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Method for producing diosgenin by combining microwave and hot pressing decomposition technology

A technology of diosgenin and decomposition technology, which is applied in the production of bulk chemicals, steroids, organic chemistry, etc., can solve the problems of difficult organic solvent, low extraction rate of saponin, and long time for thermal decomposition, so as to reduce the shielding effect. , changing the chemical balance, resolving time-consuming effects

Active Publication Date: 2019-08-27
广东丰绿源生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At home and abroad, various improvements have been made around increasing the yield of saponin, reducing production costs, and reducing pollution emissions. Some have carried out pre-fermentation or enzymatic hydrolysis before hydrolysis, and some have used microwave extraction and ultrasonic extraction in the extraction stage, but the main The production technology route has not changed fundamentally, and saponin is still extracted by first hydrolyzing and then extracting, the amount of waste water has not been significantly reduced, cellulose and starch cannot be comprehensively utilized, and the environmental protection problem cannot be fundamentally solved; The cellulose and starch in the plant are separated, and then hydrolyzed and extracted. Although this method reduces the amount of acid and waste water, it does not completely solve the problem of pollution discharge, and the extraction rate of saponin is often not high; there are reports Some people use thermal decomposition method to extract saponin, because saponin exists in plants in the form of saponin and is wrapped by starch, so this method cannot completely convert saponin into saponin, even if it is converted into saponin, it is difficult to extract Because the starch is gelatinized at high temperature, it is difficult for the organic solvent to penetrate into the plant, the thermal decomposition takes a long time, the glycosidic bond cracking rate is not complete, and the saponin extraction rate is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Raw materials: 1000kg of 2-year-old fresh chrysanthemum-leaf yams produced in Yangxi County, Yangjiang City, Guangdong Province after cleaning and removing impurities

[0019] 1. Raw material crushing: add 2000kg of water, use a ball mill to fully grind, dissociate the fiber, starch, and saponin complex monomers, pass through an 80-mesh sieve, wash with water to separate the fibers, and let the filtrate stand for 4 hours to settle, remove the upper layer The supernatant and the lower layer precipitated starch, take the saponin complex suspension in the middle layer, and set aside;

[0020] 2. Centrifugation: centrifuge the above-mentioned saponin complex suspension at a centrifugal speed of 5000r / min to obtain about 95kg of saponin complex solids;

[0021] 3. Microwave radiation and pressure decomposition: place the above-mentioned saponin composite solid in a closed microwave device for microwave radiation, control the microwave radiation power at 300W, control the tem...

Embodiment 2

[0027] Raw materials: 1000kg of 2-year-old fresh chrysanthemum-leaf yams produced in Yangxi County, Yangjiang City, Guangdong Province after cleaning and removing impurities

[0028]1. Raw material crushing: Add 2000kg of water, use a ball mill to fully grind, dissociate the fiber, starch, and saponin complex monomers, pass through an 80-mesh sieve, and wash with water to separate the fibers. The filtrate is left to settle for 6 hours, and the upper layer is removed. The supernatant and the lower layer precipitated starch, take the saponin complex suspension in the middle layer, and set aside;

[0029] 2. Centrifugation: centrifuge the above-mentioned saponin complex suspension at a centrifugal speed of 5000r / min to obtain about 97kg of saponin complex solids;

[0030] 3. Microwave radiation and pressure decomposition: put the above-mentioned saponin composite solid in a closed microwave device for microwave radiation, control the microwave radiation power at 600W, control the...

Embodiment 3

[0036] Raw materials: 1000kg of 2-year-old fresh chrysanthemum-leaf yams produced in Yangxi County, Yangjiang City, Guangdong Province after cleaning and removing impurities

[0037] 1. Raw material crushing: add 2000kg of water, use a ball mill to fully grind, dissociate the fiber, starch, and saponin complex monomers, pass through an 80-mesh sieve, wash with water to separate the fibers, and let the filtrate stand for 8 hours to settle, remove the upper layer The supernatant and the lower layer precipitated starch, take the saponin complex suspension in the middle layer, and set aside;

[0038] 2. Centrifugation: centrifuge the above-mentioned saponin complex suspension at a centrifugal speed of 5000r / min to obtain about 99kg of saponin complex solids;

[0039] 3. Microwave radiation and pressure decomposition: place the above-mentioned saponin composite solid in a closed microwave device for microwave radiation, control the microwave radiation power at 900W, control the tem...

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Abstract

The invention discloses a method for producing diosgenin through combined use of microwaves and hot pressing decomposition technology. A microwave radiation pressurized decomposition method is used; asaponin compound separated from dioscorea plant raw materials is put into a sealed microwave device for microwave radiation; the microwave power radiation power is controlled at 300 to 900 W; the temperature in the reaction system is controlled to be 100 to 200 DEG C; the pressure is 1 to 10 MPa; the pressure maintaining time is 5 to 30min; then, the pressure relief is performed; the dioscin is subjected to glycosyl removal under the microwave radiation and pressurized heating conditions and is converted into diosgenin. The method has the advantages that the glucosidic bonds of the dioscin can be effectively cracked in a short time; the diosgenin extraction rate is improved; the production cost is reduced. In the production process, acid hydrolysis is not needed; a great amount of acid waste water generated by acid hydrolysis can be avoided; starch and cellulose obtained through separation can be comprehensive utilized; the method is a diosgenin clean production process suitable for industrial mass production.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a production method of diosgenin. Background technique [0002] Diosgenin (commonly known as saponin), diosgenin is an ideal precursor for the synthesis of various steroid hormones and steroidal contraceptives, more than 60% of the steroid hormones produced in the world use it as a raw material. At present, there are many manufacturers in my country producing steroid hormone drugs and steroid oral contraceptives, which are an important field next to antibiotics in drug production. my country has used the self-produced diosgenin ligands to synthesize more than 200 kinds of drugs. In addition to hormones for anti-inflammation and contraception, it also uses steroid starting materials to synthesize analgesics, anesthetics, and coronary heart disease drugs. [0003] Diosgenin, that is, diosgenin, is insoluble in water but soluble in organic solvents such as methanol and petroleu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
CPCC07J71/0005Y02P20/54
Inventor 陈顺钦赵长伟
Owner 广东丰绿源生物医药科技有限公司