CN100516084C - Vaporizing-acid acid splitting method for extracting dioscorea saponin element - Google Patents
Vaporizing-acid acid splitting method for extracting dioscorea saponin element Download PDFInfo
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- CN100516084C CN100516084C CNB2005100189404A CN200510018940A CN100516084C CN 100516084 C CN100516084 C CN 100516084C CN B2005100189404 A CNB2005100189404 A CN B2005100189404A CN 200510018940 A CN200510018940 A CN 200510018940A CN 100516084 C CN100516084 C CN 100516084C
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Abstract
This invention is a method of acidolysis by vaporization acid to distilling diosgenin, its characteristic is: Keep yam of granular or powdery in touch to the steam of the acid liquid, carry on the acidolysis to the plant with the hot acid gas, filtrate, neutralization, drying, extraction, then get the powdery diosgenin products. Under the condition not less than general hydrolysis, acid solution and neutralization water can be used repeatedly, acidolysis product needn't be water-wash, therefore does not have waste water need to be arranged basically.
Description
Technical field
The present invention relates to the extraction and the environment protection of diosgenin.
Technical background
Diosgenin also claims diosgenin, be called for short saponin, belong to the derivative of different spiral steroid alkene alkane, be the hydrolysate of dioscin (dioscin) in the Dioscoreaceae yam rhizome, its form with glucoside extensively is present in the natural plant, and is wherein maximum with Dioscoreaceae content especially.The plant that contains diosgenin mainly contains yellow ginger, Dioscorea nipponica Mak. Ningpo Yam Rhizome, cucurbit fragrant plant etc.
Diosgenin has estrogen effect, but reducing cholesterol, cough-relieving, eliminates the phlegm, desensitizes, recovers pathological tissues and stimulate heparinocyte and choleresis.It can be used as the semi-synthetic raw material of steroidal anti-inflammatory medicine, sexual hormoue, female contraceptive agent.China's Chinese yam aboundresources; It is main in the world diosgenin producing country.But the domestic technology that adopts is the conventional acid hydrolysis method mostly at present, and all there are a lot of problems in processes such as hydrolysis, extraction.So the researchist is devoted to new processing method is improved or sought to the production technique of conventional acid hydrolysis method for a long time always.
The raw material of producing saponin mainly contains yellow ginger, Dioscorea nipponica Mak. Ningpo Yam Rhizome, cucurbit fragrant plant etc., and its main component is starch, Mierocrystalline cellulose, glucosides and xylogen.Wherein yellow ginger is the topmost plant that produces saponin.This is that the production cycle is lacked (yellow ginger is 2 years, and Dioscorea nipponica Mak. Ningpo Yam Rhizome is 4-5) because of saponin content height (turmeric saponin content can reach 2.5%, and Dioscorea nipponica Mak. Ningpo Yam Rhizome content is 1.2%, and cucurbit fragrant plant seed content is 0.8%-1.2%) in the yellow ginger.
The steps in sequence of conventional acid hydrolysis method is: raw material, to pulverize, and 2.0mol/L hydrochloric acid or sulfuric acid solution 5～6 hours filter, neutralization, water washing, drying is pulverized, and No. 120 petrolic solvent extracts, concentrated extracting solution, product is filtered in crystallization.
The extraction yield of conventional acid hydrolysis method is low generally below 85%.
Produce in the process of saponin, trade effluent is startling to the pollution that environment causes.According to statistics, 1 ton of saponin of every production needs 130～180 tons of cadmium yellow ginger, 15～20 tons of 35% technical hydrochloric acids, and 1 ton in 10% sodium hydroxide, 6 tons in 120# gasoline, the waste water that is produced is up to 500～1000 tons.Produce 800 tons of calculating of saponin, about 40～800,000 tons of China's saponin waste water quantity discharged per year with China.Waste water mainly comes from acid hydrolysis, filters the spent acid sewage that the back produces in the production process, and neutralizes, washs the comprehensive wastewater that the back produces.
