CN102745840B - Method for recycling diosgenin saponin acidolysis waste acid - Google Patents
Method for recycling diosgenin saponin acidolysis waste acid Download PDFInfo
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- CN102745840B CN102745840B CN201210269041.1A CN201210269041A CN102745840B CN 102745840 B CN102745840 B CN 102745840B CN 201210269041 A CN201210269041 A CN 201210269041A CN 102745840 B CN102745840 B CN 102745840B
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- Prior art keywords
- acidolysis
- slurry
- turmeric saponin
- saponin
- spent acid
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- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 85
- 229930182490 saponin Natural products 0.000 title claims abstract description 84
- 239000002253 acid Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 56
- 239000002699 waste material Substances 0.000 title abstract description 13
- 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 6
- 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 6
- -1 diosgenin saponin Chemical class 0.000 title abstract 6
- 238000004064 recycling Methods 0.000 title abstract 3
- 235000003392 Curcuma domestica Nutrition 0.000 claims abstract description 76
- 235000003373 curcuma longa Nutrition 0.000 claims abstract description 76
- 235000013976 turmeric Nutrition 0.000 claims abstract description 76
- 244000008991 Curcuma longa Species 0.000 claims abstract description 73
- 239000002002 slurry Substances 0.000 claims abstract description 69
- 239000007787 solid Substances 0.000 claims abstract description 40
- 238000001914 filtration Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000011268 mixed slurry Substances 0.000 claims abstract description 6
- 150000007949 saponins Chemical class 0.000 claims description 78
- 239000000835 fiber Substances 0.000 claims description 38
- 230000003311 flocculating effect Effects 0.000 claims description 35
- 244000062245 Hedychium flavescens Species 0.000 claims description 25
- 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 25
- 238000013467 fragmentation Methods 0.000 claims description 19
- 238000006062 fragmentation reaction Methods 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 13
- 238000000053 physical method Methods 0.000 claims description 12
- 238000000855 fermentation Methods 0.000 claims description 6
- 230000004151 fermentation Effects 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 235000019362 perlite Nutrition 0.000 claims description 2
- 239000010451 perlite Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000012141 concentrate Substances 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 4
- 244000163122 Curcuma domestica Species 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Fertilizers (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a method for recycling diosgenin saponin acidolysis waste acid, which comprises the following steps: (a) filtering hydrolyzed slurry of the diosgenin saponin in the industry to obtain a waste acid liquor; (b) smashing turmeric, concentrating obtained diosgenin saponin slurry to enable the solid content of the diosgenin saponin slurry to be more 10wt%, and sufficiently and directly mixing the waste acid liquor with the diosgenin saponin material with the solid content more than 10wt%; and (c) carrying out acidolysis on the mixed slurry by adopting a traditional acidolysis process so as to directly recycle reacted acid in the waste acid liquor. The method can be used for directly recycling the waste acid liquor to production without any treatment after the waste acid liquor is recovered, so the generation and drainage of 80%-90% of acid waste liquid are reduced.
Description
Technical field
The present invention relates to the method for a kind of turmeric saponin acidolysis spent acid reuse, be applied to turmeric saponin processing industry hydrolyzate processing link.
Background technology
The traditional technology that turmeric saponin processing industry generally takes yellow ginger pulverizing-fermentation-acidolysis-hydrolyzate-saponin to extract at present.In this technique acidolysis process, can produce a large amount of acid solutions, because wherein acid content is low, be difficult to recycle, mostly directly discharge.
This spent acid solution belongs to high density containing sour organic waste water, and because saponin content in yellow ginger is on average in 6 ‰ left and right, one ton of saponin of every production will produce 200-400m
3spent acid solution.Its biodegradability is poor, acidity is high, sugar part content is high, COD surpasses 100,000 mg/L, does not have so far economically viable treatment technology and method, is the key problem that turmeric saponin processing waste water is difficult to qualified discharge.
Summary of the invention
Main purpose of the present invention is to provide a kind of method that in the acid waste liquid that turmeric saponin machining produces, low-concentration waste acid is recycled that realizes, and the spent acid solution that the method can produce hydrolysis slurry be back in production technique, reduces the discharge of the spent acid of 80-90%.
For achieving the above object, the present invention adopts following technical scheme:
A method for turmeric saponin acidolysis spent acid reuse, comprises the following steps:
A. the slurries filtration after acidolysis in turmeric saponin industry is obtained to spent acid solution;
B. the turmeric saponin slurry obtaining after yellow ginger fragmentation is concentrated, make more than its solid content reaches 10wt%, spent acid solution directly fully to be mixed with turmeric saponin material more than solid content 10wt%;
C. then mixed slurry is adopted traditional acidolysis process to carry out acidolysis, realize the direct reuse of residual acid in spent acid solution.
