Preparation method of palladium-carbon catalyst for synthesizing meropenem

A technology of palladium-carbon catalyst and meropenem, which is applied in the field of preparation of palladium-carbon catalyst, can solve the problems of difficult yield of target product, high and low catalyst performance, etc., and achieves the effect of ensuring speed, high selectivity and low palladium content

Active Publication Date: 2014-07-02
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, the yield of the existing system is generally about 49%. Because of the adsorption effect of palladium carbon itself, selectivity, and the dissolution of mixed solvents, it is very difficult to increase the yield of the target product; The price is 20,000 / Kg, every increase of 1 percentage point can increase the net profit by 200 yuan, the performance of the catalyst is directly related to the production cost and competitiveness of the product

Method used

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  • Preparation method of palladium-carbon catalyst for synthesizing meropenem
  • Preparation method of palladium-carbon catalyst for synthesizing meropenem

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The palladium-carbon catalyst used in the synthesis of meropenem in this example includes an activated carbon carrier, and palladium dispersed on the activated carbon carrier as amorphous nanoparticles, and the loading amount of the palladium is 4% of the mass of the palladium-carbon catalyst;

[0029] The preparation method of the palladium carbon catalyst of the present embodiment is as follows:

[0030] Step 1. The particle size is 200-300 mesh and the specific surface area is 800m 2 / g~1000m 2 / g of wood charcoal placed in a boiling mass concentration of 2% Na 2 CO 3 Refluxing in the aqueous solution for 3 hours, then washing the refluxed wood charcoal with pure water until the pH of the washing solution is 7, drying to obtain an activated carbon carrier;

[0031] Step 2, dissolving palladium chloride containing palladium 0.8g in dilute hydrochloric acid with a mass concentration of 10%, then diluting with water to obtain an active component solution, adjusting t...

Embodiment 2

[0042] The palladium-carbon catalyst used in the synthesis of meropenem in this example includes an activated carbon carrier, and palladium dispersed on the activated carbon carrier as amorphous nanoparticles, and the loading amount of the palladium is 3.5% of the mass of the palladium-carbon catalyst;

[0043] The preparation method of the palladium carbon catalyst of the present embodiment is as follows:

[0044] Step 1. The particle size is 200-300 mesh and the specific surface area is 1000m 2 / g~1200m 2 / g of wood charcoal placed in boiling mass concentration is 5% KHCO 3 Refluxing in the aqueous solution for 1 hour, then washing the refluxed wood charcoal with pure water until the pH of the washing solution is 8, drying to obtain an activated carbon carrier;

[0045] Step 2, dissolving palladium chloride containing palladium 0.7g in dilute hydrochloric acid with a mass concentration of 5%, then diluting with water to obtain an active component solution, adjusting the pH...

Embodiment 3

[0050] The palladium-carbon catalyst used in the synthesis of meropenem in this embodiment includes an activated carbon carrier, and palladium dispersed on the activated carbon carrier as amorphous nanoparticles, and the loading amount of the palladium is 4.5% of the mass of the palladium-carbon catalyst;

[0051] The preparation method of the palladium carbon catalyst of the present embodiment is as follows:

[0052] Step 1. The particle size is 200-300 mesh, and the specific surface area is 1500m 2 / g~1700m 2 / g of wood charcoal placed in boiling solute mass concentration of 10% Na 2 CO 3 and K 2 CO 3 Reflux treatment in the mixed aqueous solution for 2h, Na in the mixed aqueous solution 2 CO 3 and K 2 CO 3 The mass ratio is 1:3, then the wood charcoal after the reflux treatment is washed with pure water to a pH value of 7.5 of the washing liquid, and dried to obtain an activated carbon carrier;

[0053] Step 2, dissolving the palladium chloride containing palladium...

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Abstract

The invention discloses a preparation method of a palladium-carbon catalyst for synthesizing meropenem. The preparation method comprises the following steps: (1) putting wood charcoal into a boiling alkali compound water solution, carrying out backflow treatment, washing by virtue of pure water, and drying to obtain an active carbon carrier; (2) preparing an active ingredient solution, and regulating the pH value of the active ingredient solution; (3) pulping the active carbon carrier, and stabilizing the active carbon carrier at a stirring condition, so as to obtain active carbon slurry; (4) adding the active ingredient solution into the active carbon slurry after the pH value of the active ingredient solution is regulated, and stirring to obtain a catalyst precursor; and (5) aging the catalyst precursor, and reducing the catalyst precursor by virtue of a reducing agent, so as to obtain a catalyst finished product. According the preparation method, a low-content alkali compound is utilized for processing the carrier so as to obtain a proper carrier with a reasonable surface chemical structure, so that the consumption of a reagent is reduced; chelated palladium ions of a certain size are prepared by regulating the pH value of the active component solution, so that purposes of controlling the activity and selectivity of the catalyst are realized; the preparation method has no special control point, is simple in process and is beneficial to the industrial large scale production.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a preparation method of a palladium-carbon catalyst used for the synthesis of meropenem. Background technique [0002] Carbapenem antibiotics mainly include meropenem, imipenem, panipenem, biapenem, ertapenem, faropenem, doripenem, etc. Among them, meropenem has the largest market demand and the most widely used widely. In the last step of its chemical synthesis, it is necessary to use palladium carbon catalyst for hydrogenolysis reaction, as shown in the following reaction formula, while removing the protecting groups PNB (p-nitrobenzyl) and PNZ (p-nitrobenzyloxycarbonyl) ), the palladium-carbon specification used to produce this product on the market is generally 5% to 7% palladium-carbon, and the catalyst charging amount is generally about 20% of the substrate quality, and the product yield is about 48%. The amount of palladium carbon catalyst used i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44
Inventor 李岳锋曾永康曾利辉田勤奋
Owner XIAN CATALYST NEW MATERIALS CO LTD
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