CN101870849A - New method for producing tanning extracts by ultrasonic-enhanced extraction of castanea mollissima bud - Google Patents
New method for producing tanning extracts by ultrasonic-enhanced extraction of castanea mollissima bud Download PDFInfo
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- CN101870849A CN101870849A CN200910082293A CN200910082293A CN101870849A CN 101870849 A CN101870849 A CN 101870849A CN 200910082293 A CN200910082293 A CN 200910082293A CN 200910082293 A CN200910082293 A CN 200910082293A CN 101870849 A CN101870849 A CN 101870849A
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Abstract
The invention relates to a new method for producing tanning extracts by ultrasonic-enhanced extraction of castanea mollissima bud. The method comprises the following steps: drying, crushing and sieving the collected castanea mollissima bud raw material; taking organic solvent water as an extraction solvent; performing ultrasonic-enhanced extraction, liquid-solid separation, concentrating, drying and crushing to obtain rough tanning extracts product; redissolving the obtained rough tanning extracts product in water to remove the insoluble substance; or directly precipitating the extract with saturated metal ion precipitant, adding water into the precipitate, mixing the water and the precipitate to obtain suspension and introducing an acidic gas into the mixture to redissolve the suspension to remove the insoluble substance; and concentrating and drying the supernatant to obtain the fine tanning extracts product. Compared with a conventional method, the extraction temperature can be reduced to room temperature, the extraction time can be greatly shortened, the yield of the tanning extracts is high, and the tanning extracts products with different tannin content can be prepared; and therefore, a new method is provided for the high-valued utilization of agricultural and forestry waste-tanning extracts bud resources.
Description
Technical field
The present invention relates to the novel method that a kind of ultrasound-enhanced extraction Chinese chestnut bud is produced tannin extract, belong to the biochemical engineering technical field.
Background technology
Chinese chestnut (Castaneamo Uissima Blume) is the perennial deciduous tree of a kind of Fagaceae Castanea, and China's Chinese chestnut aboundresources all has cultivation except that minority areas such as Heilongjiang Province, the north, Xinjiang.Unprecedented soaring along with China's Chinese chestnut output, the output of the waste during Chinese chestnut produces---Chinese chestnut bud (Involucrum Castaneae, chestnut thorn shell) also increases by Chinese chestnut bud a large amount of discarded the caused wasting of resources and environmental pollutions on a year-on-year basis.
Tannin extract be by the plant material that is rich in tannin through lixiviate with step such as concentrate and be processed into, be generally pale brown look to tan powdery or bulk.The composition of tannin extract also has non-tannis and insolubles except that the main component tannin.Tannin is divided into hydrolysis again and beats tannin and condensed tannin.From plant material, obtain through refining various vegatable tannin products, except that being used for tanning, preparation (the Sun Dawang that also is widely used in carpenter's glue stick, cement water reducing agent, petroleum drilling fluid viscosity-depression agent, pharmacy, ore dressing, water treatment, gas sweetening, anti-corrosion of metal, wood preservation, printing and dyeing, drinks clarification, lipid-antioxidant activity, daily chemicals and other multiple product, the tannin extract process technology, Beijing: the 1997:1-10. of China Forest press).The raw material of present industrial production tannin extract mainly contains black wattle plant, tamarack, acorn cup, hard wood etc., but their resource distributions and output are limited, have in addition want the harvest of forest trees resource.
Research has been found that in the Chinese chestnut bud is rich in tannin, can be used as the raw material that extracts tannin extract.People such as Yang Zhibin adopt five jar of nine step normal pressure adverse current method to carry out lixiviate, with water as vat liquor, 80 ℃ of extraction temperatures, every jar of extraction time is that 1.5h carries out lixiviate, and extracting the product tannin content only is 40%, and pH is 4.3, total colour 62.4 (red 23.7, yellow 35.3, blue 3.4) (Yang Zhibin, the loyal spring of guilt, willow, Lei Xiao, Cheng Li. the preliminary study [J] that tannin extract extracts in the Chinese chestnut bud. the Hubei forestry science and technology, 2006, (3): 34-36).Tan Wenying etc. have contrasted ethanol, water, acetone etc. and have made solvent lixiviate chestnut shell tannin extract, and experimental result shows: extract tannin content 51-63%, total colour 43-47 (red 20.2-22.1, yellow 20-22.2, blue 3.1-3.4), pH is 3.9-4.5, draws optimum process to be: adopt 30% ethanol, 95 ℃, extraction time 6h (Tan Wenying, Fang Guizhen, the extraction process of tannin extract in the chestnut shell, Northeast Forestry University's journal, 2006,34 (2): 60-61).Obviously, existing extracting method and technology can't reach the product standard (valonex standard LY/1091-93) of tannin extract, and extraction time is long, extraction temperature is high, the pH of product and colour are higher, and is bigger to the destruction of tannin.
