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A kind of highly stable palladium-nickel carbon catalyst catalyzes the method for synthesizing vitamin E intermediate

A technology of carbon catalysts and vitamins, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, and preparation of organic compounds, etc. It can solve the problems of poor catalytic activity and selectivity, poor recovery of catalysts, and poor performance of catalyst recycling. Achieve the effects of avoiding competitive adsorption, improving anti-toxicity performance, and improving application performance

Active Publication Date: 2021-08-17
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these precious metal catalysts generally have problems such as poor catalyst recovery, relatively poor catalytic activity and selectivity, and poor recycling performance of the catalyst.

Method used

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  • A kind of highly stable palladium-nickel carbon catalyst catalyzes the method for synthesizing vitamin E intermediate
  • A kind of highly stable palladium-nickel carbon catalyst catalyzes the method for synthesizing vitamin E intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Add 100g of powdered activated carbon with a particle size of 200 to 400 meshes into 1000mL 5mol / L urea aqueous solution and soak for 6 hours, centrifuge in a centrifuge to remove excess urea aqueous solution in the carbon slurry, and then place the precipitate in an oven to dry at 80 °C for 10 hours to constant weight, and then cured at 650 °C for 4 h in a nitrogen atmosphere to obtain pretreated activated carbon.

[0024] 2. Dissolve 4.24g of nickel acetate in 200mL of deionized water, and stir evenly to obtain a nickel precursor solution; add 94.5g of pretreated activated carbon into the nickel precursor solution, soak for 4 hours under stirring conditions, and then add sodium hydroxide to adjust The pH of the impregnation system is 8.5, continue to stir for 2 hours and then filter, wash the filter cake with deionized water until neutral, dry it in an oven at 80°C to constant weight, and then activate it in a hydrogen atmosphere at 800°C for 3 hours to obtain activ...

Embodiment 2

[0028] 1. Add 100g of powdered activated carbon with a particle size of 200 to 400 mesh and soak in 800mL of 6mol / L urea aqueous solution for 4 hours, centrifuge in a centrifuge to remove excess urea aqueous solution in the carbon slurry, and then place the precipitate in an oven to dry at 80 °C for 8 hours to constant weight, and then cured at 680 °C for 4 hours in a nitrogen atmosphere to obtain pretreated activated carbon.

[0029] 2. Dissolve 8.48g of nickel acetate in 200mL of deionized water, and stir evenly to obtain a nickel precursor solution; add 93g of pretreated activated carbon to the nickel precursor solution, soak for 4.5h under stirring conditions, and then add sodium carbonate to adjust the impregnation The pH of the system is 8.5, continue to stir for 3 hours and then filter, wash the filter cake with deionized water until neutral, dry it in an oven at 80°C to constant weight, and then activate it in a hydrogen atmosphere at 600°C for 2.5h to obtain activated ...

Embodiment 3

[0033]1. Add 100g of powdered activated carbon with a particle size of 200 to 400 mesh into 1200mL 4mol / L urea aqueous solution and soak for 7 hours, centrifuge in a centrifuge to remove excess urea aqueous solution in the carbon slurry, and then place the precipitate in an oven to dry at 80 °C for 9 hours to constant weight, and then cured at 600 °C for 4 hours in a nitrogen atmosphere to obtain pretreated activated carbon.

[0034] 2. Dissolve 12.387g of nickel nitrate in 200mL of deionized water, and stir evenly to obtain a nickel precursor solution; add 92.5g of pretreated activated carbon into the nickel precursor solution, soak for 4 hours under stirring conditions, and then add sodium bicarbonate to adjust The pH of the impregnation system is 10, continue to stir for 4 hours and then filter, wash the filter cake with deionized water until neutral, dry it in an oven at 80°C to constant weight, and then activate it in a hydrogen atmosphere at 500°C for 3.5h to obtain Acti...

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Abstract

The invention discloses a method for catalyzing and synthesizing a vitamin E intermediate with a highly stable palladium-nickel carbon catalyst. The method uses palladium-nickel carbon as a catalyst to catalyze the hydrogenation of trimethylbenzoquinone to synthesize trimethylhydroquinone, wherein the catalyst Using powdered activated carbon as the carrier, the carrier is treated with urea, dried, and then cured at high temperature, then the pretreated activated carbon is first loaded with auxiliary metal nickel, and the activated carbon loaded with nickel is activated at high temperature; then the nickel carbon is loaded with active metal palladium, to obtain a catalyst precursor; and finally to obtain a catalyst through reduction with a reducing agent. Compared with the existing method, the method of the invention not only has high activity and selectivity of the catalyst, but also has stable performance of the catalyst, has good mechanical performance and is convenient for recovery and reuse.

Description

technical field [0001] The invention belongs to the technical field of vitamin E synthesis, in particular to a method for synthesizing vitamin E intermediates catalyzed by a highly stable palladium-nickel carbon catalyst. Background technique [0002] Vitamin E is one of the vitamins necessary for the human body but cannot be synthesized by itself. It plays an important role in regulating the reproductive function and anti-oxidation function of the human body, so it has become one of the three pillar products of the vitamin industry. [0003] The reduction of trimethylbenzoquinone to trimethylhydroquinone is an important step in the industrial production of vitamin E. In the traditional method, the process of reducing trimethylbenzoquinone to trimethylhydroquinone is realized by adding excess reducing agent. Due to the addition of excess reducing agent in this preparation method, the separation and purification process of the product is complicated, and the residual reducin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J37/02B01J37/08B01J37/18C07C37/07C07C39/08
CPCC07C37/07B01J27/24B01J37/0207B01J37/024B01J37/082B01J37/18B01J35/394B01J35/393C07C39/08
Inventor 张洁兰陈丹颜攀敦曾利辉曾永康
Owner XIAN CATALYST NEW MATERIALS CO LTD
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