CN102464700A - Hydrolysis extraction process for yam diosgenin - Google Patents
Hydrolysis extraction process for yam diosgenin Download PDFInfo
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- CN102464700A CN102464700A CN2010105482676A CN201010548267A CN102464700A CN 102464700 A CN102464700 A CN 102464700A CN 2010105482676 A CN2010105482676 A CN 2010105482676A CN 201010548267 A CN201010548267 A CN 201010548267A CN 102464700 A CN102464700 A CN 102464700A
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- 230000007062 hydrolysis Effects 0.000 title claims abstract description 49
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 49
- 238000000605 extraction Methods 0.000 title claims abstract description 35
- DWCSNWXARWMZTG-UHFFFAOYSA-N Trigonegenin A Natural products CC1C(C2(CCC3C4(C)CCC(O)C=C4CCC3C2C2)C)C2OC11CCC(C)CO1 DWCSNWXARWMZTG-UHFFFAOYSA-N 0.000 title abstract description 3
- WQLVFSAGQJTQCK-VKROHFNGSA-N diosgenin Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)CC4=CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 WQLVFSAGQJTQCK-VKROHFNGSA-N 0.000 title abstract description 3
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 title abstract description 3
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 80
- 229930182490 saponin Natural products 0.000 claims abstract description 79
- 150000007949 saponins Chemical class 0.000 claims abstract description 79
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 26
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims description 46
- 239000003921 oil Substances 0.000 claims description 36
- 239000012065 filter cake Substances 0.000 claims description 32
- 239000002002 slurry Substances 0.000 claims description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- 235000003392 Curcuma domestica Nutrition 0.000 claims description 21
- 244000008991 Curcuma longa Species 0.000 claims description 21
- 235000003373 curcuma longa Nutrition 0.000 claims description 21
- 235000013976 turmeric Nutrition 0.000 claims description 21
- 244000062245 Hedychium flavescens Species 0.000 claims description 18
- 239000001913 cellulose Substances 0.000 claims description 18
- 229920002678 cellulose Polymers 0.000 claims description 18
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000013078 crystal Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- 238000002425 crystallisation Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 11
- 235000021463 dry cake Nutrition 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 9
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- 239000000047 product Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 230000003139 buffering effect Effects 0.000 claims description 7
- 230000004888 barrier function Effects 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
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- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
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- 238000003860 storage Methods 0.000 claims description 5
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- 239000002699 waste material Substances 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims 1
- 238000000855 fermentation Methods 0.000 abstract description 5
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- 238000010586 diagram Methods 0.000 abstract description 3
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- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 2
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a hydrolysis extraction process for yam diosgenin. The process comprises a dried substance hydrolysis process flow and a saponin extraction process flow. According to the invention, the dried substance hydrolysis process flow is improved, and diagram press filtration and diagram acid removal steps are added, so that the saponin content of a dried substance is increased greatly, and can be about 50 percent, and the petroleum loss in a saponin extraction process is reduced; meanwhile, the product quality is enhanced, and a melting point is raised from 195 DEG C to over 197 DEG C. Due to the adoption of the hydrolysis extraction process serving as a novel non-fermentation acid hydrolysis process, the problem of serious odor caused by the conventional fermentation process is solved, saponin recovery rate and product purity are increased, treatment time is saved, land and equipment utilization ratios are increased greatly, and the dosage of acid is reduced.
Description
Technical field
The present invention relates to a kind of saponin hydrolysis extraction process, be specifically related to a kind of turmeric saponin hydrolysis extraction process.
Background technology
Traditional turmeric saponin complete processing is basically: pulverize-fermentation-acidolysis in advance-extraction of hydrolyzate extraction-saponin, wherein pollution mainly comes from the hydrolyzate course of processing.Because this technology has only been utilized the saponin in the yellow ginger, and,, make it become pollutent and get in the waste water, both wasted resource, strengthened the difficulty of wastewater treatment again like starch, Mierocrystalline cellulose etc. with other physical obsolescences.The key problem in technology link of traditional technology is to utilize acid hydrolysis that the glucoside key is broken off, but meanwhile the starch in the yellow ginger also is hydrolyzed into and is glucose, produces a large amount of organic pollutants, becomes the main pollution source of waste water.According to conservative estimation, the organism that produces after the starch hydrolysis is contributed at least more than 80% the COD in the waste water.
