CN102219810B - Process method for preparing high-purity tannin from walnut green husk - Google Patents
Process method for preparing high-purity tannin from walnut green husk Download PDFInfo
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- CN102219810B CN102219810B CN201110115511.4A CN201110115511A CN102219810B CN 102219810 B CN102219810 B CN 102219810B CN 201110115511 A CN201110115511 A CN 201110115511A CN 102219810 B CN102219810 B CN 102219810B
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- weibull
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- 235000009496 Juglans regia Nutrition 0.000 title claims abstract description 26
- 235000020234 walnut Nutrition 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229920001864 tannin Polymers 0.000 title abstract description 18
- 235000018553 tannin Nutrition 0.000 title abstract description 18
- 239000001648 tannin Substances 0.000 title abstract description 18
- 230000008569 process Effects 0.000 title abstract description 6
- 239000010903 husk Substances 0.000 title abstract 4
- 240000007049 Juglans regia Species 0.000 title 1
- 238000000605 extraction Methods 0.000 claims abstract description 34
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 26
- 241000758789 Juglans Species 0.000 claims abstract description 25
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims description 27
- 238000003672 processing method Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 9
- 230000008719 thickening Effects 0.000 claims description 8
- 230000006837 decompression Effects 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000002137 ultrasound extraction Methods 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 229920006351 engineering plastic Polymers 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 15
- 238000001728 nano-filtration Methods 0.000 abstract description 14
- 238000000926 separation method Methods 0.000 abstract description 14
- 238000000746 purification Methods 0.000 abstract description 4
- 241000196324 Embryophyta Species 0.000 abstract description 2
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides a process method for preparing high-purity tannin from walnut green husk and relates to the technical field of pharmaceutical chemical engineering, and the method is designed for solving the technical problems that the extraction efficiency is low, the extraction temperature is high, effective components are easy to destroy and the like in the traditional separation and extraction method of plant tannin. The process method for preparing high-purity tannin from the walnut green husk comprises the following process flows: smashing the walnut green husk and then breaking walls with ultrasonic wave for extraction; carrying out solid-liquid separation, and then carrying out grading separation and purification by virtue of a molecular ultrafiltration membrane; and concentrating through a nanofiltration membrane, carrying out extrinsic cycle concentration at reduced pressure, and drying through microwave, so as to respectively obtain products of two specifications and applications, namely, industry-grade tannin (85%) and medicine-grade tannin (95%).
Description
Technical field
The present invention relates to pharmaceutical chemistry technical field, particularly a kind of processing method of preparing high-purity tannin from green peel of walnut.
Background technology
The extraction and separation method of vegatable tannin acid is varied.Classical extracting method has warm water decocting method, supercritical CO
2extraction process, organic solvent extraction method etc.
Water extraction method extraction efficiency is generally not high, and overheated meeting destruction effective constituent, and the composition of Polysaccharide-Rich filters also difficulty.
Supercritical fluid extraction sepn process is to utilize the dissolving power of supercutical fluid and the relation of density, utilizes pressure and temperature to carry out the impact of supercutical fluid dissolving power.When gas is during in supercritical state, become the single phase of character between liquids and gases, there is the density close with liquid, though viscosity is starkly lower than liquid higher than gas, spread coefficient is liquid 10-100 times; Therefore material is had to good perviousness and stronger dissolving power, some composition of herbal medicine can be extracted.Jiang Ping etc. have studied supercritical CO from Turkey-galls raw material
2the method of extraction Weibull [Jiang Ping, Huang Juan, Li Chunfu. supercritical CO
2the research [J] of extraction Weibull. forest chemical engineering communication, 2005,39(6): 17-19.], by each factor of impact extraction is drawn to optimum supercritical CO
2extraction conditions is: 44 ℃ of extraction temperature, and pressure 25MPa, entrainment agent are ethyl acetate, extraction time 120min, its yield is 57.8%.
Summary of the invention
The present invention be intended to solve in the extraction and separation method of traditional plant Weibull, exist extraction efficiency low, extract that temperature is high, the easy technical problem such as destroyed of effective constituent, to provide, there is the processing method of preparing high-purity tannin from green peel of walnut that extraction efficiency is high, extract the advantages such as temperature is low, reliable and stable.
The object of the invention is to be achieved through the following technical solutions.
