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A kind of method for catalyzing synthesis of biotin by a palladium-carbon catalyst with high mechanical activity

A palladium-carbon catalyst and synthetic biology technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. problem, to achieve the effect of reducing poisoning, superior performance and high activity

Active Publication Date: 2021-02-12
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problem to be solved by the present invention is to provide a method for catalytically synthesizing biotin with high catalytic activity, good catalyst recycling performance and easy recycling for the above-mentioned prior art palladium-carbon catalysts that are easily deactivated and cannot be applied mechanically.

Method used

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  • A kind of method for catalyzing synthesis of biotin by a palladium-carbon catalyst with high mechanical activity
  • A kind of method for catalyzing synthesis of biotin by a palladium-carbon catalyst with high mechanical activity

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 1. Roast the activated carbon in a tube furnace at 400°C for 6 hours under an ammonia atmosphere. Weigh 10 g of the obtained activated carbon and add it to 100 mL of hydrogen peroxide with a volume concentration of 5%. Stir at room temperature for 24 hours and then filter. Put the filtered wet carbon in an oven Dry at 150°C to constant weight; obtain pretreated activated carbon.

[0021] 2. Dilute 10mL of 0.1g / mL chloropalladium acid aqueous solution (the molar weight of palladium is 9.4mmol) to 150mL with deionized water, then add 1.44g (9.4mmol) of dopamine, reflux and stir in a water bath at 90°C for 2h, Cool to room temperature to obtain a palladium precursor solution.

[0022] 3. Add 9g of pretreated activated carbon to 200mL of ethanol aqueous solution with a volume concentration of 5% for beating, then add 150mL of palladium precursor solution dropwise to the carbon slurry under stirring conditions, and add aqueous sodium carbonate solution to control pH = 7, dro...

Embodiment 2

[0025] 1. Roast the activated carbon in a tube furnace at 450°C for 5 hours under an ammonia atmosphere. Weigh 10 g of the obtained activated carbon and add it to 100 mL of hydrogen peroxide with a volume concentration of 10%. Stir at room temperature for 24 hours and then filter. Put the filtered wet carbon in an oven Dry at 150°C to constant weight; obtain pretreated activated carbon.

[0026] 2. Dilute 10mL of 0.1g / mL chloropalladium acid aqueous solution (the molar weight of palladium is 9.4mmol) to 150mL with deionized water, then add 2.26g (37.6mmol) urea, reflux and stir in a 90°C water bath for 2h, Cool to room temperature to obtain a palladium precursor solution.

[0027] 3. Add 9g of pretreated activated carbon to 200mL of ethanol aqueous solution with a volume concentration of 20% for beating, then add 150mL of palladium precursor solution dropwise to the carbon slurry under stirring conditions, and add aqueous sodium hydroxide solution to control pH = 11.2, Stir f...

Embodiment 3

[0030] 1. Roast the activated carbon in a tube furnace at 500°C for 5 hours under an ammonia atmosphere. Weigh 10 g of the obtained activated carbon and add it to 100 mL of hydrogen peroxide with a volume concentration of 10%. Stir at room temperature for 24 hours and then filter. Put the filtered wet carbon in an oven Dry at 150°C to constant weight; obtain pretreated activated carbon.

[0031] 2. Dissolve 1.67g of soluble palladium chloride (the molar weight of palladium is 9.4mmol) in 150mL deionized water, then add 1.29g (4.69mmol) trisodium nitrilotriacetate, reflux and stir in a water bath at 90°C for 2h, and cool to room temperature to obtain a palladium precursor solution.

[0032] 3. Add 9g of pretreated activated carbon to 200mL of ethanol aqueous solution with a volume concentration of 50% to make a slurry, then add 150mL of palladium precursor solution dropwise to the carbon slurry under stirring conditions, and add ammonia water to control pH = 9, dropwise After ...

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Abstract

The invention discloses a method for catalytically synthesizing biotin with a palladium-carbon catalyst with high mechanical activity. The method uses palladium-carbon as a catalyst to catalyze the biotin intermediate cis-2-oxo-1,3-dibenzyl-4-1,3-dibenzyl-4- (4-carboxybut-1-ene)hexahydro-1H-thieno[3,4-d]imidazole is hydrogenated to synthesize biotin, wherein the catalyst uses activated carbon as a carrier, and after the carrier is treated at high temperature in an ammonia atmosphere, use Hydrogen peroxide is activated to obtain pretreated activated carbon; after the soluble palladium compound is dissolved in water, a nitrogen-containing compound is added, and reflux is stirred to obtain a palladium precursor solution; after the pretreated activated carbon is beaten with alcohol water, the palladium precursor solution is added, and Alkali is added to control the pH of the system to be 6-12, and then reduced by a reducing agent to obtain a palladium-carbon catalyst. Compared with the existing method, the method of the invention not only has high catalyst activity, but also has stable catalyst performance, can greatly increase the times of biotin synthesis in production and application, and reduce production cost.

Description

technical field [0001] The invention belongs to the technical field of biotin synthesis, and in particular relates to a method for catalytically synthesizing biotin with a highly mechanically active palladium-carbon catalyst. Background technique [0002] Biotin, also known as vitamin H and coenzyme R, belongs to the vitamin B family and is a water-soluble vitamin. It is a necessary substance for the synthesis of vitamin C and an indispensable substance for the normal metabolism of fat and protein. It is a necessary nutrient for maintaining the natural growth, development and normal human body function and health of the human body. It is mainly used in nutritional supplements, medicine and hygiene, and food. Enhancer, labeling of proteins, antigens, nucleic acids, etc. [0003] At present, most of the biotin synthesis patent documents (such as US2489232, US2489235, DE2058248, CN103833769A, etc.) reported are chemical synthesis methods, which are less related to the use of n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D495/04B01J23/44B01J35/02B01J35/00
CPCC07D495/04B01J23/44B01J35/40Y02P20/584
Inventor 颜攀敦陈丹张洁兰曾利辉曾永康
Owner XIAN CATALYST NEW MATERIALS CO LTD
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