The method that the saponin production technique of extracting yellow ginger adopts at present both at home and abroad mainly contains three kinds of biochemical process, physico-chemical process and physics methods.The biochemical process main thought is that yellow ginger is pulverized pre-treatment, through the saccharification starch-splitting, starch liquid sugar is separated with sugared slag again, and sugared slag is carried out extracting saponin after the acidolysis.The physico-chemical process main thought is with yellow ginger section, dry, pulverizing, to the lixiviate of yellow ginger dry powder, obtains saponin organic solvent medicinal extract with organic solvent, and acidolysis medicinal extract extracts saponin then.Physics method main thought be with yellow ginger directly pulverize, defibrination, adopt physical method for separation to go out Mierocrystalline cellulose and starch, then a minute fluid sink slurry, separation of supernatant concentrates, again with liquid concentrator acidolysis extraction saponin.
Above several method physics method is the simplest, and product is many.Sour water after the acidolysis is few, and acid consumption is little, and working cost is low.But in the production technique of physics method, its starch and cellulosic utilization ratio are low, cause the stock number expense, correspondingly, because have the starch and the Mierocrystalline cellulose of utilization or not, pollute harm; Secondly, in the step of acidolysis fermentation, owing to fermentation brings serious stench, contaminate environment; Once more, in the step of acidolysis fermentation, still will use a large amount of acid, cost is relatively still high, moreover the COD of hydrolyzate generation waste water is higher relatively, and the WWT difficulty is high.These defectives and deficiency, serious bitter logos extracts the development of turmeric saponin technology.Publication number is that to disclose " from yellow ginger, extracting complete processing and the equipment of saponin with direct method of isolation " and publication number be that the Chinese patent of CN1174995C discloses " the direct method of isolation yellow ginger extracts the technology of saponin " they all are that the physics method is extracted saponin to the Chinese patent of CN1268635C; Pulverizing is specifically all arranged; The step of separating and extracting, still, discover: the saponin content of the dry thing of hydrolysis that obtains according to their process method is low; Can consume a large amount of acid in the extraction link; Production cost is very high, and the intractability of sewage can be very big, do not meet whole nation's theory of present energy-saving and emission-reduction.
Summary of the invention
The object of the present invention is to provide a kind of turmeric saponin hydrolysis extraction process, it has solved the technical problem that saponin content is low and production cost is high of the dry thing of hydrolysis in the background technology.
Technical solution of the present invention is:
A kind of turmeric saponin hydrolysis extraction process, its special character is that this extraction process may further comprise the steps:
1) the dry thing technical process of hydrolysis
(1) cleans
The yellow ginger raw material after arrangement and cleaning, remove silt particle with and the earth of surface adhesion;
(2) broken mill
Insert crusher in crushing again, and slurry by volume: the water addition ratio example is 30% of a raw material, forms slurry and flows into dashpot, inserts needle mill again and is ground to the 80-100 order;
Remove large particulate matter with vibratory screening apparatus again after the grinding; Said large particulate matter is meant the particulate matter of particle diameter below 80 orders;
(3) squeezing
It is 3% sulfuric acid adjustment pH value 5-5.5 that above-mentioned slurry is used mass percent again, and stirs, and inserts belt press again, under the condition of 0.2Mpa, squeezes, and isolates Mierocrystalline cellulose and slurry, and the slurry after the squeezing is collected in the new dashpot;
(4) spiral shell for sleeping in is centrifugal
After the buffering, use sulfuric acid adjustment pH value to be 5-5.5 again, insert horizontal screw centrifuge again and separate, centrifuge speed is 4700 rev/mins, centrifugal 4-6 minute;
(5) barrier film press filtration
With the centrifugate of isolated Mierocrystalline cellulose of step (3) and step (4) in proportion, the ratio of Mierocrystalline cellulose and centrifugate is 2: 3, mixes to form mixture; Filter said mixture with diaphragm filter press, its pressure is not less than 40% block filter cake for solid content the most at last;
