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Preparation method for efficiently synthesizing palladium-carbon catalyst for biotins

A palladium-carbon catalyst and synthetic biology technology, which is applied in the preparation of sugar derivatives, physical/chemical process catalysts, chemical instruments and methods, etc., can solve problems such as limited effects, achieve convenient maintenance, mild reaction conditions, and good heat preservation effect Effect

Inactive Publication Date: 2018-10-09
徐学军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the active sites in the micropores of activated carbon play a very limited role in the reaction process, so it is necessary to improve the preparation method of the palladium carbon catalyst, and the palladium nanoparticles enter the micropores as little as possible. Catalytic hydrogenation reduction of biotin intermediate I to generate biotin intermediate II under loading conditions

Method used

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  • Preparation method for efficiently synthesizing palladium-carbon catalyst for biotins

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preparation example Construction

[0020] A kind of preparation method of palladium-carbon catalyst for efficiently synthesizing biotin of the present invention comprises the following steps:

[0021] e) Add water into the flask, put the palladium precursor into the water, stir and dissolve, add organic acid to continue stirring and dissolve, after heating up, use alkali solution to adjust the pH value of the solution system;

[0022] f) dropping activated carbon into the solution of step a for impregnation;

[0023] g) After the impregnation is completed, add a reducing agent to the solution in step b for rapid reduction;

[0024] h) After filtering and washing the solution in step c, the palladium carbon catalyst is obtained.

[0025] Specifically, the palladium precursor described in step a is one or more mixtures of palladium dichloride, sodium chloropalladate, potassium chloropalladate, palladium nitrate, ammonium chloropalladate and chloropalladic acid, step a The organic acid described in is a mixture ...

Embodiment 1

[0032] In the 500ml flask, add 150 grams of water, take by weighing 0.45 grams of palladium equivalent chloropalladium acid solution and drop into it, then add the lactic acid aqueous solution of 6.856 grams of lactic acid equivalent, and the magnetic stirrer 14 stirs the solution under the drive of the magnetic drive motor 141, Stir to combine well. The water circulation heater 43 heats the water in the water bath 4 under the drive of the water circulation heating motor 44 to increase the temperature of the solution to 40-45°C. Use 10% sodium hydroxide solution to adjust the pH to between 6.0 and 7.0. Then add 14.55 g of activated carbon and keep warm for 8 hours. Stable temperature at 40-45°C, quickly add 0.02 molar equivalent sodium hypophosphite aqueous solution. Continue to keep warm for 4 hours. Filter and wash to obtain 15 grams of 3% palladium carbon catalyst.

[0033] In a 1000ml autoclave, add 100 grams of biotin intermediate I, 200 grams of methanol, add 5 grams...

Embodiment 2

[0035] In a 500ml flask, add 150 grams of water, weigh 0.75 grams of palladium equivalent palladium nitrate solution into it, then add 0.057 molar equivalents of citric acid aqueous solution, stir and mix evenly. Raise the temperature to 25-30°C. Use 10% sodium carbonate solution to adjust the pH to between 5.5 and 6.0. Then add 14.25 g of activated carbon and keep warm for 8 hours. Stabilize the temperature at 25-30°C, and quickly add 0.035 molar equivalent of sodium hypophosphite aqueous solution. Continue for 4 hours. 15 g of 5% palladium carbon catalyst were obtained by filtering and washing.

[0036] In a 1000ml autoclave, add 100 grams of biotin intermediate I, 200 grams of methanol, add 2.5 grams of the 5% palladium carbon catalyst prepared above, replace nitrogen three times, replace hydrogen three times, pressurize to 2.5 MPa, and heat up to 60 ° C. Leave on for 2 hours. The conversion rate of biotin intermediate I detected by liquid phase was 99.5%.

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Abstract

The invention discloses a preparation method for efficiently synthesizing a palladium-carbon catalyst for biotins. The preparation method comprises the following steps: adding water into a flask, adding a palladium precursor into water, stirring and dissolving, adding an organic acid to continuously stir and dissolve, raising the temperature, and regulating the pH value of the solution system withaqueous alkali; adding activated carbon into the solution for impregnating; and adding a reducing agent into the solution for rapid reduction after impregnation completion, filtering and washing, thereby obtaining the palladium-carbon catalyst. According to the preparation method disclosed by the invention, the palladium salt and the organic acid are coordinated to form a stable macromolecular complex in the aqueous solution, and the activated carbon is added into the solution for impregnation. The complex strength of the organic acid and palladium and distribution thereof in the activated carbon pore channel can be controlled by controlling the pH value of the aqueous solution and a molar ratio of the organic acid to the palladium, and then rapid reduction is performed, so that the palladium is precipitated in medium and large pores of the activated carbon and the surface in a nano state as small as possible. The palladium-carbon catalyst has excellent catalytic performance while catalyzing biotin intermediate hydrogenation.

Description

【Technical field】 [0001] The invention relates to the technical field of biotin catalyst preparation, in particular to the technical field of a preparation method of a palladium-carbon catalyst for efficiently synthesizing biotin. 【Background technique】 [0002] Biotin, also known as vitamin H or coenzyme R, belongs to the B vitamins. Biotin is an important coenzyme in the intermediate metabolism of sugar, protein and fat, and is widely used in the pharmaceutical and feed industries. Reduction of (3aS,6aR)hexahydro-2-oxo-1,3-dibenzylthieno[3,4-d]imidazolyl-4-ylidenepentanoic acid (I) involved in biotin synthesis (3aS,6aR) Hexahydro-2-oxo-1,3-dibenzylthieno[3,4-d]imidazolyl-4-ylpentanoic acid (II). [0003] At present, this step reduction method has palladium acetate or dichlorobis(benzonitrile) palladium used in patent US5498721 and US5859260, using a homogeneous catalyst, and the reaction conditions are relatively mild, but the recovery process of palladium is loaded down...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07D495/04C07H1/00C07H17/00
CPCB01J23/44C07D495/04C07H1/00C07H17/00
Inventor 竺亚庆郑飞跃李思全
Owner 徐学军
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