Patent application " process for extracting vegetable tannin extract from Pterocarya stenoptera samara " (application number 93119018.5) is that the pulverizing of acer truncatum samara shell, 45-50 ℃ slaking 1 hour, circulation diafiltration lixiviate, vacuum concentration, spraying drying are obtained tannin extract, though mentioned the ultrasonic generator that extracted equipment configuration at specification sheets, but how not realize supersound extraction, do not extract the analytical study result of product, to the no reference of Chinese chestnut bud tannin extract preparation yet.
The present invention is a raw material with agriculture and forestry organic waste material-Chinese chestnut bud, adopt ultrasound-enhanced extraction solved extraction time long, extract the temperature height, problem such as the extract tannin content is low and colour and pH value be higher.Simultaneously, set up the tannin purification process, can satisfy the requirement of product different tannin contents.Therefore, the present invention has important economic value and social effect for the higher value application that increases tannin extract production cheap raw material, Chinese chestnut bud resource provides the method with actual application value.
Goal of the invention and content
The present invention seeks to the problem that preparation exists at Chinese chestnut bud tannin extract, the novel method that provides a kind of ultrasound-enhanced extraction Chinese chestnut bud to produce tannin extract, adopt agriculture and forestry organic waste material-Chinese chestnut bud to carry out problems such as tannin extract production process extraction time is long, temperature is high, the extract tannin content is low, colour height to solve, realize quick, the less energy-consumption production of Chinese chestnut bud tannin extract product, reduce production costs, satisfy the requirement of the different tannin contents of tannin extract product.The present invention mainly may further comprise the steps:
(1) raw material is handled: the Chinese chestnut bud is dry, be crushed to the 10-120 order;
(2) supersound extraction: solid-liquid is than pressing kilogram: be upgraded to 1: 5-1: 50, organic solvent (one or more in ethanol, acetone, tetrahydrofuran (THF), the methyl alcohol)-aqueous solution that raw material that adding is handled well in supersound extraction equipment and mass content are 10%-80% is at ultrasonic power 5-600W/cm
2, extract under 10-60 ℃ of condition of temperature, extracted 10-60 minute at every turn, to extract 1-3 time, liquid-solid separation (in centrifugal, press filtration or the vacuum filtration a kind of) obtains the tannin extract extracting solution;
(3) thick tannin extract preparation: united extraction liquid, concentrate, dry, pulverize and can obtain thick tannin extract product;
(4) tannin extract is refining: the tannin extract crude product that step (3) is obtained compares by kilogram at solid-liquid: be upgraded to 1: 3-1: adding water under 10 conditions dissolves again, remove the tannin extract liquid that undissolved residue obtains, or the tannin extract extracting solution that step (2) is obtained, at tannin extract liquid: saturated precipitation by metallic ion agent (one or more in cupric chloride, neutralized verdigris, the plumbic acetate) solution is by rising: be upgraded to 1: 0.01-1: precipitate liquid-solid separation (in centrifugal, press filtration or the vacuum filtration a kind of) collecting precipitation under 1 condition; Precipitating: water is pressed kilogram: be upgraded to 1: 2-1: add distilled water under 30 conditions, through mixing the formation suspension liquid; Feed sour gas (hydrogen sulfide or sulfurous gas) to suspension liquid and make its redissolution, supernatant liquor is collected in liquid-solid separation (in centrifugal, press filtration or the vacuum filtration a kind of); The supernatant liquor that obtains can be obtained refining tannin extract product through concentrated, drying.
Embodiment:
Embodiment only is part embodiment of the present invention; but protection scope of the present invention is not limited thereto; any those skilled in the art that are in the technical scope that the present invention discloses, and the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Embodiment 1
40 gram dryings, pulverizing, the Chinese chestnut bud of crossing 10 mesh sieves and 2000 milliliter of 40% ethanol-water solution are added ultrasonic extraction device, and 30 ℃ were extracted power 600W/cm 30 minutes
2, vacuum filtration gets the tannin extract extracting solution, and concentrate drying obtains tannin content 60%, pH=4.0, tannin extract 7.8 grams of total colour 28.5 (wherein red 9, yellow 19, blue 0.5).