In the acidolysis generally according to yellow ginger: the ratio of 2.0mol/L hydrochloric acid=1: 3.5～5.0 batching, so, one ton of diosgenin of every production will discharge acid hydrolysis solution more than 350 tons and the washes more than at least 150 tons, and wherein the organic impurity content height can not recycle.Waste water is brownish black, when just discharging, sends brackish burnt burning, and is of long duration, becomes acid smell again, serious environment pollution, and factory is built to the there, just endangers a side, is called as " king of pollution ".Only just there is family surplus the big or small source mill 70 Shiyan City, Hubei, mainly concentrate on red trip waterborne, threaten divert water from the south to the north project center line watershed water quality, caused the great attention of various circles of society, being hundred Wan Jiangnong interests on the one hand, is the divert water from the south to the north project of investment 1,105 hundred million on the other hand.
Saponin waste water belongs to highly difficult indegradable industrial effluent, and intractability is bigger, and at present domestic do not have a tame saponin manufacturing enterprise can carry out thoroughly effectively administering as yet, and wherein except that minority was handled it, great majority directly discharged.
Most of yellow ginger processing enterprise is the private individual enterprise in rural area, lacks environmental consciousness; Less to the understanding of national environmental protection laws and regulations, do not carry out waste water treatment basically.The yellow ginger processing waste water has become the another important industrial pollution source in upstream, Han River.In some places, a river bank just has the yellow ginger source mill that five or six families produce saponin; As Hubei, except larger saponin manufacturing and processing enterprise has carried out the wastewater treatment, the Yunxi County has that family is the elementary source mill of little saponin and the private workshop of raw material with the yellow ginger surplus in the of 10, and these processing enterprises give off a large amount of black waste water every day, just enters rivers without administering basically.Near its water port 1 kilometer with in the interior waters, aquatic organism is close to disappearance, the polluted river people and animals can't drink.
From the document that retrieves, present research mainly contains two classes: the one, around improving of the improvement of diosgenin extraction yield, as aging process, enzyme pre-treatment yellow ginger method, partition method, with carbon dioxide abstraction etc. to existing acidolysis process; The 2nd, to the various treatment process researchs of diosgenin trade effluent.Improved method can make more than the extraction rate reached to 90%, and saponin waste water reduces to some extent.But processing step is many, cost is high, and still has a large amount of waste acid waters and washing water to discharge or to handle.
Summary of the invention
The object of the present invention is to provide a kind of vaporization acid acid hydrolyzation that extracts diosgenin, it is under the condition that is not less than conventional acid hydrolysis method extraction yield, acid solution in the leaching process and in and water reuse, the acidolysis thing can not wash with water, thereby does not have waste water to arrange basically.
Technical scheme of the present invention is: extract the vaporization acid acid hydrolyzation of diosgenin, it is characterized in that: the hot gas of acid solution is contacted with granular or powdered yam, with hot sour gas plant is carried out acidolysis, filter neutralization, drying, extract, get powdery diosgenin product.
The vaporization acid acid hydrolyzation of aforesaid extraction diosgenin, it is characterized in that: described yam is at least one of yellow ginger, Dioscorea nipponica Mak. Ningpo Yam Rhizome, cucurbit fragrant plant.
The vaporization of aforesaid extraction diosgenin acid acid hydrolyzation is characterized in that: when described yam is yellow ginger, when in the phlegma of the acidolysis gas of contacted plant during glassy yellow acidolysis can stop.
The vaporization acid acid hydrolyzation of aforesaid extraction diosgenin, it is characterized in that: described acid solution is a hydrochloric acid solution, the concentration when its acid gas condensation is liquid is 1.0mol/L～63mol/L.
The vaporization acid acid hydrolyzation of aforesaid extraction diosgenin, it is characterized in that: the concentration when acid gas condensation is liquid is preferably 1.8mol/L～3.5mol/L.
The vaporization acid acid hydrolyzation of aforesaid extraction diosgenin, it is characterized in that: the amount concentration of the fluent meterial of hydrochloric acid solution is 3.1mol/L～6.3mol/L.
