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Method for recovering progesterone from progesterone production mother liquor

A technology of progesterone and mother liquor, applied in the direction of steroids, organic chemistry, etc., can solve environmental hazards and other problems, achieve the effects of reducing pollution, reducing emissions, and improving economic benefits

Active Publication Date: 2014-03-19
陕西汉江药业集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides a method for recovering progesterone from progesterone production mother liquor to solve the problem that the mother liquor contains a large amount of steroid hormone compounds and is very harmful to the environment

Method used

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  • Method for recovering progesterone from progesterone production mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1] Mother liquor pretreatment:

[0034] 1.1] 200kg of the progesterone production mother liquor is pumped into the reaction tank and distilled. The end temperature of the distillation is 90°C, and 150kg of solvent is evaporated, so the residue weight M1 is 50kg; The crude product mother liquor produced in the oxidation production process;

[0035] 1.2] Add 50kg of toluene to the residue and raise the temperature to 70-80°C to completely dissolve the residue. Toluene can be replaced by one or more of benzene, chloroform, and methylene chloride;

[0036] 2) Remove some impurities: add 50kg of dilute hydrochloric acid solution with a concentration of 5% by mass, stir for 30 minutes, let it stand for 30 minutes, separate the layers, separate the acid layer, and repeat the pickling operation once; wash the toluene layer with 50kg of water, Repeat the operation 2 times until the pH>6. The dilute hydrochloric acid solution can be replaced with one or more of dilute sulfuric...

Embodiment 2

[0050] 1] Mother liquor pretreatment

[0051]1.1] 500kg of the progesterone production mother liquor is pumped into the reaction tank and distilled. The end temperature of the distillation is 95°C, and 378kg of solvent is evaporated; the residue weight is 122kg; Refined mother liquor produced in the oxidation production process;

[0052] 1.2] Add 250kg of toluene to the residue and raise the temperature to 70-80°C to completely dissolve the residue. Toluene can be replaced by one or more mixtures of benzene, chloroform, and methylene chloride.

[0053] 2) Remove some impurities: add 250kg of dilute sulfuric acid solution with a concentration of 5% by mass, stir for 30 minutes, let stand for 30 minutes, separate the layers, and separate the acid layer; repeat the pickling operation once; wash the toluene layer with 250kg of water 3 times, to PH>6. The dilute sulfuric acid solution can be replaced with one or more of dilute hydrochloric acid, dilute acetic acid and dilute for...

Embodiment 3

[0067] 1] Mother liquor pretreatment

[0068] 1.1] 1950kg of the progesterone production mother liquor is pumped into the reaction tank and distilled. The end temperature of the distillation is 100°C, and 1602kg of solvent is evaporated; then the residue weight M1 is 348kg; The mother liquor produced in the oxidation production process is a mixture of crude mother liquor and refined mother liquor;

[0069] 1.2] Add 1392kg of toluene to the residue and raise the temperature to 70-80°C to completely dissolve the residue. Toluene can be replaced by one or more mixtures of benzene, chloroform, and methylene chloride.

[0070] 2] Remove some impurities: add 1392 kg of dilute hydrochloric acid solution with a concentration of 10% by mass, stir for 30 minutes, let stand for 30 minutes, separate the layers, and separate the acid layer; repeat the pickling operation once; wash the toluene layer 2 with 700 kg of water times, to PH>6. The dilute hydrochloric acid solution can be repla...

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Abstract

The invention relates to a method for recovering progesterone from a progesterone production mother liquor. The progesterone production mother liquor can be a crude product mother liquor generated in a process for producing progesterone by oxidizing pregnenolone and a refined mother liquor. The method comprises the following steps: steaming out a solvent in the mother liquor, dissolving mother liquor residues obtained after distillation in a new solvent, washing with a dilute acid, washing with water to neutrality, carrying out refluxing water diversion, detecting the weight of each of main components comprising progesterone and pregnenolone after the water diversion, oxidizing pregnenolone by cyclohexanone and aluminum isopropoxide, adding an acid to neutralize, washing with water, steaming out the new solvent, adding a crystallization solvent for crystallizing to obtain crude progesterone, and refining the crude progesterone to obtain progesterone. The method changing the progesterone mother liquor to valuables has the following advantages: progesterone in the mother liquor is recovered, so the total yield of progesterone is improved by about 4.0%, thereby the economic benefit of progesterone is improved; and the emission of dangerous wastes (containing hormone compounds) is reduced, so the pollution to the environment is reduced.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, and in particular relates to a method for recovering progesterone from progesterone production mother liquor. Background technique [0002] Progesterone, also known as progesterone, is a progestin hormone. In vivo has a marked morphological effect on the estrogen-stimulated endometrium, which is necessary for the maintenance of pregnancy. Progesterone is clinically used in the reactive diagnosis of threatened abortion, habitual abortion, amenorrhea or the cause of amenorrhea, etc. Progesterone is not only an important steroid hormone drug, but also a pharmaceutical intermediate, and the market demand is very strong. And its production of mother liquor is also increasing. Taking the process of producing progesterone by pregnenolone method as an example, the characteristics of progesterone mother liquor are: [0003] (1) It is large in size and contains a large amount of solvent. [0004] (2) C...

Claims

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Application Information

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IPC IPC(8): C07J7/00
Inventor 张佳燕国武陈峙张全冰唐耀光
Owner 陕西汉江药业集团股份有限公司
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