Embodiment 2
40 gram dryings, pulverizing, the Chinese chestnut bud of crossing 120 mesh sieves and 200 milliliter of 80% methanol-water solution are added ultrasonic extraction device, and 60 ℃ were extracted power 200W/cm 10 minutes
2, centrifugation gets the tannin extract extracting solution, and residue adds 80% methanol-water solution again and repeats to extract 2 times by aforementioned condition, merge 3 times filtrate, concentrate drying obtains tannin content 55%, pH=3.7, tannin extract 8.4 grams of total colour 26.4 (wherein red 10, yellow 15.4, blue 1).
Embodiment 3
40 gram dryings, pulverizing, the Chinese chestnut bud of crossing 80 mesh sieves and 1200 milliliter of 10% acetone+30% tetrahydrofuran (THF)-aqueous solution are added ultrasonic extraction device, and 10 ℃ are extracted power 5W/cm 60 minutes 1 time
2, press filtration separate the tannin extract extracting solution, residue adds 10% acetone+30% tetrahydrofuran (THF)-aqueous solution again and repeats to extract once by aforementioned condition, merge filtrate twice, concentrate drying obtains tannin content 65%, pH=3.6, tannin extract 7.2 grams of total colour 27.1 (wherein red 11.1, yellow 16).
Embodiment 4
The tannin extract 8 that embodiment 2 is obtained restrains, adding 24 ml waters dissolves again, undissolved residue is removed in vacuum filtration, by clear liquid: the saturated acetic acid lead solution is that 1: 1 (rising: rise) precipitated, centrifugation, by precipitating: water is that 1: 1 (kilogram: rise) adds distilled water, mix the formation suspension liquid, feed hydrogen sulfide and make its redissolution, undissolved residue is removed in vacuum filtration, and supernatant liquor is obtained tannin content 75%, pH=4.1 through concentrated, drying, the tannin extract 5.7 gram tannin extract products of total colour 28 (wherein red 12, yellow 16).
Embodiment 5
Obtain the tannin extract extracting solution by embodiment 3, by the tannin extract extracting solution: saturated Cupric Chloride Solution is that 1: 0.01 (rising: rise) precipitated, centrifugation, by precipitating: water is that 1: 30 (kilogram: rise) adds distilled water, mixes the formation suspension liquid, feed sulfurous gas and make its redissolution, undissolved residue is removed in vacuum filtration, and supernatant liquor is obtained tannin content 90%, pH=4.0 through concentrated, drying, the tannin extract 4.8 gram tannin extract products of total colour 30 (wherein red 13, yellow 17).
Embodiment 6
The tannin extract 4 that embodiment 1 is obtained restrains, adding 40 ml waters dissolves again, undissolved residue is removed in vacuum filtration, by clear liquid: the saturated acetic acid copper solutions is that 1: 0.1 (rising: rise) precipitated, centrifugation, by precipitating: water is that 1: 15 (kilogram: rise) adds distilled water, mix the formation suspension liquid, feed hydrogen sulfide and make its redissolution, undissolved residue is removed in vacuum filtration, and supernatant liquor is obtained tannin content 85%, pH=3.8 through concentrated, drying, the refining tannin extract product of tannin extract 2.6 grams of total colour 27 (wherein red 12, yellow 15).
Claims (5)
1. novel method that ultrasound-enhanced extraction Chinese chestnut bud is produced tannin extract is characterized in that: may further comprise the steps:
(1) raw material is handled: the Chinese chestnut bud is dry, be crushed to the 10-120 order;
(2) supersound extraction: solid-liquid is than pressing kilogram: be upgraded to 1: 5-1: 50, and adding raw material and the mass content handled well in supersound extraction equipment is organic solvent-aqueous solution of 10%-80%, at ultrasonic power 5-600W/cm
2, extract under 10-60 ℃ of condition of temperature, extracted 10-60 minute at every turn, to extract 1-3 time, liquid-solid separation obtains the tannin extract extracting solution;
(3) thick tannin extract preparation: united extraction liquid, concentrate, dry, pulverize and can obtain thick tannin extract product;
(4) tannin extract is refining: the tannin extract crude product that step (3) is obtained compares by kilogram at solid-liquid: be upgraded to 1: 3-1: adding water under 10 conditions dissolves again, remove the tannin extract liquid that undissolved residue obtains, or the tannin extract extracting solution that step (2) is obtained, at tannin extract liquid: saturated precipitation by metallic ion agent solution is by rising: be upgraded to 1: 0.01-1: precipitate liquid-solid separated and collected precipitation under 1 condition; Precipitating: water is pressed kilogram: be upgraded to 1: 2-1: add distilled water under 30 conditions, through mixing the formation suspension liquid; Feed sour gas to suspension liquid and make its redissolution, liquid-solid separated and collected supernatant liquor; The supernatant liquor that obtains can be obtained refining tannin extract product through concentrated, drying.
