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Androstenedione purification method

A purification method and the technology of androstenedione, which are applied in the field of chemical engineering, can solve problems such as low yield, large solvent consumption, and complicated operation, and achieve the effects of high yield, improved product quality, and easy operation

Inactive Publication Date: 2013-08-21
ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to purify the product, repeated crystallization with a solvent is required. Not only is the operation complicated, the solvent consumption is large, and the yield is low, but also the effect of removing impurities is not very ideal, and the purity can only reach about 95%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Put 800 kg of crude crystals (AD content 85%) into the crystal washing pot, add 2 t of n-hexane and ethyl acetate as a 1:1 composite solvent, stir and wash the crystals for 2 hours, and centrifuge to obtain 745 kg of crystal powder (dried); add 1.49 t n-Hexane and ethyl acetate as a 1:1 composite solvent, stirring and washing for 2 hours again, centrifuged to obtain 699.5 kg of crystal powder (dried), the AD content was 94.5%, and the crystal washing yield was 97.20%. Drying and recrystallization with methanol yielded 602.7 kg of crystal powder with an AD purity of 99.11% and a drying loss of 0.1%.

Embodiment 2

[0016] Put 800kg of crude crystals (AD content 85%) into the crystal washing pot, add 1.8t of n-hexane and ethyl acetate 1:1 composite solvent, stir and wash the crystals for 2 hours, and centrifuge to obtain 761.1kg of crystal powder (dried); add 1.3t n-hexane and ethyl acetate 1:1 composite solvent, stirred and washed crystals again for 2 hours, and centrifuged to obtain 715.5kg (dried) crystal powder, AD content was 92.3%, and crystal washing yield was 97.12%. Drying and recrystallization with methanol yielded 589.3 kg of crystal powder with an AD purity of 98.4% and a drying loss of 0.1%.

Embodiment 3

[0018] Put 800kg of crude crystals (AD content 85%) into the crystal washing pot, add 2.2 t of n-hexane and ethyl acetate 1:1 composite solvent, stir and wash the crystals for 2 hours, and centrifuge to obtain 741.0 kg of crystal powder (dried), add 1.3t of n-hexane and ethyl acetate 1:1 composite solvent, stirred again for 2 hours to wash the crystals, and centrifuged to obtain 695.1kg of crystal powder (dried), the AD content was 94.4%, and the crystal washing yield was 96.5%. Drying and recrystallization with methanol yielded 592.6 kg of crystal powder with an AD purity of 99.1% and a drying loss of 0.1%.

[0019] Through the comparison of 3 examples, it is found that the low amount of composite solvent used in example 2 will lead to incomplete removal of impurities, and the product purity will not meet the standard. The proportion of composite solvent used in embodiment 3 is large, and part of the crystal powder is washed away, and the yield of the resulting crystal powder...

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PUM

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Abstract

The invention relates to an androstenedione purification method comprising the steps of crystal washing and recrystallizaiton, wherein a composite solvent composed of normal hexane and ethyl acetate in the proportion of 1:1 is adopted in the step of crystal washing, and methyl alcohol is used as a solvent in the step of recrystallization. The androstenedione purification method comprises the concrete steps of: (1) primary crystal washing: adding a macrocrystalline and a composite solvent according to the proportion of 1:2.5, stirring the macrocrystalline and the composite solvent for 2h, and then, carrying out centrifugal separation to obtain crystal powder A; (2) secondary crystal washing: adding the crystal powder A and the composite solvent according to the proportion of 1:2, stirring the crystal powder A and the composite solvent for 2h, and then, carrying out centrifugal separation to obtain crystal powder B; (3) recrystallization: drying the crystal powder B, and then recrystallizing by using the methyl alcohol to obtain a finished product with the purity of over 99%, wherein the dosage ratio of the methyl alcohol to the crystal powder B is 1:16; and (4) solvent recovery: inspissating the washing solutions obtained in the primary and secondary crystal washing processes through a membrane lifting concentrator to recover the composite solvent. By using the androstenedione purification method, impurities can be effectively removed, the operation can be simplified, a great number of solvents can be saved, the energy consumption during solvent recovery is also reduced, and finally, the finished product with the purity of over 99% is obtained.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, in particular to a method for purifying androstenedione. Background technique [0002] Androstenedione (androst-4-ene-3,17-dione or "AD") is an irreplaceable intermediate of steroid hormone drugs, which plays a very important role in regulating the body and is widely used in rheumatoid Sexual arthritis, contraceptive diuresis and control of various infectious inflammations. In the past, the production of androstenedione in our country was mainly obtained by extracting diosgenin from wild Chinese medicinal materials such as "Chuandilong" and other plants through chemical synthesis. The process is very complicated, the consumption cost is high, and it pollutes the environment. At present, the preparation of androstenedione is to convert phytosterols into androstenedione through microbial fermentation, and the androstenedione fermentation broth is dehydrated, methanol ultrasonic extrac...

Claims

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Application Information

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IPC IPC(8): C07J1/00
Inventor 肖国林冯佩杰祝金山王银泉傅业件
Owner ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD
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