Visible light catalyst for catalyzing conversion of trichlorotoluene into ester and preparation method and application of visible light catalyst

A technology that catalyzes the conversion of trichlorotoluene into organic compounds, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., and can solve problems such as many side reactions and difficult to control reactions , to achieve good photoresponsiveness, wide spectral response, and good application prospects

Active Publication Date: 2019-04-16
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the reaction of converting methyl benzoate by trichlorotoluene needs to be obtained through a series of reflux and distillation at high temperature, the reaction is difficult to control, and there are many side reactions

Method used

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  • Visible light catalyst for catalyzing conversion of trichlorotoluene into ester and preparation method and application of visible light catalyst
  • Visible light catalyst for catalyzing conversion of trichlorotoluene into ester and preparation method and application of visible light catalyst
  • Visible light catalyst for catalyzing conversion of trichlorotoluene into ester and preparation method and application of visible light catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 A visible light catalyst N3-TiO that catalyzes the conversion of trichlorotoluene into esters 2 -B 12

[0026] (1) The preparation method is as follows:

[0027] 1. Vitamin B containing carboxyl groups 12 Preparation of derivatives:

[0028] Take 30ml of 98% concentrated sulfuric acid and slowly add it dropwise into 100ml of methanol, controlling the temperature at 0°C to 5°C. Then slowly add vitamin B 12 (commercially available, 2.0 g, 1.5 mmol) in 200 ml of methanol solution. After reflux for 72 h, the solution was concentrated to 100 ml, and saturated sodium carbonate solution was added dropwise to adjust the pH value to 7-8, and methanol was removed under reduced pressure. The remaining aqueous solution was extracted three times with carbon tetrachloride (3×100ml), the extracts were combined, and the solvent was removed to obtain ester group vitamin B 12 Derivatives [(CN)(H 2 O) Cob(III)7Cester]Cl, yield 1.1 g, yield 65%.

[0029] esterified vitam...

Embodiment 2

[0045] Example 2 A visible light catalyst N3-TiO that catalyzes the conversion of trichlorotoluene into ester 2 -B 12 Applications

[0046] Figure 5 For the complex N3-TiO 2 -B 12 Schematic illustration of the photocatalytic conversion of trichlorotoluene to esters.

[0047] Method: the N3-TiO prepared in Example 1 2 -B 12 (10mg) ultrasonically dispersed in 6ml trichlorotoluene (3×10 -3 mol / L) in methanol solution, and triethanolamine (0.2mol / L) was added thereto. Use xenon lamp with λ≥420nm filter as light source, 100mW / cm 2 , distance: 10cm, irradiation 20 ~ 60min. After the reaction finishes, the catalyst is centrifuged, and the centrifuged reaction solution is taken to add internal standard biphenyl, and the product and yield are determined by GC-MS and GC respectively, and the GC-MS spectrogram ( Figure 7 ) proves that the product is methyl benzoate. The relevant catalytic data are listed in Table 1.

[0048] Table 1 N3-TiO driven by visible light 2 -B 12 ...

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PUM

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Abstract

The invention relates to a visible light catalyst for catalyzing conversion of trichlorotoluene into ester and a preparation method and application of the visible light catalyst. According to the technical scheme, a vitamin B12 derivative and a photosensitizer ruthenium complex N3 are jointly adsorbed onto the surface of a TiO2 nanosphere, thereby obtaining the composite light catalyst with catalytic activity under the induction of visible light, and the catalyst can catalyze the trichlorotoluene to be dechlorinated completely under the irradiation of the visible light and convert the trichlorotoluene into an environment-friendly ester compound.

Description

technical field [0001] The invention belongs to the field of catalyst materials, and in particular relates to a photocatalyst with catalytic activity in the visible light region, a preparation method and application thereof. Background technique [0002] Trichlorotoluene is a very important organic intermediate, which has a wide range of applications in printing, agriculture, and organic synthesis. In the prior art, the reaction of converting trichlorotoluene into methyl benzoate needs to be obtained through a series of reflux and distillation at high temperature, the reaction is difficult to control, and there are many side reactions. At present, visible light catalysis for organic synthesis has attracted widespread attention. It is usually carried out at normal temperature and pressure, easy to operate, and generally does not produce secondary pollution, which opens up a new synthetic route for organic synthesis. Vitamin B 12 It and its derivatives are widely used in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C67/00C07C69/78
CPCC07C67/00B01J31/1691B01J31/1815B01J35/004C07C69/78
Inventor 张薇郭利梅郭欣吴阳吴抒遥宋溪明
Owner LIAONING UNIVERSITY
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