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Preparation method of rhodium-carbon catalyst for synthesis of minocycline hydrochloride

A technology of minocycline hydrochloride and catalyst, which is applied in the field of preparation of rhodium carbon catalyst for the synthesis of minocycline hydrochloride, can solve the problems of poor repeatability, no involvement of rhodium carbon technology, low efficiency of rhodium metal colloid, etc., and achieve reduction of catalyst Activity, the preparation method is simple and easy to control, and the effect of ensuring the activity of the catalyst

Pending Publication Date: 2020-02-28
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN 103055854 B relates to a rhodium carbon catalyst for hydroformylation of olefins. The invention adopts a colloid method to prepare rhodium colloids, load them on activated carbon, and reduce them again to obtain rhodium carbon catalysts. The application of olefin hydroformylation reaction has mild reaction conditions, It has the characteristics of high catalytic activity, good selectivity, long service life and high product purity, but the preparation of rhodium metal colloid in this catalyst process has the defects of low efficiency and poor repeatability
[0006] Wang Chunxing's master's thesis "Study on the Synthesis Process of Minocycline Hydrochloride" (2017, Zhejiang University) investigated in detail the performance comparison of different rhodium carbons from domestic and foreign catalyst manufacturers, but did not involve the specific development and research of rhodium carbon technology
[0007] In summary, the existing published patents and literature have not done any special research on the rhodium carbon catalyst dedicated to the dehydroxylation step in the synthesis of minocycline hydrochloride, only the description of the use effect

Method used

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  • Preparation method of rhodium-carbon catalyst for synthesis of minocycline hydrochloride
  • Preparation method of rhodium-carbon catalyst for synthesis of minocycline hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The rhodium carbon catalyst for the synthesis of minocycline hydrochloride of the present embodiment comprises a carrier and rhodium nanoparticles dispersed on the carrier, the carrier is powdered activated carbon treated with an aqueous solution of sodium hydroxide under microwave conditions, and the amount of rhodium in the catalyst is The mass percentage content is 5%.

[0033] The preparation method of the rhodium carbon catalyst of the present embodiment may further comprise the steps:

[0034] Step 1. The particle size is 200-400 mesh, and the specific surface area is about 900m 2 / g of wood charcoal, under microwave heating conditions, reflux treatment with 5% sodium hydroxide aqueous solution for 3h with a mass concentration, then wash with pure water until pH is 7.5, and dry to obtain pretreated activated carbon; the microwave-heated charcoal The temperature is 80°C;

[0035] Step 2, dissolving 1.0 g of rhodium-containing rhodium trichloride hydrate with pure...

Embodiment 2

[0042] The rhodium carbon catalyst for the synthesis of minocycline hydrochloride of the present embodiment comprises a carrier and rhodium nanoparticles dispersed on the carrier, the carrier is powdered activated carbon treated with an aqueous solution of sodium hydroxide under microwave conditions, and the amount of rhodium in the catalyst is The mass percentage content is 5%.

[0043] The preparation method of the rhodium carbon catalyst of the present embodiment may further comprise the steps:

[0044] Step 1. The particle size is 200-400 mesh, and the specific surface area is about 800m 2 / g of wood charcoal, under microwave heating conditions, reflux treatment of 3% sodium hydroxide aqueous solution with mass concentration for 2h, then wash with pure water until pH is 7.0, and dry to obtain pretreated activated carbon; The temperature is 90°C;

[0045] Step 2, dissolving 1.0 g of rhodium-containing rhodium trichloride hydrate with pure water at 100° C. to obtain soluti...

Embodiment 3

[0052] The rhodium carbon catalyst for the synthesis of minocycline hydrochloride of the present embodiment comprises a carrier and rhodium nanoparticles dispersed on the carrier, the carrier is powdered activated carbon treated with an aqueous solution of sodium hydroxide under microwave conditions, and the amount of rhodium in the catalyst is The mass percentage content is 5%.

[0053] The preparation method of the rhodium carbon catalyst of the present embodiment may further comprise the steps:

[0054] Step 1. The particle size is 200-400 mesh, and the specific surface area is about 1000m 2 / g wood charcoal, under microwave heating conditions, reflux treatment with 10% sodium hydroxide aqueous solution with mass concentration for 4h, then wash with pure water until pH is 8.0, and dry to obtain pretreated activated carbon; The temperature is 100°C;

[0055] Step 2. Dissolve 1.0 g of rhodium-containing rhodium trichloride hydrate with pure water at 80° C. to obtain solutio...

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Abstract

The invention discloses a preparation method of a rhodium-carbon catalyst for synthesis of minocycline hydrochloride. The rhodium-carbon catalyst comprises a carrier and rhodium nanoparticles dispersed on the carrier, the carrier is powdered activated carbon treated with a sodium hydroxide aqueous solution under microwave conditions, and the mass percentage of rhodium in the rhodium-carbon catalyst is 5%. The rhodium-carbon catalyst is prepared by adopting one-pot method, the activity of the rhodium-carbon catalyst is improved by introducing a chelating agent, the activity of the rhodium-carbon catalyst is properly reduced by microwave heating, and the selectivity of the rhodium-carbon catalyst is improved with ensured activity of the rhodium-carbon catalyst. The prepared rhodium-carbon catalyst is applied to a dehydroxylation step in minocycline hydrochloride synthesis, is high in selectivity, can effectively reduce the generation of side reaction dehydration impurities and improve the yield of target product sancycline hydrochloride, and is of great significance on reduction of production cost of minocycline hydrochloride and the improvement of the product quality.

Description

technical field [0001] The invention belongs to the technical field of preparation of noble metal catalysts, in particular to a preparation method of rhodium carbon catalyst for minocycline hydrochloride synthesis. Background technique [0002] Minocycline hydrochloride (MINO, Minocycline Hydrochloride), also known as: minocycline hydrochloride, minocycline, a new generation of tetracycline antibiotics was first developed and marketed by the American Lederle company, chemical name: 4S-(4a,4aa, 5aa,12aa)-4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11 -Dioxo-2-tetracenecarboxamide hydrochloride. The antibacterial activity of the drug against Gram-positive bacteria is 2-4 times stronger than that of the first-generation tetracycline. One of the most effective varieties of antibiotics. [0003] Compared with other tetracycline antibiotics, minocycline hydrochloride has many advantages, but its synthesis process is more complicated, and fac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46C07C231/12C07C237/26
CPCB01J23/464C07C231/12C07C2603/46C07B2200/07C07C237/26
Inventor 李岳锋张之翔曾永康万克柔曾利辉王昭文张鹏陈丹闫江梅
Owner XIAN CATALYST NEW MATERIALS CO LTD
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