(6) stirring and dissolving
With above-mentioned filter cake according to a certain percentage, the ratio of filter cake and acid solution is 1: 1.5, and being dissolved in mass percent is 30% sulfuric acid liquid, and in the acid waste liquid that discharges after the acidolysis, the formation acid hydrolysis solution stirs;
(7) barrier film depickling
Above-mentioned acid hydrolysis solution is inserted depickling with in the diaphragm filter press, and at first press filtration becomes solid content to be not more than 30% filter cake, and the spent acid solution that leaches is collected into acid solution storage tank after the hydrolysis; Filter cake is carried out the wash cycles depickling, is neutral until water outlet pH; Again filter cake is pressed into solid content and is not less than 50% dry cake;
(8) oven dry
With above-mentioned dry cake through centrifuge dehydration, kibbler pulverize be no more than the fine granularity of 1cm for diameter after, get into baking room and dry 22-26h not being higher than under 80 ℃ the condition, be the dry thing of hydrolysis;
2) saponin extraction process flow process:
(1) solvent extraction
The dry thing of hydrolysis is inserted in the extractor, add solvent oil No. 120, the ratio of hydrolyzate and solvent oil is 1: 4, and through No. 120 solvent oils to 85 in the steam heating extractor ℃-95 ℃, the continuous backflow extraction is 6-8 hour with this understanding;
(2) distillation concentrates
After extract finishing, saponin and No. 120 solvent oils form the saponin solvents, and it is 1: 40 concentration than solvent oil volume ratio that the saponin solvent is distilled to saponin;
(3) crystallisation by cooling
Again the saponin solvent is inserted crystallization in the crystallizer, through the time crystallization more than 24 hours, get crystal solution, the temperature of crystal solution is not higher than 20 ℃;
(4) separate oven dry
Crystal solution is inserted whizzer separate,, and send to drying baker after the oil filter done, take out again after the drying, be the finished product turmeric saponin through being crushed to 300 orders again through No. 120 solvent oils washings.
Above-mentioned (3) squeezing step comprises twice pressing or the repeatedly squeezing with (3) squeezing step same operation.
Also comprise between above-mentioned (2) broken mill step and (3) squeezing step: remove large particulate matter with vibratory screening apparatus again after the grinding; Said large particulate matter is meant the particulate matter of particle diameter more than 80 orders;
Crouch and also comprise between spiral shell centrifugation step in above-mentioned (3) squeezing step and (4): the slurry that step (3) obtains is inserted vibratory screening apparatus, remove fibrous residue residual in the slurry after, insert another new dashpot buffering and precipitate, carry out fine separation, cushion 24 hours;
What in above-mentioned (7) barrier film depickling step filter cake is carried out that the wash cycles depickling adopts is that multistage recirculated water cleans.
Above-mentioned squeezing machine is a belt press.
Above-mentioned whizzer is a horizontal screw centrifuge.
The present invention realizes starch and cellulosic high-efficiency comprehensive utilization, and resource utilization is high.The process for cleanly preparing that order of the present invention adopts is set up on physics method basis.
Operational path of the present invention is abideed by the guiding theory of comprehensive utilization, recycling economy, cleaner production; Biology characteristics according to yellow ginger; Constantly absorb the modern technique of research of the same trade both at home and abroad, use modern food production theory, set up yellow ginger and produced the cleaner production demonstration line of saponin.This technical characterstic is following:
(1) with the theory follow through of recycling industries and clean production process exploitation with use, make every effort under economically viable prerequisite, utilize the yellow ginger resource fully, avoid secondary pollution, be convenient to large-scale promotion.
(2) studied successfully yellow ginger slurry nonfermented acidolysis novel process; Eliminate the serious stench problem that traditional zymotic technology is brought, and improved the saponin recovery and product purity, saved the treatment time; Increase substantially soil and equipment efficiency of usage, reduced sour consumption.
(3) reduce wastewater flow rate significantly and also reduced the COD of hydrolyzate generation waste water in the production process effectively, reduced acidolysis, significantly reduced WWT difficulty and expense with the acid amount.
