Preparation method and application of catalyst for hydrogenation of steroid compounds

A technology of catalysts and compounds, which is applied in the field of preparation of precious metal catalysts, can solve the problems of poor catalyst activity and stability, catalysts can only be used once, and complex catalyst preparation process, etc., to achieve good catalytic activity and selectivity, mild conditions, and convenient recycling Effect

Active Publication Date: 2013-11-13
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation process of this catalyst is complicated, and nitrogen protection is required in this process, which has certain limitations on the large-scale industrialization of this catalyst.
[0005] Chinese patent CN102603841A has reported another preparation method for the preparation of steroid drug intermediates, wherein NaBH 4 or KBH 4 It is a reducing agent, but there are many experimental steps and complicated process, the yield of the final target product is only about 80%, and the catalyst can only be used once, which is easy to decompose
[0006] In addition, Chinese patents such as CN101177443A, CN101362789A,

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  • Preparation method and application of catalyst for hydrogenation of steroid compounds

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[0029] Example 1

[0030] Step 1: Add 10g of activated carbon to HNO with a concentration of 12mol / L 3 Soak in the solution for 2 hours, then wash the soaked activated carbon with deionized water to neutrality and filter to obtain pretreated activated carbon; the particle size of the activated carbon is 200-300 mesh, and the specific surface area of ​​the activated carbon is 1000m 2 / g;

[0031] Step 2: Dissolve palladium chloride with a palladium content of 0.5 g and cobalt chloride with a cobalt content of 0.1 g in water, and stir uniformly to obtain a precursor solution;

[0032] Step 3. Weigh 9.4 g of the pretreated activated carbon carrier described in step one and add it to the precursor solution described in step two, immerse it for 5 hours under agitation, then adjust the pH value of the impregnation system to 10, continue stirring for 3 hours and then filter , Get the filter cake, and then wash the filter cake with water to neutral;

[0033] Step 4. The filter cake washed to ...

Example Embodiment

[0034] Example 2

[0035] This embodiment is the same as embodiment 1, except that: the auxiliary agent is platinum, ruthenium, rhodium, or nickel, or at least two of platinum, ruthenium, rhodium, cobalt, and nickel.

Example Embodiment

[0036] Example 3

[0037] Step 1: Add 10g of activated carbon to HNO with a concentration of 15mol / L 3 Soak in the solution for 1 hour, and then wash the soaked activated carbon with deionized water to neutrality and filter to obtain pretreated activated carbon; the particle size of the activated carbon is 300 mesh to 400 mesh, and the specific surface area of ​​the activated carbon is 1500 m 2 / g;

[0038] Step 2: Dissolve palladium nitrate with a palladium content of 0.2g, palladium chloride with a palladium content of 0.1g, and ruthenium chloride with a ruthenium content of 0.05g in water, and stir uniformly to obtain a precursor solution;

[0039] Step 3. Weigh 9.65g of the pretreated activated carbon carrier described in step one and add it to the precursor solution described in step two, immerse for 6 hours under stirring conditions, then adjust the pH value of the dipping system to 9, continue stirring for 1 hour and then filter , Get the filter cake, and then wash the filter ...

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Abstract

The invention discloses a preparation method of a catalyst for hydrogenation of steroid compounds. The method comprises the following steps: 1, pretreating active carbon; 2, dissolving a dissoluble palladium compound and dissoluble salt of an auxiliary agent into water and stirring uniformly to obtain a precursor solution; 3, adding a pretreated active carbon carrier into the precursor solution, dipping, adjusting the pH value of a dipping system, continuously stirring for 1 to 5 hours, filtering and washing a filter cake; and 4, pulping the filter cake which is washed to be neutral with pure water to obtain pulp, adjusting the pH value of the pulp, adding a reducing agent to reduce the pulp, filtering, washing and drying to obtain the catalyst for hydrogenation of the steroid compounds. In addition, the invention also discloses a method for catalyzing hydrogenation of the steroid compounds by using the catalyst. The catalyst prepared by the method is applicable to catalytic hydrogenation of the steroid compounds; the yield of products exceeds 95 percent; the mass percentage content of isomers in the products is less than 5 percent; and the catalyst has stable performance and good repeatability.

Description

technical field [0001] The invention belongs to the technical field of preparation of noble metal catalysts, and in particular relates to a preparation method and application of a catalyst for hydrogenation of steroid compounds. Background technique [0002] Steroids are the second largest class of drugs after antibiotics. After decades of research and development, steroidal drugs have formed a large class of drugs with a wide variety of clinical applications, mainly for the treatment of rheumatism, cardiovascular, collagenous diseases, lymphatic leukemia, tumors, bacterial encephalitis , skin diseases, endocrine disorders, senile diseases, etc. From the perspective of the development of the international steroid drug industry, sales in 2006 have reached 40 billion US dollars, accounting for about 10% of the world's sales of pharmaceutical products. my country's annual output value exceeds 18 billion yuan, accounting for 7% of the total output value of the pharmaceutical i...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/46B01J23/89C07J75/00C07J1/00
Inventor 李小虎张之翔李岳锋曾利辉谭志勇
Owner XIAN CATALYST NEW MATERIALS CO LTD
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