Process for recovering androstenedione from androstenedione fermentation waste liquid

A technology of androstenedione and fermentation waste liquid, which is applied in the direction of steroids and organic chemistry, can solve the problems that fermentation waste liquid is easy to pollute the environment and occupy the space of factories and enterprises, and achieve efficient recovery and waste recycling. Effect

Pending Publication Date: 2022-05-10
NANYANG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fermentation waste liquid containing 4-androstenedione, 4-androstenedione structural analog impurities, complex organic solvents and oils is easy to pollute the environment, and also occupies a lot of space in factories and enterprises. How to deal with this waste has become a constraint for enterprises A developmental problem that needs to be resolved urgently

Method used

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  • Process for recovering androstenedione from androstenedione fermentation waste liquid
  • Process for recovering androstenedione from androstenedione fermentation waste liquid
  • Process for recovering androstenedione from androstenedione fermentation waste liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0035] The processing method of androstenedione fermentation waste liquid, the steps are as follows:

[0036] 1) Add lye with pH 12 to the androstenedione fermentation waste liquid according to the material-to-liquid ratio of 1:2, and at 40-50°C, sonicate for 5 minutes, wash 5-7 times, then add water to wash 3-5 times, wash Until the solution is basically transparent;

[0037] 2) Add 6-10 times methanol to the washed sample, ultrasonicate for 5 min at 40-50°C, dissolve thoroughly, and centrifuge at 4000-6000rpm to remove the precipitate;

[0038] 3) Adjust the concentration of methanol in the supernatant to 78-80%, and centrifuge to remove the black oil;

[0039] 4) Add 5% of the sample weight to the supernatant with activated carbon for decolorization for 1 hour, filter, and rotate to evaporate to 20% water, freeze for 1 hour, pour off the water phase, and continue to concentrate to anhydrous;

[0040] 5) Add 1-1.5 times of ethyl acetate to dissolve, then add 0.5-0.7 times ...

Embodiment 2

[0043] 1) Take 200 grams of androstenedione fermentation waste liquid, add 400 mL of lye solution with pH 12 to the androstenedione fermentation waste liquid, and wash it 7 times by ultrasonication for 5 min at 40~50 °C, and then wash with water for 400 °C Wash 4 times with mL until the solution is basically transparent;

[0044] 2) Add about 120-150 grams of the washed sample into 720 mL of methanol, sonicate for 5 minutes at 40-50 ℃, dissolve thoroughly, and centrifuge at 6000 rpm to remove the precipitate;

[0045] 3) Add about 700 mL of supernatant to 175 mL of water to adjust the concentration of methanol to 80%, and centrifuge to remove the black oil;

[0046] 4) Add 5 g of activated carbon to the supernatant to decolorize the sample weight (100 g), shake on a shaker at 50 ° C for 1 hour, filter, and rotate to evaporate to 20% water content, freeze for 1 hour, pour off the water phase, and continue to concentrate to nothing. water, about 60 grams;

[0047] 5) Add 90 mL o...

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Abstract

The invention discloses a process for recovering androstenedione from androstenedione fermentation waste liquid, which comprises the following steps: adding an alkaline cleaning agent, a cleaning emulsifier, water-soluble impurities, water-soluble pigments and part of grease into the androstenedione fermentation waste liquid according to a material-to-liquid ratio of 1: 2, then washing to obtain a precipitate, adding 6 times by weight of absolute methanol into the precipitate part, and ultrasonically dissolving for 5 minutes, centrifuging to remove precipitate impurities, centrifuging supernate to adjust the methanol concentration to be 75-80%, centrifuging to remove lower black oily substances, concentrating methanol extract, adding ethyl acetate and petroleum ether according to the ratio of 1: 0.5 to crystallize, and recrystallizing crystals with methanol for four times to obtain high-purity 4-AD. According to the method, the defects of saponification, membrane treatment and resin purification are overcome, the androstenedione can be efficiently recovered from the androstenedione fermentation waste, the effect of recycling the waste is achieved, and additional economic benefits are created for enterprises.

Description

technical field [0001] The invention belongs to the technical field of androstenedione fermentation production, in particular to a process for recovering androstenedione from androstenedione fermentation waste liquid. Background technique [0002] Androst-4-ene-3,17-dione (referred to as androstenedione, androst-4-ene-3,17-dione or 4AD) is also known as androsterone and androsterone, which is the raw material drug for the production of hormones Almost all steroid hormone drugs can be produced with AD as the starting material, such as for the production of more than 100 kinds of drugs such as corticosteroids, sex hormones, progestins and anabolic hormones. Qualified androstenedione is obtained through microbial transformation, oil-water separation, methanol extraction, decolorization, concentration, crystallization, and recrystallization. The waste liquid after microbial fermentation to produce androstenedione is dark brown or black, oily and viscous. The waste liquid conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 王莹宋晓中李嘉欣孙唯玉金永福薛刚
Owner NANYANG INST OF TECH
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