(4) the hydrolyzate saponin content is for to bring up to 45-50% from traditional 12-14%, reduced the gasoline loss in the saponin leaching process, for the increase of subsequent technique benefit provides prerequisite; Quality product also is improved simultaneously; Fusing point is increased to more than 197 ℃ from 195 ℃.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment 1:
A kind of turmeric saponin hydrolysis extraction process comprises: 1) the dry thing technical process of hydrolysis
(1) the yellow ginger raw material is after arrangement and cleaning, remove silt particle with and the earth of surface adhesion;
(2) insert crusher in crushing again, and slurry by volume: the water addition ratio example is 30% of a raw material, forms slurry and flows into dashpot, inserts needle mill again and is ground to 80 orders;
(3) above-mentioned slurry being used mass percent again is 3% sulfuric acid adjustment pH value 5, and stirs, and inserts belt press again, under the condition of 0.2Mpa, squeezes, and isolates Mierocrystalline cellulose and slurry, and the slurry after the squeezing is collected in the new dashpot; Fully can carry out twice pressing or repeatedly squeezing in order to squeeze;
(4) after the buffering, using sulfuric acid adjustment pH value again is 5, inserts horizontal screw centrifuge again and separates, and centrifuge speed is 4700 rev/mins, centrifugal 4 minutes;
(5) with the centrifugate of isolated Mierocrystalline cellulose of step (3) and step (4) in proportion, the ratio of Mierocrystalline cellulose and centrifugate is 2: 3, mixes to form mixture; Filter said mixture with diaphragm filter press, it is pressed and is the block filter cake of solid content 50% the most at last;
(6) according to a certain percentage, the mass ratio of filter cake and acid solution is 1: 1.5, and being dissolved in mass percent is 30% sulfuric acid liquid, and in the acid waste liquid that discharges after the acidolysis, the formation acid hydrolysis solution stirs with above-mentioned filter cake;
(7) above-mentioned acid hydrolysis solution is inserted depickling with in the diaphragm filter press, at first press filtration becomes the filter cake of solid content 20%, and the spent acid solution that leaches is collected into acid solution storage tank after the hydrolysis; Adopting multistage recirculated water to carry out the wash cycles depickling to filter cake, is neutral until water outlet pH; Again filter cake is pressed into the dry cake of solid content 50%;
(8) with above-mentioned dry cake through centrifuge dehydration, kibbler pulverize be no more than the fine granularity of 1cm for diameter after, get into baking room and under 70 ℃ condition, dry 22h, be the dry thing of hydrolysis, the dry thing saponin content of this hydrolysis is 30%;
2) saponin extraction process flow process:
(1) the dry thing of hydrolysis is inserted in the extractor, add solvent oil No. 120, the ratio of hydrolyzate and solvent oil is 1: 4, and through No. 120 solvent oils to 85 in the steam heating extractor ℃, the continuous backflow extraction is 6 hours with this understanding;
(2) extract to finish after, saponin and No. 120 solvent oils form the saponin solvents, it is 1: 40 concentration than solvent oil volume ratio that the saponin solvent is distilled to saponin;
(3) again the saponin solvent is inserted crystallization in the crystallizer, the time crystallization through 24 hours gets crystal solution, 20 ℃ of the temperature of crystal solution;
(4) crystal solution is inserted whizzer and separate,, and send to drying baker after the oil filter done, take out again after the drying, be the finished product turmeric saponin through being crushed to 300 orders again through No. 120 solvent oils washings.
