CN1325510C - Method for producing dioscin by directly extracting saponin without pollution - Google Patents

Method for producing dioscin by directly extracting saponin without pollution Download PDF

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Publication number
CN1325510C
CN1325510C CNB2004100607773A CN200410060777A CN1325510C CN 1325510 C CN1325510 C CN 1325510C CN B2004100607773 A CNB2004100607773 A CN B2004100607773A CN 200410060777 A CN200410060777 A CN 200410060777A CN 1325510 C CN1325510 C CN 1325510C
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saponin
finished product
extraction
concentrate
slurry
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CN1616480A (en
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王元华
郭敏霞
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王元华
郭敏霞
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Abstract

The present invention provides a method for producing diosgenin by directly extracting saponin without pollution, which comprises the following technology steps: 1, raw material pretreatment: a dioscorea is cleaned by clear water and is pulverized by a pulverizer; after being pulverized, the dioscorea is ground into dioscorea pulp by a grinding mill; thus, the granule of the dioscorea pulp reaches 40 to 150 meshes, and the concentration reaches 5 to 12%; 2, saponin pulp extraction: by using a multi-stage cyclone group, the saponin with low specific gravity is separated from fiber and starch to obtain saponin pulp; 3, dewatering concentration: filter dehydration is carried out by a filtering machine or manpower, and about 70 to 80 % of water is removed to obtained concentrated saponin pulp; 4, finished product treatment by the concentrated saponin pulp: by using a conventional technological method, a finished product is obtained after at least the following steps, such as acid hydrolysis, extraction, concentration and crystallization. The technological steps of the present invention are simple, the defect of a large amount of waste water generated by sieving fiber is overcome, the production cost is reduced, and the diosgenin can be produced basically without pollution under the condition of no increase of environmental protection facilities. Simultaneously, the yield and the quality of the product are increased, the resource degree is improved, and the diosgenin can be produced on a scale.