The processing method of preparing high-purity tannin from green peel of walnut of the present invention, comprises the steps:
A) green peel of walnut is pulverized for 10-20 order, 1:4-12 adds water and is uniformly mixed in mass ratio;
B) aforementioned mixture is imported to extraction in ultrasonic extraction equipment, ultrasonic frequency 20～80Hz, extracts 35 ℃～40 ℃ of temperature, 60～80 minutes extraction times, afterwards separating filtrate and residue;
C) after filtrate coarse filtration step b being obtained, carry out ultrafiltration, ultra-filtration membrane molecular weight is 60000～2000;
D) filtrate that adopts the nanometer film concentration of molecular weight below 100 to obtain through ultrafiltration, during concentration, controlling temperature is 10～30 ℃, after concentrating, is 1:5～10 with concentrated front filtrate volume ratio, nanometer film inlet and outlet pressure is poor is 0.3-0.5MPa;
E) adopt decompression outer circulation to do the filtrate after concentrated further concentrated, 60 ℃～65 ℃ of thickening temperatures, are concentrated into that filtrate ratio weighs 1.17～1.20, dissolved solids content > 50%;
F) after being carried out to microwave vacuum drying, the filtrate after step e is concentrated can obtain finished product.
The processing method of preparing high-purity tannin from green peel of walnut of the present invention, the coarse filtration in wherein said step c is specially first uses 100 order stainless (steel) wires to carry out coarse filtration to the filtrate obtaining through step b, then by the filtrate 2m obtaining
3flame filter press filter.
The processing method of preparing high-purity tannin from green peel of walnut of the present invention, the ultrafiltration of wherein said step c is one-level or two-stage ultrafiltering; When adopting two-stage ultrafiltering, first step ultra-filtration membrane molecular weight cut-off is 30000-60000, and its inlet and outlet pressure is poor is 0.2-0.4Mpa, and second stage ultra-filtration membrane molecular weight cut-off is 2000-4000.
The processing method of preparing high-purity tannin from green peel of walnut of the present invention, the ultra-filtration membrane in wherein said step c is tubular type or rolled film, material is tubular fibre or engineering plastics or pottery.
The processing method of preparing high-purity tannin from green peel of walnut of the present invention, when concentrated in wherein said step e, vacuum tightness is 0.07-0.09Pa.
The processing method of preparing high-purity tannin from green peel of walnut of the present invention, in wherein said step f, microwave drying frequency is 2200～3200MHz, and the time is 20～180 minutes, and temperature is 30 ℃～40 ℃, and vacuum tightness is 0.08～0.09MPa.
The present invention prepares the beneficial effect of the processing method of high-purity tannin from green peel of walnut:
1. extract temperature low, avoid the detrimentally affect of long-time heating to Weibull in conventional decocting method and circumfluence method, product biological activity is high;
2. ultrasonic wave also has certain germicidal action, can guarantee that extracting solution is not perishable, and has increased substantially the extraction yield of Weibull;
3. the macromolecule membrane of the natural or synthetic of the refining employing of Weibull, take outside energy or chemical potential difference is impellent, multi-component solute and solvent is carried out separated, has effectively realized the stock grading of different molecular weight and has held back, fine work Weibull content is up to 97.5%, and yield is 95.6%;
4. ultrasonic extraction and membrane separation technique are respectively used to extraction and the purifying of Weibull, can improve yield and the purity of Weibull;
5. adopt microwave to be dried following feature to material: efficient, energy-conservation, stable, reliable, be particularly useful for the high responsive Weibull of heat dry.
Embodiment
The present invention is a kind of processing method of preparing high-purity tannin from green peel of walnut, its technical process is: after green peel of walnut is pulverized, with supersonic wave wall breaking, extract, solid-liquid separation, molecule ultra-filtration membrane fractional separation purifying, then nanofiltration membrane is concentrated, decompression outer circulation is concentrated, and microwave drying can obtain respectively the product of (95%) two specification of technical grade Weibull (85%) and medicine and Weibull and purposes.
Application principle of the present invention, is further described by following embodiment.
