for chromatographic separation, and the trivalent gold complex is obtained through the recrystallization process.

[0036] The trivalent gold complex is carried out nuclear magnetic resonance (H spectrogram sees figure 2 ), measured: 1 HNMR(DMSO,500MHz):δ8.31(2H,s),8.20(1H,s),7.99(4H,t,J=9.2),7.94(2H,s),7.80(2H,d,J=7.6 ),7.62(2H,d,J=7.9),7.52(2H,d,J=7.9),7.46(2H,s),7.38(4H,m),1.44(16H,s). Elemental analysis, calculated value :C 46 h 39 NAu: C, 68.74; H, 5.02; N, 1.74. Found: C, 68.48; H, 5.14; + . Calculated value: 804.77.

Embodiment 3

[0038] Mix 0.1mL phenylacetylene with 0.43mmol[Au(C^N^C)Cl], 0.38mmol[Au( t BuC^N^C t Bu)Cl] (molar ratio is 2:5) was added in the mixed solution that is made up of 20mg cuprous iodide, 35mL methylene chloride and 2mL triethylamine, stirred at room temperature for 6h, after the reaction was finished, the solvent was spin-dried Chromatographic separation was carried out on a silica gel column with n-hexane and dichloromethane at a volume ratio of 2:1 as the eluent, and the trivalent gold complex was obtained through recrystallization.

[0039] The trivalent gold complex is carried out nuclear magnetic resonance (H spectrogram sees image 3 ), measured: 1 HNMR (DMSO, 500MHz): δ8.10 (1H, t, J = 8.0), 8.04 (2H, d, J = 1.5), 7.86 (2H, d, J = 8.0), 7.81 (2H, d, J = 8.2), 7.49 (2H, d, J = 7.3), 7.42 (2H, t, J = 7.5), 7.35 (3H, m), 1.34 (18H, s). Elemental analysis, calculated value: C 33 h 32 NAu: C, 61.97; H, 5.04; N, 2.19. Found: C, 61.86; H, 5.12; + . Calculated value: 639.5...

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Abstract

The invention relates to a trivalent gold complex. The general chemical formula of the trivalent gold complex is MAuL, wherein M refers to 2,6-diphenyl pyridine or 2,6-bis(4-tertiary butyl phenyl) pyridine, L refers to phenylacetylene or 3,6-2-tertiary butyl-9-(4-acetenyl phenyl)-9H-carbazole. A preparation method comprises the steps that a chlorine gold (III) precursor and L are dissolved in a mixed solution formed by cuprous iodide, dichloromethane and triethylamine, stirring is carried out for 6 h to 12 h at room temperature, and after the reaction is finished, the reaction product is purified to obtain the trivalent gold complex. The trivalent gold complex achieves visible-light responses, and is a catalyst capable of fast reducing water to prepare hydrogen.

Description

technical field [0001] The invention relates to a trivalent gold complex and belongs to the technical field of photocatalysts. Background technique [0002] The development of today's society mainly relies on traditional fossil energy. The application of fossil energy promotes the development of society, but resources are increasingly depleted; at the same time, the unrestrained use of fossil energy has caused serious environmental pollution and climate change. The development and utilization of renewable new energy has become the focus of human attention. [0003] Solar energy has the characteristics of universal, harmless and long-term use, and is regarded as the clean energy with the most development potential in the 21st century. Whether hydrogen can be used as a fuel mainly depends on the hydrogen production process. Of all the ways to produce hydrogen, electrolysis of water can be used to produce hydrogen on a large scale. However, the hydrogen atoms in water molecu...

Claims

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Application Information

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IPC IPC(8): C07F1/12B01J31/22C01B3/04
CPCC01B3/042C07F1/00B01J31/0244B01J31/2286B01J2531/18C01B2203/0277C01B2203/1094C01B2203/1041B01J35/39Y02E60/36
Inventor 于振涛杨凌霞李永辉邹志刚
Owner NANJING UNIV
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