In aforesaid method, described spent acid solution is to filter gained acid waste liquid after turmeric saponin acidolysis.In step a, described filter type is conventional filtration, as: plate-and-frame filter press filtration and belt filter press filtration etc.In step b, the slurry of the simmer down to of turmeric saponin slurry after to yellow ginger fragmentation utilizes plate-and-frame filter press concentrated.The mass ratio that spent acid solution mixes with more than solid content 10wt% turmeric saponin slurry is 1:1-20:1.
The concentrated of described turmeric saponin slurry comprises the steps:
The concentrated method of material before turmeric saponin acidolysis, comprises the following steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
B. in slurry, add a certain proportion of flocculating aids, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
The concentrated method of material before turmeric saponin acidolysis, comprises the following steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
A1. lower concentration turmeric saponin slurry is carried out to fermentative processing;
B. in slurry, add a certain proportion of flocculating aids, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
The concentrated method of material before turmeric saponin acidolysis, comprises the following steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
A2. robust fibre is mixed with lower concentration turmeric saponin slurry, obtain mixed slurry;
B. in mixed slurry, add a certain proportion of flocculating aids, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
The concentrated method of material before turmeric saponin acidolysis, comprises the following steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
A3. robust fibre is mixed with lower concentration turmeric saponin slurry, then carry out fermentative processing;
B. in mixed slurry, add a certain proportion of flocculating aids, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
In steps A 2, A3, the mass ratio of described robust fibre and lower concentration turmeric saponin slurry is 0.01:1~5:1, is preferably yellow ginger is cleaned to robust fibre and all mixing again of slurry that broken rear separation obtains.
The concentrated method of material before turmeric saponin acidolysis, comprises the following steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
A4-1. robust fibre is adopted to common process acidolysis, lower concentration turmeric saponin slurry is carried out to fermentative processing simultaneously;
A4-2. the complete robust fibre of acidolysis is filtered with plate-and-frame filter press, after filtration, filter cake is carried out to break process, make vegetalitas flocculating aids;
B. the vegetalitas flocculating aids and/or other flocculating aidss that in the slurry after fermentative processing, add above-mentioned gained, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
The concentrated method of material before turmeric saponin acidolysis, comprises the following steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
A5-1. robust fibre is adopted to common process acidolysis;
A5-2. the robust fibre after acidolysis is filtered with plate-and-frame filter press, after filtration, filter cake is carried out to break process, make vegetalitas flocculating aids;
B. the vegetalitas flocculating aids and/or other flocculating aidss that in lower concentration turmeric saponin slurry, add above-mentioned gained, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
In aforesaid method, described slurry can be the separated robust fibre slurry that do not ferment, and also can be separated robust fibre fermentation slurry; Can also, for mixing with robust fibre the slurry that do not ferment, also can be and robust fibre mixed fermentation slurry simultaneously.
In aforesaid method, described physical method for separation is that conventional mechanical is separated: as separated with whizzer etc. in belt filter press is separated, plate-and-frame filter press is separated.
In aforesaid method, described flocculating aids is for conventional flocculating aids, as vegetalitas flocculating aids, perlite and diatomite etc.Described vegetalitas flocculating aids is the robust fibre after hydrolyzate, lignin residue or acidolysis.Robust fibre after described acidolysis is that the robust fibre going out by physical method for separation after yellow ginger cleaning fragmentation filters the solid substance obtaining under sour environment after acidolysis; Described hydrolyzate is that in yellow ginger processing, slurry filters the solid substance obtain after by acidolysis; Described lignin residue is that hydrolyzate extracts the residue after saponin.
In aforesaid method, described flocculating aids and the mass ratio of slurry are 0.01:1~5:1.
In aforesaid method, plate-and-frame filter press is conventional plate-and-frame filter press.
In step c, described acidolysis process is in the acid hydrolysis solution that is 4-5wt% in acidity, and temperature is at 90-130 ℃, acidolysis 1-4 hour.Preferred temperature is 120 ℃ of left and right, acidolysis approximately 2 hours.
The present invention obtains spent acid solution after filtration by the slurry after acidolysis, then adds solid content to be not less than the Turmeric slurry of 10wt%, regulates acidity to processing requirement, by traditional technology requirement, carries out acidolysis.After the method can reclaim spent acid solution without any processing direct reuse in producing, reduce generation and the discharge of the acid waste liquid of 80-90%.