The vaporization acid acid hydrolyzation of aforesaid extraction diosgenin, it is characterized in that: with the hot gas of acid solution with before granular or powdered yam contact, elder generation water or 2.0 ± 0.5mol/L acid solution mix granular or powdered yam wet, placed 10～24 hours, the sour gas of reusable heat carries out acidolysis to granular or powdered yam then.
The vaporization acid acid hydrolyzation of aforesaid extraction diosgenin, it is characterized in that: with the hot gas of acid solution with before granular or powdered yam contact, earlier carry out pre-treatment with aging process, enzyme method for pretreating, partition method, the sour gas of reusable heat carries out acidolysis to the material that contains diosgenin then.
The vaporization of aforesaid extraction diosgenin acid acid hydrolyzation is characterized in that: the hot/cold acid solution and the Zhong Heshui of yam are crossed in acidolysis, directly the next batch raw material is reused; Or hot acid liquid is cooled to normal temperature, its precipitate is rejected back revaporization use.
The vaporization acid acid hydrolyzation of aforesaid extraction diosgenin, it is characterized in that: the acid liquor temperature of yam uppermost surface is at 96～110 ℃.
Beneficial effect
Produce a large amount of waste water serious environment pollution problems at from yam (as yellow ginger, Dioscorea nipponica Mak. Ningpo Yam Rhizome, cucurbit fragrant plant), extracting diosgenin at present, the present invention is with vaporization acid solution acidolysis yam, acid hydrolysis solution can recycle, byproduct in the circulation acid hydrolysis solution constantly the enrichment back direct crystallization that reaches capacity separate out, overcome the defective that existing recovery byproduct need concentrate a large amount of mother liquors forfeiture economic benefits; The eccysis simultaneously of vaporization acid solution the byproduct in the yellow ginger, in and water can circulate repeatedly, the acidolysis thing needn't wash again, just can obtain fusing point and be the product more than 195 ℃; With existing common process relatively, extraction yield high by 0.3% (2.2～1.9%) is produced one ton of diosgenin and is discharged 336 tons of spent acid solutions, 136.9 tons of waste water less.
Concrete embodiment
Embodiments of the invention 1 (A technology)
Get yellow ginger (doing) 50g of powder essence, add 2.0mol/L hydrochloric acid 75mL (about ratio: yellow ginger: 2.0mol/L hydrochloric acid=1: 1.2-1.7), use the glass stick mixing, wetting yellow ginger, naturally place after 24 hours, the gas of packing into is carried in the tube, the hydrochloric acid 150mL of the 6.0mol/L that packs in the vaporization bottle, when being heated to 110 ℃, electric mantle voltage is adjusted in the solution boiling, is generally 75V, guarantee that gas carries that vertical yellow ginger surface temperature is 102～104 ℃ in the tube, after the acidolysis 4 hours, filter neutralization, dry, Petroleum ether extraction gets diosgenin product 1.1g, white, extraction yield 2.2%, 207～208 ℃ of fusing points.
Be used for correlated existing common process method (B technology)
2.0mol/L the direct acidolysis yellow ginger of hydrochloric acid technology----diosgenin content in the yellow ginger surveyed, so that compare with novel process.
Get the yellow ginger 50g of powder essence, add 2.0mol/L hydrochloric acid 215mL (add gradually acid to can normally stir the time only, obtain 215mL), stir, when being heated to 102 ℃, the solution boiling, after the acidolysis 10 hours, neutralization, washing, drying, Petroleum ether extraction, get product 0.9g, extraction yield 1.8%, fusing point: 207～208 ℃.
Revision test once gets product 1.0g, extraction yield 2.0%, fusing point: 207～208 ℃.Twice weight in average: 0.95g, average extraction yield: 1.9%.