2. according to the novel method of the described a kind of ultrasound-enhanced extraction Chinese chestnut bud production tannin extract of claim 1, it is characterized in that: the described organic solvent of step (2) is one or more in ethanol, acetone, tetrahydrofuran (THF), the methyl alcohol.
3. the novel method of producing tannin extract according to the described a kind of ultrasound-enhanced extraction Chinese chestnut bud of claim 1 is characterized in that: described liquid-solid a kind of in centrifugal, press filtration or the vacuum filtration of being separated into of step (2) or step (4).
4. according to the novel method of the described a kind of ultrasound-enhanced extraction Chinese chestnut bud production tannin extract of claim 1, it is characterized in that: the described saturated precipitation by metallic ion agent of step (4) is one or more in cupric chloride, neutralized verdigris, the plumbic acetate.
5. according to the novel method of the described a kind of ultrasound-enhanced extraction Chinese chestnut bud production tannin extract of claim 1, it is characterized in that: the described sour gas of step (4) is hydrogen sulfide or sulfurous gas.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140123A (en) * | 2011-03-02 | 2011-08-03 | 北京农学院 | Method for extracting ellagic acid tannin from chestnut bur |
| CN102643310A (en) * | 2012-03-27 | 2012-08-22 | 中国林业科学研究院林产化学工业研究所 | Method for extracting chestnut shell tannin through microwave composite technique |
| CN103610212A (en) * | 2013-12-05 | 2014-03-05 | 北京农学院 | Application of castanea mollissima blume ellagitannin in preparing antioxidant |
| CN104910813A (en) * | 2015-04-27 | 2015-09-16 | 崇夕山 | Refined oil tea fruit shell tannin extract preparation method |
| CN105778017A (en) * | 2016-03-09 | 2016-07-20 | 河南工程学院 | Preparation method of building concrete water reducing agent |
| CN105800986A (en) * | 2016-03-09 | 2016-07-27 | 河南工程学院 | Method for preparing concrete water reducing agent |
| CN107488413A (en) * | 2017-08-24 | 2017-12-19 | 成都圻坊生物科技有限公司 | The extracting method of tannin extract in a kind of granatum |
| CN112029415A (en) * | 2020-08-28 | 2020-12-04 | 广西灵水林化有限公司 | Method for extracting acacia melanoxylon tannin extract by ultrasonic-assisted biological enzyme method |
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| GB190713879A (en) * | 1907-06-15 | 1908-02-20 | Plato Leonidas Aslanoglou | An Improved Preparation for use in Tanning. |
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| GB190713879A (en) * | 1907-06-15 | 1908-02-20 | Plato Leonidas Aslanoglou | An Improved Preparation for use in Tanning. |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140123A (en) * | 2011-03-02 | 2011-08-03 | 北京农学院 | Method for extracting ellagic acid tannin from chestnut bur |
| CN102643310A (en) * | 2012-03-27 | 2012-08-22 | 中国林业科学研究院林产化学工业研究所 | Method for extracting chestnut shell tannin through microwave composite technique |
| CN103610212A (en) * | 2013-12-05 | 2014-03-05 | 北京农学院 | Application of castanea mollissima blume ellagitannin in preparing antioxidant |
| CN103610212B (en) * | 2013-12-05 | 2015-06-17 | 北京农学院 | Application of castanea mollissima blume ellagitannin in preparing antioxidant |
| CN104910813A (en) * | 2015-04-27 | 2015-09-16 | 崇夕山 | Refined oil tea fruit shell tannin extract preparation method |
| CN105778017A (en) * | 2016-03-09 | 2016-07-20 | 河南工程学院 | Preparation method of building concrete water reducing agent |
| CN105800986A (en) * | 2016-03-09 | 2016-07-27 | 河南工程学院 | Method for preparing concrete water reducing agent |
| CN105800986B (en) * | 2016-03-09 | 2017-11-17 | 河南工程学院 | A kind of preparation method of cement water reducing agent |
| CN105778017B (en) * | 2016-03-09 | 2018-07-13 | 河南工程学院 | A kind of preparation method of building concrete water-reducing agent |
| CN107488413A (en) * | 2017-08-24 | 2017-12-19 | 成都圻坊生物科技有限公司 | The extracting method of tannin extract in a kind of granatum |
| CN112029415A (en) * | 2020-08-28 | 2020-12-04 | 广西灵水林化有限公司 | Method for extracting acacia melanoxylon tannin extract by ultrasonic-assisted biological enzyme method |
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