Embodiment 2:
A kind of turmeric saponin hydrolysis extraction process comprises: 1) the dry thing technical process of hydrolysis
(1) the yellow ginger raw material is after arrangement and cleaning, remove silt particle with and the earth of surface adhesion;
(2) insert crusher in crushing again, and slurry by volume: the water addition ratio example is 30% of a raw material, forms slurry and flows into dashpot, inserts needle mill again and is ground to 100 orders;
(3) above-mentioned slurry being used mass percent again is 3% sulfuric acid adjustment pH value 5.5, and stirs, and inserts belt press again, under the condition of 0.2Mpa, squeezes, and isolates Mierocrystalline cellulose and slurry, and the slurry after the squeezing is collected in the new dashpot; Fully can carry out twice pressing or repeatedly squeezing in order to squeeze;
(4) after the buffering, using sulfuric acid adjustment pH value again is 5.5, inserts horizontal screw centrifuge again and separates, and centrifuge speed is 4700 rev/mins, centrifugal 6 minutes;
(5) with the centrifugate of isolated Mierocrystalline cellulose of step (3) and step (4) in proportion, the ratio of Mierocrystalline cellulose and centrifugate is 2: 3, mixes to form mixture; Filter said mixture with diaphragm filter press, it is pressed and is the block filter cake of solid content 40% the most at last;
(6) according to a certain percentage, the mass ratio of filter cake and acid solution is 1: 1.5, and being dissolved in mass percent is 30% sulfuric acid liquid, and in the acid waste liquid that discharges after the acidolysis, the formation acid hydrolysis solution stirs with above-mentioned filter cake;
(7) above-mentioned acid hydrolysis solution is inserted depickling with in the diaphragm filter press, at first press filtration becomes the filter cake of solid content 30%, and the spent acid solution that leaches is collected into acid solution storage tank after the hydrolysis; Adopting multistage recirculated water to carry out the wash cycles depickling to filter cake, is neutral until water outlet pH; Again filter cake is pressed into the dry cake of solid content 50%;
(8) with above-mentioned dry cake through centrifuge dehydration, kibbler pulverize be no more than the fine granularity of 1cm for diameter after, get into baking room and dry 26h not being higher than under 80 ℃ the condition, be the dry thing of hydrolysis, the dry thing saponin content of this hydrolysis is 35%;
2) saponin extraction process flow process:
(1) the dry thing of hydrolysis is inserted in the extractor, add solvent oil No. 120, the ratio of hydrolyzate and solvent oil is 1: 4, and through No. 120 solvent oils to 95 in the steam heating extractor ℃, the continuous backflow extraction is 8 hours with this understanding;
(2) extract to finish after, saponin and No. 120 solvent oils form the saponin solvents, it is 1: 40 concentration than solvent oil volume ratio that the saponin solvent is distilled to saponin;
(3) again the saponin solvent is inserted crystallization in the crystallizer, the time crystallization through 26 hours gets crystal solution, 18 ℃ of the temperature of crystal solution;
(4) crystal solution is inserted whizzer and separate,, and send to drying baker after the oil filter done, take out again after the drying, be the finished product turmeric saponin through being crushed to 300 orders again through No. 120 solvent oils washings.
Embodiment 3
A kind of turmeric saponin hydrolysis extraction process comprises: 1) the dry thing technical process of hydrolysis
(1) the yellow ginger raw material is after arrangement and cleaning, remove silt particle with and the earth of surface adhesion;
(2) insert crusher in crushing again, and slurry by volume: the water addition ratio example is 30% of a raw material, forms slurry and flows into dashpot, inserts needle mill again and is ground to 100 orders;
(3) above-mentioned slurry being used mass percent again is 3% sulfuric acid adjustment pH value 5.2, and stirs, and inserts belt press again, under the condition of 0.2Mpa, squeezes, and isolates Mierocrystalline cellulose and slurry, and the slurry after the squeezing is collected in the new dashpot; Fully can carry out twice pressing or repeatedly squeezing in order to squeeze;
(4) after the buffering, using sulfuric acid adjustment pH value again is 5.2, inserts horizontal screw centrifuge again and separates, and centrifuge speed is 4700 rev/mins, centrifugal 5 minutes;
(5) with the centrifugate of isolated Mierocrystalline cellulose of step (3) and step (4) in proportion, the ratio of Mierocrystalline cellulose and centrifugate is 2: 3, mixes to form mixture; Filter said mixture with diaphragm filter press, it is pressed and is the block filter cake of solid content 40% the most at last;
(6) according to a certain percentage, the mass ratio of filter cake and acid solution is 1: 1.5, and being dissolved in mass percent is 30% sulfuric acid liquid, and in the acid waste liquid that discharges after the acidolysis, the formation acid hydrolysis solution stirs with above-mentioned filter cake;
(7) above-mentioned acid hydrolysis solution is inserted depickling with in the diaphragm filter press, at first press filtration becomes the filter cake of solid content 25%, and the spent acid solution that leaches is collected into acid solution storage tank after the hydrolysis; Adopting multistage recirculated water to carry out the wash cycles depickling to filter cake, is neutral until water outlet pH; Again filter cake is pressed into the dry cake of solid content 50%;
(8) with above-mentioned dry cake through centrifuge dehydration, kibbler pulverize be no more than the fine granularity of 1cm for diameter after, get into baking room and under 75 ℃ condition, dry 24h, be the dry thing of hydrolysis, the dry thing saponin content of this hydrolysis is 35%;
2) saponin extraction process flow process:
(1) the dry thing of hydrolysis is inserted in the extractor, add solvent oil No. 120, the ratio of hydrolyzate and solvent oil is 1: 4, and through No. 120 solvent oils to 90 in the steam heating extractor ℃, the continuous backflow extraction is 7 hours with this understanding;
(2) extract to finish after, saponin and No. 120 solvent oils form the saponin solvents, it is 1: 40 concentration than solvent oil volume ratio that the saponin solvent is distilled to saponin;
(3) again the saponin solvent is inserted crystallization in the crystallizer, the time crystallization through 26 hours gets crystal solution, 20 ℃ of the temperature of crystal solution;
(4) crystal solution is inserted whizzer and separate,, and send to drying baker after the oil filter done, take out again after the drying, be the finished product turmeric saponin through being crushed to 300 orders again through No. 120 solvent oils washings.