The comparison of two kinds of extraction processes of table 1
The hydrochloric acidolysis yellow ginger technology (A technology) of vaporization 6.0mol/L, when test had just begun, the air-flow of rising can make yellow ginger blackening immediately, after about 10 minutes, backflow is arranged, and phegma is chocolate, and along with return time prolongs, color is thin out gradually, finally is glassy yellow.In and the little band of water yellow, yellow ginger also can obtain white crystals without washing after the acidolysis.After the acid hydrolysis solution cooling, separate out a large amount of black precipitates, these phenomenons and result show, in acidolysis yellow ginger process, the hydrochloric acid air-flow eccysis a large amount of impurity in the yellow ginger, so, economize out washing process in the test, and recycled Zhong Heshui, greatly reduced wastewater discharge.Also may be that water consumption is few, reduce the diosgenin loss, just improve the extraction yield of diosgenin.
By more above-mentioned technology as can be seen, the hydrochloric acidolysis yellow ginger (A technology) of vaporization 6.0mol/L of the present invention is excellent.
Sour gas can also obtain with other several different methods except the method described in the embodiment 1 is obtained, such as: yellow ginger is added certain water yield in advance, by feed hydrogen chloride gas in the yellow ginger to obtain sour gas, separate yellow ginger with this sour gas disacidify.
Embodiment 1 carries out in normal pressure, and suitably pressurization can reduce the time of acidolysis, raises the efficiency.
The yam of embodiment 1 is a yellow ginger, if select one of Dioscorea nipponica Mak. Ningpo Yam Rhizome, cucurbit fragrant plant for use, similar effect is arranged also.
Raw materials used among the embodiment 1 is dried yellow ginger, so it is mixed wet with sour water earlier, make it initiate, when the particulate state yellow ginger that the acidolysis of vaporization acid solution is stacked, can well contact with the material in the heap, can not absorb steam generation volumetric expansion because of the dried yellow ginger grain of heap table and stop the interior material of vaporization acid solution contact heap, influence acidolysis effect or other accidents take place.If as cadmium yellow ginger, then water or sour water are not mixed, or few water or sour water, or the time of placing be less than 10 hours, such as 3-5 hour.
Embodiment 2 hydrochloric acid amount of substance concentration are selected
In the existing industrial production, hydrochloric acid or sulfuric acid (in normal pressure or pressurization) about general use 2.0mol/L come the acidolysis yellow ginger, selecting hydrochloric acid amount of substance concentration is that 2.0mol/L must be the result that forefathers conscientiously study, so, in the novel process of design, hydrochloric acid amount of substance concentration all is foundation with 2.0mol/L.In vaporization hydrochloric acidolysis yellow ginger embodiment, how to guarantee that the hydrochloric acid amount of substance concentration on yellow ginger surface reaches 2.0mol/L? designed following test:
The hydrochloric acid 150mL that gets 6.3mol/L, 6.0mol/L, 5.8mol/L, 5.5mol/L respectively joins in the three neck round-bottomed flasks, carry at gas and to add 50g yellow ginger (yellow ginger is used 75mL, 2.0mol/L salt acid soak 24 hours in advance) in the letter respectively, heating vaporization hydrochloric acid is after 2 hours, stop heating, naturally cooling is poured out gas and is carried yellow ginger in the tube, suction filtration, generally obtain filtrate 29～37mL, use the sodium hydroxide titrimetry, the result is as follows:
Concentration of hydrochloric acid and the concentration of hydrochloric acid relation that is vaporized in table 2 filtrate
※ annotates the water content difference in the yellow ginger, can obtain different results.
Test finds that when vaporization amount of substance concentration was the hydrochloric acid of 5.8mol/L, it is longer 96～98 ℃ of times that gas is put forward the temperature maintenance that is close to the yellow ginger surface in the tube, just slowly rises to 101～102 ℃ then; When vaporization amount of substance concentration is the hydrochloric acid of 6.0mol/L, the temperature maintenance that is close to the yellow ginger surface is at 98～100 ℃ after about 10 minutes, just rise to 102～104 ℃ rapidly, and maintain in this temperature range motionless, close with the solution boiling point of the direct acidolysis yellow ginger of hydrochloric acid (B technology) that adopts 2.0mol/L, so in the test, the hydrochloric acid amount of substance concentration of preferably vaporizing is: 6.0mol/L.
