Method for recycling DCPC (deacetyl cephalosporin C) from cephalosporin C resin adsorption waste liquor

A technology of resin adsorption and spore bacteria, applied in the field of chemical pharmaceuticals, can solve the problems of polluted environment, poor product quality, low adsorption capacity, etc.

Active Publication Date: 2015-06-03
SUNRESIN NEW METERIALS CO LTD XIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the adsorption raffinate of various manufacturers does not recycle the DCPC in it, and directly discharges it into the wastewater system, which not only pollutes the environment, but also causes a great waste of resources.
[0004] The disclosed method of USP3926729 is to use macroporous strong base anion exchange resin etc. to adsorb DCPC. The decolorization effect of pigment impurities is relatively poor
Yu Haijun (the separation and purification of deacetylcephalosporin C, "Journal of Chemical Industry", 2010, 61) mentioned that the coal-based granular activated carbon with a particle size distribution of 0.27-1.70mm is used as an adsorbent to carry out the adsorption separation of DCPC. This method has the following defects : (1) The use of granular activated carbon has a low adsorption capacity (only 11g/L), and organic solvents are required for desorption and regeneration, causing secondary pollution to the environment and high extraction costs; (2) Using anion exchange resin to directly adsorb DC Then desorb on the resin, which increases the co

Method used

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  • Method for recycling DCPC (deacetyl cephalosporin C) from cephalosporin C resin adsorption waste liquor
  • Method for recycling DCPC (deacetyl cephalosporin C) from cephalosporin C resin adsorption waste liquor
  • Method for recycling DCPC (deacetyl cephalosporin C) from cephalosporin C resin adsorption waste liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1) Ion exchange resin desalination: the cephalosporin C resin adsorption raffinate (pH2.8, DC content 423ug / ml) is passed through 100ml of LXT-200 resin (gel-type strong base) from top to bottom at a flow rate of 2BV / h Anion exchange resin, produced by Xi’an Lanxiao Technology New Materials Co., Ltd.), the effluent was detected with 1% (w / w) barium chloride solution, and when a small amount of white precipitate was produced, the resin adsorption was stopped, and the effluent was collected as desalination liquid.

[0048] 2) Resin adsorption and desorption: pass the obtained desalination solution (pH3.1, DC content 410ug / ml) through 100ml LXT-081 (styrene-divinylbenzene macroporous adsorption) at a flow rate of 1BV / h from top to bottom Resin, produced by Xi'an Lanxiao Science and Technology New Material Co., Ltd.), the DCPC titer in the resin column effluent was detected by liquid chromatography, and the resin adsorption was stopped when the effluent titer was 4ug / ml. T...

Embodiment 2- Embodiment 6

[0052] In order to further illustrate the embodiment, each process factor of the present invention is examined separately.

[0053] Adjust the pH of the cephalosporin C resin adsorption raffinate to 2.5, 2.8, 3.2, 3.5, 4.0 respectively, and pass through 5 parts of 100ml LXT-203 resin (macroporous weak base anion exchange Resin, produced by Xi'an Lanxiao Technology New Material Co., Ltd.), the effluent is detected with 1% barium chloride solution, and if white precipitation occurs, it shows that there is sulfate radical leakage, and the adsorption is stopped. Investigate the processing capacity of the resin under different pH conditions (after the anion exchange resin fails, the pH will gradually decrease).

[0054] Example

Embodiment 7- Embodiment 11

[0056] Ion exchange resins perform desalting at different flow rates:

[0057] Example

[0058] Adjust the pH of the cephalosporin C resin adsorption raffinate to 2.73, and the DC content to 531ug / ml, and pass through 5 each Part 100ml of LXT-207 resin (gel strong base anion exchange resin, produced by Xi'an Lanxiao Technology New Materials Co., Ltd.), the effluent is detected with 1% (w / w) barium chloride solution. If white precipitation occurs, then It shows that there is leakage of sulfate radical, stop the adsorption. Investigate the processing capacity of the resin under different pH conditions (after the anion exchange resin fails, the pH will gradually decrease)

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Abstract

The invention provides a method for recycling DCPC from cephalosporin C resin adsorption waste liquor. According to the method, an anion exchange resin 1 is firstly used for removing residual inorganic anions, particularly sulfate ions, in the adsorption raffinate; and the remaining feed liquid is adsorbed by a macroporous adsorption resin, a salt solution is used as desorption agent, the elutriant is directly concentrated by nanofiltration after being decolored through an anion exchange resin 2, further, after the processes of splitting decomposition, crystallization, drying, and so on, a D-7ACA qualified product with purity of not less than 98% and color grade of more than 4 is obtained. Resin extraction yield is not less than 85%, and total yield of the process is not less than 45%.

Description

Technical field: [0001] The invention belongs to the field of chemical pharmacy, and in particular relates to a method for recovering DCPC from cephalosporin C resin adsorption waste liquid by adopting resin. Background technique: [0002] Cephalosporin C is the raw material for the semi-synthesis of cephalosporin antibiotic intermediate 7-aminocephalosporanic acid (abbreviated 7-ACA). At present, the production of cephalosporin C is generally carried out by solid-liquid separation after three-stage or four-stage fermentation of Cephalosporin acremonium to obtain a clarified supernatant, and then undergo two to three-step resin treatment to remove cephalosporin C analogues and pigments and other impurities, the resulting solution is directly subjected to enzymatic cleavage to produce 7-ACA. [0003] After the cephalosporin C fermentation liquid is obtained through solid-liquid separation to clarify the supernatant, the cephalosporin C (hereinafter referred to as CPC) in the...

Claims

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Application Information

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IPC IPC(8): C12P35/06C07D501/28C07D501/12
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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