Unit product consumption indicators table of the present invention (ton saponin)
The old and new's technology contrast table
Diosgenin quality standard (Shaanxi DB185-85)
| Project | Index |
| Outward appearance | White or little yellow lightweight powder |
| Color and luster | Must not be deeper than standard color solution |
| Purity | 1: 100 (saponin: 95% ethanol) remarkable alcohol insoluble solids must not be arranged |
| Fusing point | ≥195℃ |
| Weight loss on drying | ≤0.5％ |
Main technique technical parameter of the present invention
| The technical parameter title | Index |
| Concentrate end of a period saponin solution | Saponin: solvent oil=1: 40 |
| Crystallization end of a period crystal solution temperature | Be not higher than 20 ℃ |
| Saponin oven dry back is weightless | Less than 5 ‰ |
| Fragmentation adds water | Fresh ginger: water=1: 2 |
| The hydrolysis vapor pressure | 0.2MPa |
| The hydrolysis cycle | 4h |
| Drying temperature | Be not higher than 80 ℃ |
| Time of drying | About 24h |
| The dry thing of hydrolysis is moisture | Be not higher than 5% |
Claims (7)
1. turmeric saponin hydrolysis extraction process, its special character is that this extraction process may further comprise the steps:
1) the dry thing technical process of hydrolysis
(1) cleans
The yellow ginger raw material after arrangement and cleaning, remove silt particle with and the earth of surface adhesion;
(2) broken mill
Insert crusher in crushing again, and slurry by volume: the water addition ratio example is 30% of a raw material, forms slurry and flows into dashpot, inserts needle mill again and is ground to the 80-100 order;
(3) squeezing
It is 3% sulfuric acid adjustment pH value 5-5.5 that above-mentioned slurry is used mass percent again, and stirs, and inserts belt press again, under the condition of 0.2Mpa, squeezes, and isolates Mierocrystalline cellulose and slurry, and the slurry after the squeezing is collected in the new dashpot;
(4) spiral shell for sleeping in is centrifugal
After the buffering, use sulfuric acid adjustment pH value to be 5-5.5 again, insert horizontal screw centrifuge again and separate, centrifuge speed is 4700 rev/mins, centrifugal 4-6 minute;
(5) barrier film press filtration
With the centrifugate of isolated Mierocrystalline cellulose of step (3) and step (4) in proportion, the ratio of Mierocrystalline cellulose and centrifugate is 2: 3, mixes to form mixture; Filter said mixture with diaphragm filter press, its pressure is not less than 40% block filter cake for solid content the most at last;
(6) stirring and dissolving
With above-mentioned filter cake according to a certain percentage, the ratio of filter cake and acid solution is 1: 1.5, and being dissolved in mass percent is 30% sulfuric acid liquid, and in the acid waste liquid that discharges after the acidolysis, the formation acid hydrolysis solution stirs;
(7) barrier film depickling
Above-mentioned acid hydrolysis solution is inserted depickling with in the diaphragm filter press, and at first press filtration becomes solid content to be not more than 30% filter cake, and the spent acid solution that leaches is collected into acid solution storage tank after the hydrolysis; Filter cake is carried out the wash cycles depickling, is neutral until water outlet pH; Again filter cake is pressed into solid content and is not less than 50% dry cake;
(8) oven dry
With above-mentioned dry cake through centrifuge dehydration, kibbler pulverize be no more than the fine granularity of 1cm for diameter after, get into baking room and dry 22-26h not being higher than under 80 ℃ the condition, be the dry thing of hydrolysis;
2) saponin extraction process flow process:
(1) solvent extraction
The dry thing of hydrolysis is inserted in the extractor, add solvent oil No. 120, the ratio of hydrolyzate and solvent oil is 1: 4, and through No. 120 solvent oils to 85 in the steam heating extractor ℃-95 ℃, the continuous backflow extraction is 6-8 hour with this understanding;
(2) distillation concentrates
After extract finishing, saponin and No. 120 solvent oils form the saponin solvents, and it is 1: 40 concentration than solvent oil volume ratio that the saponin solvent is distilled to saponin;
(3) crystallisation by cooling
Again the saponin solvent is inserted crystallization in the crystallizer, through the time crystallization more than 24 hours, get crystal solution, the temperature of crystal solution is not higher than 20 ℃;
(4) separate oven dry
Crystal solution is inserted whizzer separate,, and send to drying baker after the oil filter done, take out again after the drying, be the finished product turmeric saponin through being crushed to 300 orders again through No. 120 solvent oils washings.