Embodiment mono-
Get 100 kilograms of green peel of walnut (Weibull content 27.65%), be ground into 10 orders, add 1000 kilograms, water, enter together in tubular ultrasonic ripple counterflow extraction apparatus, ultrasonic frequency 25Hz, 80 minutes extraction times.Residue after extraction is discharged from slag notch, and extracting solution injects storage tank from liquid discharge pipe, with 100 order stainless (steel) wires, carries out coarse filtration, obtains filtrate, and extraction yield is 94.5%.Filtrate is being used flame filter press (2m
3) filter, filtrate is imported to ultrafiltration system, the ultra-filtration membrane molecular weight cut-off of selecting is 50000, regulate the pressure difference of import and outlet to 0.3MPa, primary ultrafiltration is poured two-stage ultrafiltering film into through liquid and is carried out separation, and molecular weight cut-off is 3000, again carries out separation and purification.Ultrafiltration sees through liquid importing nanofiltration system and carries out nanofiltration, and nanofiltration membrane molecular weight cut-off is 100, regulates the poor most 0.4MPa of inlet and outlet pressure, concentrated ratio 5:1.Nanofiltration trapped fluid is transferred in decompression outer circulation thickening equipment, concentrates, and thickening temperature is 60 ℃, vacuum tightness 0.08pa, and concentrated solution ratio weighs 1.17.The concentrated microwave vacuum drying, 40 ℃ of drying temperatures, vacuum tightness 0.08Pa of carrying out.Pulverize, pack, obtain Weibull (pharmaceutical grade) 20.2kg, purity 98.2%.
Embodiment bis-
Get 100 kilograms of green peel of walnut (Weibull content 27.65%), be ground into 20 orders, add 1000 kilograms, water, enter together in tubular ultrasonic ripple counterflow extraction apparatus, ultrasonic frequency 30Hz, 80 minutes extraction times.Residue after extraction is discharged from slag notch, and extracting solution injects storage tank from liquid discharge pipe, with 80 order stainless (steel) wires, carries out coarse filtration, obtains filtrate, and extraction yield is 94.7%.Filtrate is being used flame filter press (2m
3) filter, filtrate is imported to ultrafiltration system, the ultra-filtration membrane molecular weight cut-off of selecting is 50000, regulate the pressure difference of import and outlet to 0.3MPa, primary ultrafiltration is poured two-stage ultrafiltering film into through liquid and is carried out separation, and molecular weight cut-off is 3000, again carries out separation and purification.Ultrafiltration sees through liquid importing nanofiltration system and carries out nanofiltration, and nanofiltration membrane molecular weight cut-off is 100, regulates the poor most 0.4MPa of inlet and outlet pressure, concentrated ratio 8:1.Nanofiltration trapped fluid is transferred in decompression outer circulation thickening equipment, concentrates, and thickening temperature is 63 ℃, vacuum tightness 0.08pa, and concentrated solution ratio weighs 1.19.The concentrated microwave vacuum drying, 40 ℃ of drying temperatures, vacuum tightness 0.08Pa of carrying out.Pulverize, pack, obtain Weibull (pharmaceutical grade) 21.3kg, purity 95.2%.
Embodiment tri-
Get 100 kilograms of green peel of walnut (Weibull content 27.65%), be ground into 10 orders, add 1000 kilograms, water, enter together in tubular ultrasonic ripple counterflow extraction apparatus, ultrasonic frequency 25Hz, 60 minutes extraction times.Residue after extraction is discharged from slag notch, and extracting solution injects storage tank from liquid discharge pipe, with 100 order stainless (steel) wires, carries out coarse filtration, obtains filtrate, and extraction yield is 94.5%.Filtrate is being used flame filter press (2m
3) filter, filtrate is imported to ultrafiltration system, the ultra-filtration membrane molecular weight cut-off of selecting is 50000, regulate the pressure difference of import and outlet to 0.3MPa, primary ultrafiltration is poured two-stage ultrafiltering film into through liquid and is carried out separation, and molecular weight cut-off is 3000, again carries out separation and purification.Ultrafiltration sees through liquid importing nanofiltration system and carries out nanofiltration, and nanofiltration membrane molecular weight cut-off is 100, regulates the poor most 0.4MPa of inlet and outlet pressure, concentrated ratio 5:1.Nanofiltration trapped fluid is transferred in decompression outer circulation thickening equipment, concentrates, and thickening temperature is 60 ℃, vacuum tightness 0.08pa, and concentrated solution ratio weighs 1.17.The concentrated microwave vacuum drying, 40 ℃ of drying temperatures, vacuum tightness 0.08Pa of carrying out.Pulverize, pack, obtain Weibull (technical grade) 28.5kg, purity 85.2%.