If with acid gas condensation liquid concentration is control condition, the concentration when its acid gas condensation is liquid is that 1.0mol/L～6.3mol/L all can.But the concentration when being liquid state with the acid gas condensation is good at 1.8mol/L～3.5mol/L.1.0 the concentration during～1.8mol/L needs the long acidolysis time; 3.5 during～6.3mol/L, will cause more fiber degradation, can reduce the extraction yield of diosgenin, and cause the sex change of diosgenin.
Embodiment 3 hydrochloric acid, in and the recycling of water
In hydrochloric acid recycles nine processes, co-processing 9 * 50g=450g yellow ginger, do not see extraction yield and reduce phenomenon, remove when recycling for the 7th time, the product fusing point that obtains is outside 197～201 ℃, the other products fusing point is 207～208 ℃, shows to recycle hydrochloric acid to extraction yield and not influence of quality product.Limited time and will handle acid hydrolysis solution just, and abandon recirculation test.Hydrochloric acid, in and water cycle use-testing result as follows:
Table 3 recycle hydrochloric acid, in and water to the influence of product
※Annotate: in the 4th test, the part of because of carelessness extracting solution having been splashed.
Recycle in the process at hydrochloric acid and to find, after hydrochloric acid uses cooling for the first time, separate out 6.0g black sand shape precipitation; After the circulation, separate out the 11.0g black precipitate for the second time, shake bottle, overwork white cube crystallization around the bottle inwall, throw out easily is dissolved in water, can perfect combustion on electric furnace.After four circulations, the acid hydrolysis solution boiling point rises to 111 ℃, about 1 hour of heating acid hydrolysis solution, one coke charge shape thing just appears in solution surface, filter, recirculation is used, still have burnt shape thing to separate out, think by analysis: the burnt shape thing state that only reaches capacity just can be separated out, so the round-robin acid hydrolysis solution is actually burnt shape thing saturated solution at normal temperatures, in the working cycle of a new round, because constantly new burnt shape thing under the wash-out will form the saturated solution under the boiling temperature gradually, separates out phenomenon again thereby burnt shape thing occurs.So, after each circulation, as filtering acid hydrolysis solution, generally obtain 9～13g precipitation, and add the hydrochloric acid of an amount of 6.0mol/L to remove out insolubles, can avoid separating out in heat-processed too much burnt shape thing influences the hydrochloric acid vaporization.
Yellow ginger after the acidolysis is through neutralization, generally can produce 72～81mL in and waste water, it recycles situation such as table three, in and water through six circulations after, when the 7th time was used, the little band of product was yellow, the fusing point reduction.Now the diosgenin product all with fusing point as the quality of requirements, general fusing point reaches just thinks qualified more than 195 ℃, though the product fusing point that obtains after seven times of circulating is still qualified, the product tape look has just been changed Zhong Heshui.Be total in the acquisition and water 81g.
Embodiment 4 saves water-washing step
In and water and washing water are second roots that existing technology produces waste water, in vaporization hydrochloric acidolysis yellow ginger process, find, incipient phegma is chocolate, be faint yellow after about 2 hours, the little band of whole phegma is yellow, different with existing technology is that yellow ginger has passed through the repeatedly washing of vaporization hydrochloric acid in the acidolysis process, can save neutralization and washing step? try to have done single test, yellow ginger after the acidolysis is divided into two parts, and a copy of it does not neutralize and does not wash yet, and directly extract dry back, the extraction yield of diosgenin is 1.4% as a result, another part is merely hit and is not washed, and the extraction yield of diosgenin is constant as a result, and product colour does not change yet, this part shows, after the acidolysis in the yellow ginger residual acid be only the factor that influences extraction yield, so, thereafter the test in saving water-washing step.