The invention provides a kind of concentration method of turmeric saponin material, can efficiently to Turmeric slurry, concentrate.The present invention has improved the solid content of turmeric saponin slurry, reduces the total amount of acidolysis, thereby reduces acid black liquor generation.The vegetalitas flocculating aids that the method is made the robust fibre that before turmeric saponin acidolysis, slurry interpolation yellow ginger self produces, utilizes plate-and-frame filter press to carry out filtering and concentrating, improves the solid content of acidolysis material.The method, guaranteeing, under the prerequisite that saponin does not lose, to have realized the efficient concentration of saponin in Turmeric slurry, reduces the generation of acid black liquor.
The invention provides the method for a kind of turmeric saponin acidolysis spent acid reuse, can significantly save sour consumption, significantly reduce the discharge of the spent acid solution of acidolysis generation, realize turmeric saponin wastewater qualified discharge on the basis of existing waste water treatment process.
Embodiment
Embodiment mono-
A. by the slurries filtration after acidolysis in turmeric saponin industry, obtain 5t spent acid solution;
B. turmeric saponin slurry 3t(3m will be obtained after yellow ginger fragmentation
3) and the robust fibre 1.2t of solid content 30wt%;
C. 1.2t robust fibre is made to the vegetalitas flocculating aids of 0.5t solid content 30wt% after by acidolysis, simultaneously by 3t turmeric saponin slurry fermentation 24h;
D. the above-mentioned vegetalitas flocculating aids making is all added in the 3t turmeric saponin slurry after fermentation, utilize plate-and-frame filter press concentrated, obtain the concentrate feed of 0.6t solid content 30wt%;
F. above-mentioned whole concentrate feed and 5t spent acid solution are mixed, and the sulfuric acid of supplementary 100kg98wt%, adopt traditional acidolysis process acidolysis, filter and obtain solid content 30wt% hydrolyzate 0.5t and spent acid solution 5t(5m
3).
Embodiment bis-
A. by the slurries filtration after acidolysis in turmeric saponin industry, obtain 5.1t spent acid solution;
B. the robust fibre 1.1t of turmeric saponin slurry 3t and solid content 30wt% will be obtained after yellow ginger fragmentation;
C. by the acidolysis of 1.1t robust fibre, make the vegetalitas flocculating aids of 0.5t solid content 30wt%;
D. the above-mentioned vegetalitas flocculating aids making is all added in unfermentable 3t turmeric saponin slurry, utilize plate-and-frame filter press concentrated, obtain the concentrate feed of 0.6t solid content 31wt%;
F. above-mentioned whole concentrate feed and 5.1t spent acid solution are mixed, and the sulfuric acid of supplementary 95kg98wt%, adopt traditional acidolysis process acidolysis, filter and obtain solid content 30wt% hydrolyzate 0.5t and spent acid solution 5.1t.
Embodiment tri-
A. by the slurries filtration after acidolysis in turmeric saponin industry, obtain 5.0t spent acid solution;
B. the robust fibre 1.1t of turmeric saponin slurry 3t and solid content 30wt% will be obtained after yellow ginger fragmentation;
C. by the acidolysis of 1.1t robust fibre, make the vegetalitas flocculating aids of 0.5t solid content 30wt%;
D. the above-mentioned vegetalitas flocculating aids making is all added in unfermentable 3t turmeric saponin slurry, and the hydrolyzate 0.1t of supplementary solid content 30wt%, utilize plate-and-frame filter press concentrated, obtain the concentrate feed of 0.7t solid content 30wt%;
F. above-mentioned whole concentrate feed and 5.0t spent acid solution are mixed, and the sulfuric acid of supplementary 100kg98wt%, adopt traditional acidolysis process acidolysis, filter and obtain solid content 30wt% hydrolyzate 0.6t and spent acid solution 5.1t.
Embodiment tetra-
A. by the slurries filtration after acidolysis in turmeric saponin industry, obtain 5.0t spent acid solution;
B. the robust fibre 1.1t of turmeric saponin slurry 3t and solid content 30wt% will be obtained after yellow ginger fragmentation;
C. by the acidolysis of 1.1t robust fibre, make the vegetalitas flocculating aids of 0.5t solid content 30wt%, simultaneously by 3t turmeric saponin slurry fermentation 24h;
D. the above-mentioned vegetalitas flocculating aids making is all added in unfermentable 3t turmeric saponin slurry, and the xylogen 0.2t of supplementary solid content 30wt%, utilize plate-and-frame filter press concentrated, obtain the concentrate feed of 0.8t solid content 30wt%;
F. above-mentioned whole concentrate feed and 5.0t spent acid solution are mixed, and the sulfuric acid of supplementary 100kg98wt%, adopt traditional acidolysis process acidolysis, filter and obtain solid content 30wt% hydrolyzate 0.7t and spent acid solution 5.0t.
After the present invention reclaims spent acid solution without any processing direct reuse in producing, reduce generation and the discharge of the acid waste liquid of 80-90%.