Description

Pollution-free direct extraction saponin is produced the method for diosgenin
Technical field
The invention belongs to vegetable chemistry engineering field, relate in particular to the method that a kind of pollution-free direct extraction saponin is produced diosgenin.
Background technology
Diosgenin is the basic raw material of multiple steroid drugss such as synthetic anti-inflammatory hormone, progestogen, sexual hormoue.Glucocorticosteroid particularly has anti-inflammatory, antianaphylaxis, antishock, antitoxin and anticancer effect, is the indispensable main medicine of pharmaceutically widespread use.
At present, the diosgenin that China produces accounts for world's total amount 50%, mainly is to propose from Rhizome of Peltate Yam.The Rhizome of Peltate Yam vegetable fibre accounts for 35-40%, starch accounts for 45-50%, water-soluble substances accounts for 10%, saponin content only accounts for 1-2.5%, and be difficult to separation and Extraction, common process is at high temperature with Rhizome of Peltate Yam, high pressure, be hydrolyzed under the high acid environment, one ton of saponin of every production needs 150 tons of cadmium yellow ginger, 20 tons of consumption hydrochloric acid, produce high-concentration waste water more than 500 tons, its COD is up to 30000mg/L (BOD8000mg/L), pH value 1.0-2.5, thereby traditional technology production cost height, labour intensity is big, and quality product is difficult to control, and especially environmental pollution is serious, it is huge to handle waste water consumption matter, has influenced the development of China's Chinese yam industry.The kinds of processes reform this occurred, concluded to get up to be divided into hydrolysis pre-treatment and hydrolyzation post-processing technique.Hydrolyzation post-processing technique need be handled a large amount of waste water, is generally acknowledged unpromising.The hydrolysis pre-treating technology that has now occurred is: after isolating fiber and starch at first respectively, carry out acid hydrolysis again; But the proterties behind the yellow ginger defibrination, need the saponin in the most fiber of a large amount of washings during decision screening fiber, need water doubly with 20-30, though water can be recycled, but being difficult to dehydration concentrates, not only strengthen the isolating treatment capacity of starch, and the therefrom isolated saponins slurry that contains the 1-2% solids in a large number also is difficult to dehydration and concentrates, production cost and labour intensity are big.In addition, also having a kind of technology is to sieve fiber earlier, and the ultrafiltration and concentration starch slurry is used the alcohol extraction saponin more then; In this technology, because not separation of starch, thereby the ultrafiltration difficulty, extraction cost height is difficult to promote.
Summary of the invention
To produce a large amount of waste water in order solving in the existing method of utilizing Chinese yam to produce saponin, to be difficult to the shortcoming concentrated, that production cost is high of dewatering, utilize resources synthetically, reduce production costs when production environment is innoxious, the present invention proposes the method that pollution-free direct extraction saponin is produced diosgenin.
Theoretical foundation of the present invention is: starch, saponin are present in the parenchyma cell, and by fiber, xylogen embedding, when yellow ginger is ground to certain fineness, cell walls destroys, xylogen, fiber, starch, saponin dissociate out, saponin proportion minimum wherein, the available physical method is at first separated saponin.
For this reason, technical scheme of the present invention is as follows: pollution-free direct extraction saponin is produced the method for diosgenin, is realized by following processing step:
(1), raw materials pretreatment: clean Chinese yam with clear water, use crusher in crushing, pulping is ground with grinding machine in broken back, makes the particle of Chinese yam slurry reach the 40-150 order, and concentration is 5-12%;
(2), extract saponins slurry: with multistage swirler group, the saponin that proportion is lighter separates with fiber, starch, obtains saponins slurry;
(3), dehydration concentrates: with filter or artificial filter dehydration, remove the water of about 70%-80%, must concentrate saponins slurry;
(4), concentrate the processing of saponins slurry to finished product: processing method routinely obtains finished product through acid hydrolysis, extraction, concentrated, crystallization at least.
Beneficial effect: processing step of the present invention is simple, has avoided the step of screening fiber, has saved a large amount of water; In the process of extracting saponins slurry, utilize directly that proportion is the lighter saponin of swirler group from the Chinese yam slurry, to extract, utilize the characteristic of swirler to obtain the saponins slurry of suitable concn, enter then and concentrate and, the fiber of from the swirler group, separating and the starch mixed pulp can make alcohol or drying is made feed to the step of finished product.Compare with existing method, processing step is more simple and clear, produces the drawback of a large amount of waste water when having avoided the screening fiber, has reduced the discharging of waste water, and saponins slurry is concentrated easily, has shortened the process time, reduces production costs, and has improved product yield and quality; Produce 100 tons of saponin traditional technology year, produce 50,000 tons of waste water, and waste water reduces to 10% only 5000 tons among the present invention, and the recycling alcohol of doing, basic environmentally safe.
Description of drawings
Fig. 1 is technological process of production figure of the present invention.
Embodiment
According to process flow sheet shown in Figure 1, it is as follows to describe the present invention in detail:
(1), raw materials pretreatment: comprising cleaning, pulverize defibrination, specifically is to clean Chinese yam with clear water, uses crusher in crushing, and pulping is ground with grinding machine in broken back, makes the particle of Chinese yam slurry reach the 40-150 order, and concentration is 5-12%; Grinding machine adopts double plate mill or taper thread grinding;
(2), extract saponins slurry: adopting cyclonic separation, specifically is that the saponin that proportion is lighter separates with fiber, starch, obtains saponins slurry with multistage swirler group, and fiber and starch mixed pulp are utilized and made alcohol or feed;
(3), dehydration concentrates: with filter or artificial filter dehydration, remove the water of about 70%-80%, must concentrate saponins slurry;
(4), concentrated saponins slurry is divided into 3 kinds of approach again to the processing of finished product as shown in Figure 1, following description respectively:
The 1st kind of approach: will concentrate saponins slurry and directly carry out acid hydrolysis, then through extraction, concentrate, crystallization obtains finished product.
The 2nd kind of approach: will concentrate saponins slurry under 25-45 ℃ condition, spontaneous fermentation is about 48 hours; Then through acid hydrolysis, extraction, concentrate, crystallization obtains finished product.
The 3rd kind of approach: will concentrate saponins slurry with the organic solvent methyl alcohol of 75-90%, ethanol, propyl alcohol, amylalcohol or wherein any extraction 15-25 minute, and filter then, and use above-mentioned solvent extraction more once, last fractionation by distillation goes out saponin, and the recovery solvent; Then through acid hydrolysis, extraction, concentrate, crystallization obtains finished product.
3 kinds of approach in (4) step in the above-mentioned processing step have different effects respectively: the 1st kind of approach has the most succinct characteristics, but it is more to produce waste water during acid hydrolysis.Acid hydrolysis again after the 2nd kind of approach adopts and ferment, less with acid, waste water is still more.Acid hydrolysis again behind the 3rd kind of approach employing organic solvent extraction not only reduces during acid hydrolysis with acid amount and waste water, and has reduced subsequent step and extracted the cost of saponin, good product quality.
Processing step of the present invention is physics, chemical reaction process, and technology is short and sweet, is not increasing under the environmental protection facility condition, reaches free of contamination substantially production diosgenin, and suitable for mass production is easy to promote.
Characteristics of the present invention are: avoided the step of screening fiber, directly adopted cyclonic separation that saponin and fiber, starch are separated, saved a large amount of water, avoided the generation of a large amount of waste water, dehydration concentrates easily, and the labour intensity in the production process is little, and production cost is low.

