Method for removing cobalt from reactant and extracting reactant

A compound and mixture technology, applied in the field of extracting triacetyl compounds, can solve the problems of loss of active ingredients, low cobalt enrichment, and affecting production cycle, etc., and achieve the effects of reducing resin loss, shortening production process, and high resin efficiency

Active Publication Date: 2012-05-02
WUXI JIYU SHANHE PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The resin is saturated after 3-4 batches, and must be treated with acid and alkali, and the treatment produces a large amount of waste water, which brings great pressure to sewage treatment
Moreover, during the treatment process, the residual adsorbed active ingredients in the resin are also lost due to acid-base treatment, resulting in a large loss of yield.
Therefore, not only the enrichment degree of cobalt in the original process is not high (in the acid-base treatment solution and cobalt removal waste residue), but also the yield is low and the loss of resin due to frequent treatment is large, which affects the production cycle

Method used

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  • Method for removing cobalt from reactant and extracting reactant
  • Method for removing cobalt from reactant and extracting reactant

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Get 40kg of diammonium hydrogen phosphate and dissolve it in 400kg of water. Stir, the synthesis solution containing triacetyl compound in the production process of etimicin sulfate is 25l / min (500L reaction solution is exhausted in 20 minutes) with flow rate, slowly sucks in the diammonium hydrogen phosphate solution. Continue to stir and draw in 12L of ammonium sulfide solution (reagent grade), and stir for 10 minutes after the pumping is complete. Then pump in 6kg of powdered activated carbon, stir and heat to 50°C to 60°C, and keep warm for 15 minutes. Press it into a flat plate filter to obtain a light yellow filtrate, and use an ammonium sulfide test solution to detect that there is no residual cobalt ion.

[0039] Extract according to extraction method 1: pass the filtrate with complete decobalt removal into the separation column equipped with ammonium type 001×7 strong acidic cation exchange resin for adsorption, after the adsorption is completed within 6 hours...

Embodiment 2

[0041] Get diammonium hydrogen phosphate 36kg and dissolve in 360kg water. Stir, the synthesis solution containing triacetyl compound in the production process of etimicin sulfate is 16l / min (500L reaction solution is exhausted in 30 minutes) with flow rate, slowly sucks in the diammonium hydrogen phosphate solution. Continue to stir and draw in 10L of ammonium sulfide solution (reagent grade), and stir for 10 minutes after the pumping is complete. Then pump in 6kg of powdered activated carbon, stir and heat to 50°C to 60°C, and keep warm for 15 minutes. Press it into a flat plate filter to obtain a light yellow filtrate, and use an ammonium sulfide test solution to detect that there is no residual cobalt ion.

[0042] Extract according to extraction method 1: pass the filtrate with complete decobalt removal into the separation column equipped with ammonium type 001×7 strong acidic cation exchange resin for adsorption, after the adsorption is completed within 6 hours, rinse w...

Embodiment 3

[0044] Get diammonium hydrogen phosphate 36kg and dissolve in 360kg water. Stir, the synthesis solution containing triacetyl compound in the production process of etimicin sulfate is 16l / min (500L reaction solution is exhausted in 30 minutes) with flow rate, slowly sucks in the diammonium hydrogen phosphate solution. Continue to stir and draw in 10L of ammonium sulfide solution (reagent grade), and stir for 10 minutes after the pumping is complete. Then pump in 6kg of powdered activated carbon, stir and heat to 50°C to 60°C, and keep warm for 15 minutes. Press it into a flat plate filter to obtain a light yellow filtrate, and use an ammonium sulfide test solution to detect that there is no residual cobalt ion.

[0045]Extract according to extraction method 2: Add 120-150L of concentrated ammonia water to the filtrate that has completely decobalted, pass it into a separation column equipped with D1300 macroporous adsorption resin, and absorb it. After the adsorption is complet...

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Abstract

The invention relates to a method for removing cobalt from a reactant and extracting the reactant. The method comprises the following steps: adding a phosphate solution into synthetic reaction liquid; stirring and depositing complex cobalt in the reaction liquid, and then adding in a sulfide solution; after completely depositing, utilizing active carbon to heat, stirring and decolorizing, thereby obtaining a cobalt ion-free light yellow solution; and utilizing an ammonium type cation exchange resin or macro-porous adsorption resin to adsorb and elute, and concentrating an eluent, thereby obtaining a triacetyl compound.

Description

technical field [0001] The invention relates to a new method for removing complexed cobalt and extracting the triacetyl compound from the synthesis solution containing the triacetyl compound in the production process of the semi-synthetic aminoglycoside antibiotic etimicin sulfate. Background technique [0002] At present, the intermediate product of the first step in the production of semi-synthetic aminoglycoside antibiotic etimicin sulfate is a triacetyl compound, 3,2',6'-tri(N-acetyl)gentamycin C 1a (hereinafter referred to as P1), its structure is: [0003] [0004] The reaction scheme of this reaction is: [0005] [0006] At present, most of the patents and literature reports are the technology of removing complexed cobalt from the synthesis reaction solution by resin adsorption or crystallization; Ammonia water elution and concentration, the residual cobalt ions in it are passed into hydrogen sulfide to remove, then adsorbed by macroporous resin, and then con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/236C07H1/06
Inventor 郭永忠
Owner WUXI JIYU SHANHE PHARM CO LTD
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