Claims (5)
1. from green peel of walnut, prepare the processing method of Weibull, it is characterized in that this technique comprises the steps:
A) green peel of walnut is pulverized for 10-20 order, 1:4-12 adds water and is uniformly mixed in mass ratio;
B) aforementioned mixture is imported to extraction in ultrasonic extraction equipment, ultrasonic frequency 20～80Hz, extracts 35 ℃～40 ℃ of temperature, 60～80 minutes extraction times, afterwards separating filtrate and residue;
C) after filtrate coarse filtration step b being obtained, carry out two-stage ultrafiltration, first step ultra-filtration membrane molecular weight cut-off is 30000-60000, and its inlet and outlet pressure is poor is 0.2-0.4Mpa, and second stage ultra-filtration membrane molecular weight cut-off is 2000-4000;
D) filtrate that adopts the nanometer film concentration of molecular weight below 100 to obtain through ultrafiltration, during concentration, controlling temperature is 10～30 ℃, after concentrating, is 1:5～10 with concentrated front filtrate volume ratio, nanometer film inlet and outlet pressure is poor is 0.3-0.5MPa;
E) adopt decompression outer circulation to do the filtrate after concentrated further concentrated, 60 ℃～65 ℃ of thickening temperatures, are concentrated into that filtrate ratio weighs 1.17～1.20, dissolved solids content > 50%;
F) after being carried out to microwave vacuum drying, the filtrate after step e is concentrated can obtain finished product.
2. the processing method of preparing Weibull from green peel of walnut as claimed in claim 1, is characterized in that: the coarse filtration in described step c is specially first uses 100 order stainless (steel) wires to carry out coarse filtration to the filtrate obtaining through step b, then by the filtrate 2m obtaining
3flame filter press filter.
3. the processing method of preparing Weibull from green peel of walnut as claimed in claim 1, is characterized in that: the ultra-filtration membrane in described step c is tubular type or rolled film, and material is tubular fibre or engineering plastics or pottery.
4. the processing method of preparing Weibull from green peel of walnut as claimed in claim 1, is characterized in that: when concentrated in described step e, vacuum tightness is 0.07-0.09Pa.
5. the processing method of preparing Weibull from green peel of walnut as claimed in claim 1, it is characterized in that: in described step f, microwave drying frequency is 2200～3200MHz, time is 20～180 minutes, and temperature is 30 ℃～40 ℃, and vacuum tightness is 0.08～0.09MPa.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617653A (en) * | 2012-02-21 | 2012-08-01 | 安徽农业大学 | Extraction and purification method of carya cathayensis shell polyphenol |
| CN102887924A (en) * | 2012-10-24 | 2013-01-23 | 天津科技大学 | Preparation of active components for tyrosinase inhibition from agricultural and forestry waste walnut shell and application of active components |
| CN103360435B (en) * | 2013-06-09 | 2016-09-07 | 陕西师范大学 | A kind of response phase method optimizes the extraction process of tannin in dogwood kernel |
| CN103524571B (en) * | 2013-10-08 | 2016-03-02 | 河北科技大学 | Walnut slag reclaims the method preparing Weibull |
| CN104055838B (en) * | 2014-07-15 | 2017-12-01 | 新疆农业大学 | A kind of extracting method of green peel of walnut polyphenol |
| CN105816518B (en) * | 2016-04-29 | 2020-02-07 | 华南农业大学 | Walnut green seedcase phenol natural antioxidant and preparation method and application thereof |
| CN106319492A (en) * | 2016-11-02 | 2017-01-11 | 常州市鼎日环保科技有限公司 | Preparation method of surface complexation film coated FeCuNbSiB strip |
| CN108976266A (en) * | 2017-06-05 | 2018-12-11 | 喀什龙盛生物科技有限公司 | Tannin processing technology is extracted in a kind of green peel of walnut |
| CN110074267A (en) * | 2019-05-21 | 2019-08-02 | 兰州大学 | A kind of feed formula and its application method improving sheep quality of mutton |
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| CN101838294A (en) * | 2010-04-07 | 2010-09-22 | 云南瑞宝生物科技有限公司 | Method for preparing high-purity Tara tannic acid |
| CN101993460A (en) * | 2010-12-02 | 2011-03-30 | 南宁圣特生物科技有限公司 | Method for separating and purifying ellagitannic acid in raspberry |
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