Claims (3)

1, the method for CR production diosgenin is characterized in that being realized by following processing step:
(1), raw materials pretreatment: clean Chinese yam with clear water, use crusher in crushing, pulping is ground with grinding machine in broken back, makes the particle of Chinese yam slurry reach the 40-150 order, and concentration is 5-12%;
(2), extract saponins slurry: with multistage swirler group, the saponin that proportion is lighter separates with fiber, starch, obtains saponins slurry;
(3), dehydration concentrates: with filter or artificial filter dehydration, remove the water of about 70%-80%, must concentrate saponins slurry;
(4), concentrate the processing of saponins slurry to finished product: processing method routinely obtains finished product through acid hydrolysis, extraction, concentrated, crystallization at least.
2, the method for CR production diosgenin according to claim 1, it is characterized in that concentrating in the described step (4) processing of saponins slurry to finished product, specifically: will concentrate saponins slurry with the organic solvent methyl alcohol of 75-90%, ethanol, propyl alcohol, amylalcohol or wherein any extraction 15-25 minute, filter then, use above-mentioned solvent extraction more once, distill sub-argument at last and go out saponin, and reclaim solvent; Then through acid hydrolysis, extraction, concentrate, crystallization obtains finished product.
3, the method for CR production diosgenin according to claim 1 is characterized in that concentrating the processing of saponins slurry to finished product in the described step (4), and specifically: will concentrate saponins slurry under 25-45 ℃ condition, spontaneous fermentation is about 48 hours; Then through acid hydrolysis, extraction, concentrate, crystallization obtains finished product.
CNB2004100607773A 2004-08-28 2004-08-28 Method for producing dioscin by directly extracting saponin without pollution Expired - Fee Related CN1325510C (en)

Priority Applications (1)

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CN1325510C true CN1325510C (en) 2007-07-11

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101294189B (en) * 2008-06-11 2011-11-02 王元华 Preprocessing method for saponins slurry in dioscorea opposita saponin production process
CN102020693B (en) * 2009-09-18 2014-04-23 张万举 Clean production method of yam saponin
CN101885750B (en) * 2010-03-08 2012-08-22 李绍通 Method for circularly processing and utilizing rhizome in dioscorea

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
旋流分离技术强化甘蔗糖浆除杂的研究 邓立高等,广西轻工业,第2期 2001 *
薯蓣皂甙分离工艺的研究及其综合利用 周振起等,西北植物学报,第15卷第3期 1995 *
薯蓣皂甙分离工艺的研究及其综合利用 周振起等,西北植物学报,第15卷第3期 1995;旋流分离技术强化甘蔗糖浆除杂的研究 邓立高等,广西轻工业,第2期 2001 *

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Assignee: Hubei Danjiangkou Danao Pharmaceutical Chemical Co.,Ltd.

Assignor: Wang Yuanhua|Guo Minxia

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Denomination of invention: Method for producing dioscin by directly extracting saponin without pollution

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