Claims (9)
1. a method for turmeric saponin acidolysis spent acid reuse, comprises the following steps:
A. the slurries filtration after hydrolysis in turmeric saponin industry is obtained to spent acid solution;
B. the turmeric saponin slurry obtaining after yellow ginger fragmentation is concentrated, the concentrated mode of turmeric saponin slurry is for utilizing plate-and-frame filter press concentrated to the slurry after yellow ginger fragmentation, make more than its solid content reaches 10wt%, spent acid solution directly fully to be mixed with turmeric saponin material more than solid content 10wt%;
C. then mixed slurry is adopted traditional acidolysis process to carry out acidolysis, realize the direct reuse of residual acid in spent acid solution.
2. the method for turmeric saponin acidolysis spent acid according to claim 1 reuse, is characterized in that: described filter type is for adopting plate-and-frame filter press to filter and belt filter press filtration.
3. the method for turmeric saponin acidolysis spent acid according to claim 1 reuse, is characterized in that: the concentrated of described turmeric saponin slurry comprises the steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
B. in slurry, add a certain proportion of flocculating aids, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
4. the method for turmeric saponin acidolysis spent acid according to claim 1 reuse, is characterized in that: the concentrated of described turmeric saponin slurry comprises the steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
A4-1. robust fibre is adopted to common process acidolysis, lower concentration turmeric saponin slurry is carried out to fermentative processing simultaneously;
A4-2. the robust fibre after acidolysis is filtered with plate-and-frame filter press, after filtration, filter cake is carried out to break process, make vegetalitas flocculating aids;
B. the vegetalitas flocculating aids and/or other flocculating aidss that in the slurry after fermentation, add above-mentioned gained, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
5. the method for turmeric saponin acidolysis spent acid according to claim 1 reuse, is characterized in that: the concentrated of described turmeric saponin slurry comprises the steps:
A. at yellow ginger, clean after fragmentation, by physical method for separation, obtain robust fibre and lower concentration turmeric saponin slurry;
A5-1. robust fibre is adopted to common process acidolysis;
A5-2. the robust fibre after acidolysis is filtered with plate-and-frame filter press, after filtration, filter cake is carried out to break process, make vegetalitas flocculating aids;
B. the vegetalitas flocculating aids and/or other flocculating aidss that in lower concentration turmeric saponin slurry, add above-mentioned gained, utilize plate-and-frame filter press to carry out filtering and concentrating, more than solid content is increased to 10wt%.
6. according to the method for the turmeric saponin acidolysis spent acid reuse described in any one in claim 3-5, it is characterized in that: described flocculating aids is vegetalitas flocculating aids, perlite and/or diatomite.
7. the method for turmeric saponin acidolysis spent acid according to claim 6 reuse, it is characterized in that: described vegetalitas flocculating aids is that yellow ginger cleans the robust fibre going out by physical method for separation after fragmentation and under sour environment, after acidolysis, filters the solid substance obtaining, or in yellow ginger processing, slurry filters the hydrolyzate or the hydrolyzate that obtain after by acidolysis and extracts the residue after saponin.
8. according to the method for the turmeric saponin acidolysis spent acid reuse described in any one in claim 3-5, it is characterized in that: described flocculating aids and the mass ratio of slurry are 0.01: 1~5: 1.
9. the method for turmeric saponin acidolysis spent acid according to claim 1 reuse, is characterized in that: described acidolysis process is in the acid hydrolysis solution that is 4-5wt% in acidity, and temperature is at 90-130 ℃, acidolysis 1-4 hour.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101544438A (en) * | 2009-04-17 | 2009-09-30 | 北京盖雅技术中心有限公司 | Method for reusing yellow-ginger saponin industrial waste acid solution |
CN101580531A (en) * | 2009-06-05 | 2009-11-18 | 汪琳博 | Production technology for yam diosgenin |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
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EP2282752A4 (en) * | 2008-03-26 | 2011-06-15 | Ca Nat Research Council | Saponin extract from saponaria spp and uses thereof |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101544438A (en) * | 2009-04-17 | 2009-09-30 | 北京盖雅技术中心有限公司 | Method for reusing yellow-ginger saponin industrial waste acid solution |
CN101580531A (en) * | 2009-06-05 | 2009-11-18 | 汪琳博 | Production technology for yam diosgenin |
Non-Patent Citations (2)
Title |
---|
李美秀等.酸2菌2酶法处理黄姜皂素生产废渣的工艺.《西北农业学报》.2010,第19卷(第7期), |
酸2菌2酶法处理黄姜皂素生产废渣的工艺;李美秀等;《西北农业学报》;20100730;第19卷(第7期);196-201 * |
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