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Process for recovering 7-ACA (aminocephalosporanic acid) crystallization mother liquor

A technology of 7-ACA, crystallization mother liquor, applied in the direction of organic chemistry, etc., can solve the problems of rising cost, increasing processing cost, environmental pollution and so on

Inactive Publication Date: 2015-04-29
SUNRESIN NEW METERIALS CO LTD XIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Taking the production situation of a certain company as an example: 200t of 7-ACA crystallization mother liquor is produced every day, with an average potency of 1200ug / ml. These waste waters are finally discharged to environmental protection and produce a large amount of COD. At the same time, 7-ACA with greater economic value in the waste water ACA is directly discarded into the sewer, and a total of about 240 kg / day of 7-ACA is discarded, which not only causes environmental pollution, increases treatment costs, but also causes a large amount of 7-ACA loss, resulting in increased costs
[0005] At present, there are no relevant reports on the recovery of 7-ACA mother liquor in domestic and foreign literature and materials

Method used

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  • Process for recovering 7-ACA (aminocephalosporanic acid) crystallization mother liquor
  • Process for recovering 7-ACA (aminocephalosporanic acid) crystallization mother liquor
  • Process for recovering 7-ACA (aminocephalosporanic acid) crystallization mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Resin adsorption: adjust the pH of the 7-ACA crystallization mother liquor to 4.0 with 10% hydrochloric acid (7-ACA potency in the mother liquor is 1243ug / ml, purity 64.2%), and pass through 100ml LXT at a flow rate of 1BV / h from top to bottom -032 resin bed (produced by Xi'an Lanxiao Technology New Materials Co., Ltd.), when the titer of the effluent at the bottom of the resin column is 12ug / ml, stop feeding the crystallization mother liquor into the resin column.

[0037] 2. Resin desorption: 2BV of 0.3% sodium bicarbonate desorbs the resin from top to bottom at a flow rate of 1BV / h, and collects the desorption liquid.

[0038] 3. Concentration: The desorption solution is concentrated to a titer of 32000ug / ml through an organic nanofiltration membrane with a molecular weight of 500.

[0039] 4. Crystallization drying can be carried out in accordance with the current production process, and will not be described here. Finally, 0.58 g of the 7-ACA product was obtain...

Embodiment 2

[0041] 1. Resin adsorption: adjust the pH of the 7-ACA crystallization mother liquor to 2.0 with 2% sulfuric acid (the potency of 7-ACA in the mother liquor is 1452ug / ml, and the purity is 59.5%), and pass through 100ml at a uniform speed from top to bottom at a flow rate of 2BV / h LXT-030 resin bed (produced by Xi'an Lanxiao Technology New Materials Co., Ltd.), when the titer of the effluent at the bottom of the resin column is 12ug / ml, stop feeding the crystallization mother liquor into the resin column.

[0042] 2. Resin desorption: 1.5BV of 0.4% sodium acetate desorbs the resin from top to bottom at a flow rate of 1BV / h, and collects the desorption solution.

[0043] 3. Concentration: The desorption solution is concentrated to a titer of 31050ug / ml through an organic reverse osmosis membrane with a molecular weight of 200.

[0044] 4. Crystallization drying can be carried out in accordance with the current production process, and will not be described here. Finally, 1.34 g...

Embodiment 3- Embodiment 7

[0046] The specific embodiment is the same as that in Example 1, mainly investigating the influence of different mother liquor pHs on the adsorption capacity of the resin, desorbing and concentrating the resin, and not taking the crystallization process as an investigation factor.

[0047] The titer of 7-ACA in the mother liquor is 1376ug / ml, and the purity of 7-ACA is 60.55%. Feed volume 25BV, feed flow rate 1BV / h, prepare 5 parts of LXT-030 resin, each 100ml resin. The crystallization mother liquor was adjusted to pH 2, 3, 4, 5 with 5% hydrochloric acid, and the adsorption control test was done with the natural pH conditions.

[0048] Resin adsorption capacity = (feed 7-ACA titer - effluent 7-ACA titer) * feed volume / resin volume

[0049] Example

[0050] Example 5

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Abstract

The invention provides a process for recovering a 7-ACA (aminocephalosporanic acid) product from mother liquor through macroporous adsorption resin. The process mainly comprises the following steps: performing resin adsorption, performing resin desorption, concentrating and the like, wherein in the resin absorption step, the pH value of 7-ACA crystallization mother liquor is adjusted, the crystallization mother liquor passes through a macroporous adsorption resin layer from top to bottom at a certain flow speed, and when the valence of 7-ACA contained in effluent of a resin column is 1% of that of the crystallization mother liquor at an inlet, resin adsorption is stopped. According to the method, the qualified 7-ACA product with the purity of greater than or equal to 98% and the color grade of greater than 4 can be obtained; the extraction yield of the resin is greater than or equal to 90% and the total process yield is greater than or equal to 40%; based on estimation of 200t of the mother liquor produced each day, the economic benefit of a year can reach more than ten million yuan.

Description

Technical field: [0001] The invention belongs to the field of chemical pharmacy, and in particular relates to a process for recovering 7-ACA crystallization mother liquor. Background technique: [0002] 7-Aminocephalosporanic acid (abbreviated as 7-ACA) is a key intermediate of semi-synthetic cephalosporin antibiotics and occupies a very important position in the pharmaceutical industry. The contradiction between the increase in production capacity of domestic 7-ACA enterprises and the country's restrictions on the use of antibiotics, the oversupply and the continued downturn in product prices have increased the enormous pressure on various manufacturers. Although each manufacturer adopts the one-step enzymatic cleavage process in the production process, the product yield increases by about 2-4% compared with the two-step enzymatic method, which can further reduce production costs and strive for no loss or a small amount of surplus, but enterprises The competitive pressure ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/18C07D501/12
CPCC07D501/12C07D501/18
Inventor 寇晓康王刚韦卫军刘琼刘文静
Owner SUNRESIN NEW METERIALS CO LTD XIAN
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