Comprehensive go up table 1, table 3 as can be known, produces that one ton of diosgenin produces in and waste water mostly be most: 81 ÷ (1.1+1.0+1.1+0.7+1.2+1.1)=13.1 tons, at least show production technique and produce waste water less: the 150-13.1=136.9 ton.
The processing of whole waste water
Hydrochloric acidolysis liquid has just stopped continuing test after circulating through nine times, obtains spent acid solution 147g altogether.The research report that handle to extract the diosgenin spent acid solution is more, has by the distillation recovered acid
[1], also have from waste liquid and to reclaim other material
[2], the organism of having considered in the acid hydrolysis solution of acquisition enrichment has selected therefrom to reclaim the treatment process of other material.Basically according to the test method of document [2], different is not add ethanol.
Acid hydrolysis solution is behind activated carbon decolorizing, when neutralizing pH=4.0 with sodium hydroxide, separate out the grey flocks, the acid hydrolysis solution color shoals simultaneously, filters drying, obtain light grey thing 3.4g, energy perfect combustion stays lime on electric furnace, shows it is organic compound (may be the pectin of mentioning in the document [2]).
When continuing to neutralize pH=9.0, acid hydrolysis solution sends the burnt burning of intensive suddenly, filters (sad filter), drying obtains brown thing 6.7g, can perfect combustion become lime, show it is organic compound, (faint ammonia flavor is arranged, and may be the alkaloid of mentioning in the document [2]).
The about half of evaporation concentration mother liquor is separated out precipitation, filters, and during with filtrate backwash filter cake, filter cake is divided into two-layer, upper strata filter cake 21g, and color is pure white, has only a small amount of can burn (may be sodium-chlor).The brown thing 6.5g of lower floor, part can be burnt.
Continue mother liquid evaporation to doing, obtain the brown thing 46.0g that sticks, can burn at the last branch of electric furnace, a part can not be burnt, the moisture absorption in air (may be the mixture of sodium-chlor and sugar).
By top test as can be seen, do not have a large amount of byproducts of enrichment in the circulation acid hydrolysis solution, opposite with first imagination, in the acid hydrolysis solution working cycle, byproduct major part is separated out, so acid hydrolysis solution recycles the not influence of product extraction yield, performance, acid hydrolysis solution might infinite loop use, the also accidental short-cut method that has obtained to reclaim byproduct.
According to above-mentioned test, the steps in sequence of whole wastewater treatment method is:
Whole waste water, activated carbon decolorizing, the pH=4.0 that neutralizes filters 1, and the filtrate pH=9.0 that neutralizes filters 2, an amount of evaporation concentration, filter 23, mother liquor extracts glucose.
Wherein: filter for the first time and obtain pectin; Filter for the second time and obtain alkaloid; Filter for the third time and obtain sodium-chlor.
According to existing test-results, the spent acid solution of producing the generation of ton diosgenin is: 147 ÷ (1.0+1.1+1.0+1.1+0.7+1.2+1.1+1.1+1.1+1.1)=14 tons, at least now production technique produces spent acid solution less: the 350-14=336 ton.
Conclusion:
1 has searched out a kind of novel process of extracting diosgenin, and processing condition are: the hot gas of acid solution is contacted with granular or powdered yam, with hot sour gas plant is carried out acidolysis, the acidolysis slag after filtration, neutralization, after the drying, Petroleum ether extraction, evaporation, crystallization gets product.The fusing point of product is: 207～208 ℃, average extraction yield is: 2.2%, and now technology is high by 0.3%.Technology is simple, and is workable, has the real world applications meaning.
2 acid hydrolysis solutions, Zhong Heshui can recycle, and the impurity of vaporization hydrochloric acid solution in can the eccysis yellow ginger has saved washing process again.Now technology relatively with 136.9 tons of water, washing water, produces 336 tons of spent acid solutions during a ton product produces at least and gives up less together, basically eliminated with serious pollution a large amount of spent acid solution, reach the purpose that stops waste water from the source, if can implement, will benefit hundred Wan Jiangnong and divert water from the south to the north project.