2. according to the said turmeric saponin hydrolysis of claim 1 extraction process, it is characterized in that: said (3) squeezing step comprises twice pressing or the repeatedly squeezing with (3) squeezing step same operation.
3. according to the said turmeric saponin hydrolysis of claim 1 extraction process, it is characterized in that, also comprise between said (2) broken mill step and (3) squeezing step: remove large particulate matter with vibratory screening apparatus again after the grinding; Said large particulate matter is meant the particulate matter of particle diameter more than 80 orders.
4. according to the said turmeric saponin hydrolysis of claim 1 extraction process; It is characterized in that: crouch and also comprise between the spiral shell centrifugation step in said (3) squeezing step and (4): the slurry that step (3) obtains is inserted vibratory screening apparatus; After removing fibrous residue residual in the slurry; Insert another new dashpot buffering deposition, carry out fine separation, cushion 24 hours.
5. according to the said turmeric saponin hydrolysis of claim 1 extraction process, it is characterized in that: what in said (7) barrier film depickling step filter cake is carried out that the wash cycles depickling adopts is that multistage recirculated water cleans.
6. according to the said turmeric saponin hydrolysis of claim 5 extraction process, it is characterized in that: said squeezing machine is a belt press.
7. according to the said turmeric saponin hydrolysis of claim 6 extraction process, it is characterized in that: said whizzer is a horizontal screw centrifuge.
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Cited By (4)
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| CN102775464A (en) * | 2012-07-30 | 2012-11-14 | 中国环境科学研究院 | Method for washing turmeric saponin acid hydrolysate |
| CN103342731A (en) * | 2013-07-29 | 2013-10-09 | 中国环境科学研究院 | Separation, rinsing and drying integrated method in saponin extraction technology |
| CN103848882A (en) * | 2013-12-20 | 2014-06-11 | 西北农林科技大学 | Turmeric saponin extraction method without waste emission |
| CN110922446A (en) * | 2019-12-23 | 2020-03-27 | 郑州金翰粮油机械工程有限公司 | Production process of diosgenin without wastewater discharge |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775464A (en) * | 2012-07-30 | 2012-11-14 | 中国环境科学研究院 | Method for washing turmeric saponin acid hydrolysate |
| CN102775464B (en) * | 2012-07-30 | 2015-04-01 | 中国环境科学研究院 | Method for washing turmeric saponin acid hydrolysate |
| CN103342731A (en) * | 2013-07-29 | 2013-10-09 | 中国环境科学研究院 | Separation, rinsing and drying integrated method in saponin extraction technology |
| CN103342731B (en) * | 2013-07-29 | 2015-08-12 | 中国环境科学研究院 | Separation, rinsing and drying integrated method in saponin extraction technology |
| CN103848882A (en) * | 2013-12-20 | 2014-06-11 | 西北农林科技大学 | Turmeric saponin extraction method without waste emission |
| CN103848882B (en) * | 2013-12-20 | 2015-10-28 | 西北农林科技大学 | A kind of turmeric saponin extracting method of non-waste-emission |
| CN110922446A (en) * | 2019-12-23 | 2020-03-27 | 郑州金翰粮油机械工程有限公司 | Production process of diosgenin without wastewater discharge |
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