Carbon-supported multi-component catalyst and preparation method and application thereof

A multi-component, catalyst technology, applied in 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 rate is not high, there are potential safety hazards, and the quality of products is affected, so as to achieve high industrial application value, reduce catalyst costs, and reduce three wastes.

Active Publication Date: 2016-01-06
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: CIBAGEIGY (patent US5276161) uses 5% Pt / C Synthesis of UV-P by catalyst hydrogenation with a yield of 92%; patent US5104992 uses 5% Pd / C as catalyst to hydrogenate UV-320 with a yield of 87.3%; patent EP0794179A1 uses 4% Pd / C+1% Pt / C is a catalyst for the synthesis of UV-328. In this patent, adding hypophosphorous acid or sulfuric acid in the reducing system can improve the product yield, 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 relatively Too much waste acid pollutes the environment, and the liquid acid added at the same time tends 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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  • Carbon-supported multi-component catalyst and preparation method and application thereof
  • Carbon-supported multi-component catalyst and preparation method and application thereof
  • Carbon-supported multi-component catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Weigh 0.088gPdCl 2 , 0.132gH 2 PtCl 6 ·6H 2 O, 0.088gCu(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 th...

Embodiment 2

[0056] Weigh 0.066gPdCl 2 , 0.1gH 2 PtCl 6 ·6H 2 O, 0.088gCu(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 0.044gPdCl 2 , 0.066gH 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 prepared from a carrier and metal active components loaded on the carrier. The carrier is activated carbon. The metal active components comprise palladium, platinum and a transition metal element assistant. Based on the mass of the carrier, namely, the activated carbon, the capacity of palladium ranges from 0.5 wt% to 5.0 wt%, the capacity of platinum ranges from 0.5 wt% to 5.0 wt%, and the capacity of the transition metal element assistant ranges from 0.1 wt% to 2.5 wt%. Meanwhile, the mass ratio of palladium to platinum is 1:0.5-2.0. The catalyst can be applied to catalytic hydrogenation for synthesis of benzotriazole ultraviolet absorbent. The preparation method of the catalyst is easy and convenient, the catalytic activity is high, the selectivity and yield of target products are high, good stability is achieved, and meanwhile three wastes generated in the hydrogenation process are fewer.

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 Applications(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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