3 acid hydrolysis solutions are in recycling process, play the effect of enrichment byproduct simultaneously, after reaching capacity, byproduct direct crystallization from acid hydrolysis solution is separated out, avoided present recovery byproduct to need the defective of evaporation concentration mother liquor, provide possibility for further from spent acid solution, extracting product innovation.
Citing document
1. Zou Yi is flat, Xu Haichao: turmeric saponin process for treating industrial waste water and comprehensive utilization [P] .CN1488581,2004-04-14.
2. Zou Yi is flat: a kind of turmeric saponin processing method of industrial waste water [P] .CN1587081A, 2005-03-02.
Claims (10)
1, extract the sour acid hydrolyzation of vaporization of diosgenin, it is characterized in that: the hot gas of acid solution is contacted with granular or powdered yam, plant is carried out acidolysis, filter with hot sour gas, neutralization, drying is extracted, and gets powdery diosgenin product.
2, the vaporization of extraction diosgenin as claimed in claim 1 acid acid hydrolyzation, it is characterized in that: described yam is at least one of yellow ginger, Dioscorea nipponica Mak. Ningpo Yam Rhizome, cucurbit fragrant plant.
3, the vaporization of extraction diosgenin as claimed in claim 2 acid acid hydrolyzation is characterized in that: when described yam was yellow ginger, acidolysis can stop when the phlegma of the acidolysis gas of contacted plant is glassy yellow.
4, as the vaporization acid acid hydrolyzation of claim 1 or 2 or 3 described extraction diosgenins, it is characterized in that: described acid solution is a hydrochloric acid solution, and the concentration when its acid gas condensation is liquid is 1.0mol/L～6.3mol/L.
5, the vaporization of extraction diosgenin as claimed in claim 4 acid acid hydrolyzation is characterized in that: the concentration when acid gas condensation is liquid is 1.8mol/L～3.5mol/L.
6, as the vaporization acid acid hydrolyzation of claim 1 or 2 or 3 described extraction diosgenins, it is characterized in that: the amount concentration of the fluent meterial of hydrochloric acid solution is 3.1mol/L～6.3mol/L.
7, as the sour acid hydrolyzation of the vaporization of claim 1 or 2 or 3 described extraction diosgenins, it is characterized in that: with the hot gas of acid solution with before granular or powdered yam contact, elder generation's water or 2.0 ± 0.5mol/l acid solution are mixed granular or powdered yam wet, placed 10～24 hours, the sour gas of reusable heat carries out acidolysis to granular or powdered yam then.
8, as the sour acid hydrolyzation of the vaporization of claim 1 or 2 or 3 described extraction diosgenins, it is characterized in that: with the hot gas of acid solution with before granular or powdered yam contact, earlier carry out pre-treatment with aging process, enzyme method for pretreating, partition method, the sour gas of reusable heat carries out acidolysis to the material that contains diosgenin then.
9, as the vaporization of claim 1 or 2 or 3 described extraction diosgenins acid acid hydrolyzation, it is characterized in that: the hot/cold acid solution and the Zhong Heshui of yam are crossed in acidolysis, directly the next batch raw material is reused; Or hot acid liquid is cooled to normal temperature, its precipitate is rejected back revaporization use.
10, as the vaporization acid acid hydrolyzation of claim 1 or 2 or 3 described extraction diosgenins, it is characterized in that: the acid liquor temperature of yam uppermost surface is at 96～110 ℃.
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| CN1243834A (en) * | 1999-06-27 | 2000-02-09 | 中国科学院昆明植物研究所 | Process for preparing yam saponin |
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| Title |
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| 黄姜中薯蓣皂素的制取方法. 陈俊英等.农产品加工（学刊），第1期. 2005 |
| 黄姜中薯蓣皂素的制取方法. 陈俊英等.农产品加工（学刊），第1期. 2005 * |
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