A kind of carbon supported multi-component catalyst and its preparation method and application

A multi-component, catalyst technology, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the selectivity and yield of benzotriazole products The efficiency is not high, there are safety hazards, affecting product quality and other problems, to achieve high industrial application value, reduce catalyst cost, and reduce the effects of three wastes

Active Publication Date: 2018-06-29
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when Raney nickel is used as a hydrogenation catalyst, the selectivity and yield of benzotriazole products are not high; moreover, Raney nickel is flammable, and there are potential safety hazards during use
It has also been reported that carbon-supported noble metals are used as hydrogenation catalysts to synthesize benzotriazole products. Compared with Raney nickel catalysts, carbon-supported noble metal catalysts are safer. For example: CIBA GEIGY (patent US5276161) uses 5% Pt / C is the catalyst to catalyze hydrogenation to synthesize UV-P with a yield of 92%; patent US5104992 uses 5% Pd / C as a catalyst to hydrogenate UV-320 with a yield of 87.3%; patent EP0794179A1 uses 4% Pd / C+1% Pt / C is the catalyst for synthesizing UV-328. This patent can increase the product yield by adding hypophosphorous acid or sulfuric acid in the reduction system, but it needs to add a large amount of liquid acid (the molar ratio of acid / raw material is 3.0) in the reaction system, which will produce A lot of waste acid will pollute the environment, and the liquid acid added at the same time is likely to remain in the product, affecting product quality
[0016] It can be seen that the existing hydrogenation catalysts, whether they are Raney nickel catalysts or Pd / C, Pt / C catalysts, have defects such as low selectivity or the use of liquid acids.

Method used

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  • A kind of carbon supported multi-component catalyst and its preparation method and application
  • A kind of carbon supported multi-component catalyst and its preparation method and application
  • A kind of carbon supported multi-component catalyst and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Weigh 0.088g PdCl 2 , 0.132g H 2 PtCl 6 ·6H 2 O, 0.088g Cu(NO 3 ) 2 2H 2 O and 0.6g Potassium Citrate are put into there-necked flask; Add 150ml ethylene glycol in flask again and stir about 0.5h at room temperature, obtain precursor solution; Add 5g gac again in the prepared precursor solution, 25 Keep stirring and impregnating at a constant temperature at ℃ for 4 hours; after the impregnation is completed, add 5wt.% KOH / EG solution dropwise to adjust the pH value of the slurry to 10; then raise the temperature to 160°C and keep stirring at a constant temperature for 6 hours; after cooling, filter and use the filter cake Wash with deionized water until neutral; then vacuum-dry at 80°C for about 12 hours. That is, 5.125g of 1%Pd1%Pt0.5%Cu / C catalyst was obtained.

[0052] figure 1 It is the transmission electron microscope characterization figure of the catalyst 50nm scale that the present embodiment makes, from figure 1 It can be seen that the particle size of...

Embodiment 2

[0056] Weigh 0.066g PdCl 2 , 0.1g H 2 PtCl 6 ·6H 2 O, 0.088g Cu(NO 3 ) 2 2H 2 O and 0.5g Potassium Citrate are put into there-necked flask; Add 150ml ethylene glycol in flask again and stir about 0.5h at room temperature, obtain precursor solution; Then add 5g activated carbon in the prepared precursor solution, 25 Keep stirring and impregnating at a constant temperature at ℃ for 4 hours; after the impregnation is completed, add 5wt.% KOH / EG solution dropwise to adjust the pH value of the slurry to 10; then raise the temperature to 160°C and keep stirring at a constant temperature for 6 hours; after cooling, filter and use the filter cake Wash with deionized water until neutral; then vacuum-dry at 80°C for about 12 hours. That is, 5.1 g of 0.75% Pd0.75% Pt0.5% Cu / C catalyst was obtained.

Embodiment 3

[0058] Weigh 0.044g PdCl 2 , 0.066g H 2 PtCl 6 ·6H 2 O, 0.088gCu(NO 3 ) 2 2H 2 O and 0.4g Potassium Citrate are put into there-necked flask; Add 150ml ethylene glycol in flask again and stir about 0.5h at room temperature, obtain precursor solution; Add 5g gac again in the prepared precursor solution, 25 Keep stirring and impregnating at a constant temperature at ℃ for 4 hours; after the impregnation is completed, add 5wt.% KOH / EG solution dropwise to adjust the pH value of the slurry to 10; then raise the temperature to 160°C and keep stirring at a constant temperature for 6 hours; after cooling, filter and use the filter cake Wash with deionized water until neutral; then vacuum-dry at 80°C for about 12 hours. That is, 5.075 g of 0.5% Pd0.5% Pt0.5% Cu / C catalyst was obtained.

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Abstract

The invention provides a carbon-supported multi-component catalyst and a preparation method thereof. The catalyst is composed of a carrier and a metal active component loaded on the carrier, the carrier is activated carbon, and the metal active component is palladium and platinum. and a transition metal additive; based on the quality of the carrier activated carbon, the palladium loading is 0.5wt% to 5.0wt%, the platinum loading is 0.5wt% to 5.0wt%, and the transition metal additive loading is 0.1wt% ~2.5wt%; Simultaneously, the mass ratio of palladium and platinum is 1:0.5~2.0; Catalyst of the present invention can be used in catalytic hydrogenation synthesis benzotriazole ultraviolet absorber; High activity, high selectivity and yield of the target product, good stability, and less waste generated during the hydrogenation process.

Description

(1) Technical field [0001] The invention relates to a carbon-supported multi-component catalyst and a preparation method thereof. The carbon-supported multi-component catalyst can be applied to catalytic hydrogenation to synthesize benzotriazole-type ultraviolet absorbers. (2) Background technology [0002] Benzotriazole UV absorbers are the main varieties of plastic light stabilizers. They have excellent UV absorption capacity and can absorb UV rays with a wavelength of 290-400nm. And it has the advantages of lighter color, lower toxicity, less volatilization, good oil resistance, good compatibility with polymers, etc., and is widely used in polypropylene, polyethylene, polyvinyl chloride, polyoxymethylene, poly Photochemical modification of various synthetic materials such as amide, polystyrene, polyurethane, alkyd resin, etc. [0003] The synthesis of benzotriazole UV absorbers is a complex multi-step reaction. Firstly, the azo intermediate corresponding to the product ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J23/60B01J23/44B01J23/652C07D249/20
Inventor 丰枫郑红朝李小年朱宇翔张军华卢春山张群峰何火雷
Owner ZHEJIANG UNIV OF TECH
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