CN102276849A - Method for extracting gutta-percha from folium cortex eucommiae - Google Patents
Method for extracting gutta-percha from folium cortex eucommiae Download PDFInfo
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- CN102276849A CN102276849A CN2011101059672A CN201110105967A CN102276849A CN 102276849 A CN102276849 A CN 102276849A CN 2011101059672 A CN2011101059672 A CN 2011101059672A CN 201110105967 A CN201110105967 A CN 201110105967A CN 102276849 A CN102276849 A CN 102276849A
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Abstract
The invention relates to a method for extracting gutta-percha from folium cortex eucommiae, in particular to a method for extracting gutta-percha from folium cortex eucommiae by using a biological method. The method comprises the following process steps of: firstly, pretreating folium cortex eucommiae: grinding folium cortex eucommiae into pulp and carrying out enzymolysis; secondly, preparing a nitrogen source: carrying out membrane filtration, membrane concentration and resin adsorption, drying a membrane filtration concentrated solution and a solution under a column and using the obtained product as the nitrogen source for later use; and thirdly, extracting gutta-percha: inoculating eucommia fungi-16, carrying out solid fermentation, carrying out solid-liquid separation on a fermentation product, drying the obtained solution, using the obtained product as a carbon source for later use and carrying out fine laundering and refining on coarse glue to obtain fine glue. Due to the method for extracting gutta-percha, the production efficiency is high, the production cost is low, and chlorogenic acid can be co-produced so as to increase the yield.
Description
Technical field
The present invention relates to a kind of method of natural product extraction, relate in particular to a kind of method of utilizing biological process from Folium Eucommiae, to extract gutta-percha.
Background technology
Gutta-percha is a kind of white rope, chemical ingredients is anti--1, the 4-polyisoprene, has rubber-plastics duplicity, be called as second kind of natural gum, being the high-quality Jiao Yuan that subject range is the widest in the world, development potentiality is maximum, is the only substitute of natural rubber, can fundamentally solve the problem of China's natural rubber scarcity of resources.At present, about 350,000 hectares of China's cultivating eucommia area, account for more than 99% of world's bark of eucommia cultivated area, but tens tons only of the present annual production of domestic largest gutta-percha manufacturing enterprise, far can not satisfy the demand in market, these become focus with regard to feasible exploitation with Folium Eucommiae production gutta-percha technology.
Before the present invention, more existing patents about gutta-percha.From Folium Eucommiae, extract gutta-percha as Chinese patent notification number 1054985 comprehensive extraction of gutta-percha by fermentation-boiling-fine laundering-drying-solvent extraction-extraction thick glue-this operational path of purification that desolvates.Though the solation that this method can avoid mechanical process to cause loses, this method spontaneous fermentation required time long (2～3 months), it is not thorough to ferment, and fermentation substrate is dealt with improperly and can be caused environmental pollution; And before spontaneous fermentation, stoste is not carried out pre-treatment, shine into the material treatment capacity production costs such as big, increase capital construction.Chinese patent notification number 101157827 extracts filament gutta-percha from Folium Eucommiae and skin method discloses following technology: Folium Eucommiae, Cortex Eucommiae cutting-sodium hydroxide solution dissolving Folium Eucommiae stratum corneum and xylogen-cellulase hydrolysis-sherwood oil lixiviate-filtration-and freezing.Though this method has shortened extraction time, fiber and gutta-percha are that form with clamp region exists in the Folium Eucommiae, are layer of fibers-glue-line-layer of fibers-glue-line-fibrolaminar five-layer structures.Though soaking with sodium hydroxide solubilized stratum corneum and xylogen expose cellulose layer, the layer of fibers between glue-line can't contact with sodium hydroxide solution, makes that follow-up enzymolysis operation hydrolysis is not thorough, and the gutta-percha extraction yield is not high.Chinese patent application numbers 201010252992.9 1 kinds is extracted gutta-percha from Folium Eucommiae woods germinating branch skin method disclose a kind of from the bark of eucommia virgin forest strain screening fermentation Cortex Eucommiae, again by towards glue, the refining operational path that obtains smart glue.Though this technology can improve the gutta-percha yield, the primer-detonator in this technology need add alien species (Semen Maydis powder), and fermentation time is longer.In glue process, adopt the water blast gun flushing can cause the gutta-percha flow velocity serious.
Summary of the invention
The objective of the invention is: problems such as the production cycle at existing gutta-percha extraction process existence is long, extraction efficiency is low, other effective constituents are not used propose a kind of production efficiency height, low, the additional high process program of the output value of production cost.
Through a large amount of experiment and research, the inventor separates bacterium 32 strains in the soil ulmin in bark of eucommia forest zone, mould 67 strains.By to the screening of purifying bacterial classification with induce, obtaining to be the mould of polysaccharide and soluble substance with the Folium Eucommiae fiber degradation, and we are his called after bark of eucommia mould-16, and it is cultivated.
The invention provides a kind of method of utilizing biological process from Folium Eucommiae, to extract gutta-percha, comprise following processing step:
(1) pre-treatment: Folium Eucommiae adds 2 times of water (quality multiple, down together) defibrination, adds 6 times of water and 5 ‰ (in the cured leaf quality, down together) protease hydrolysis again, and wherein pH is 6, and temperature is 50～60 ℃, hydrolysis 1～2h, solid-liquid separation.
(2) preparation of nitrogenous source: enzymolysis solution is by micro-filtrate membrane filtration, concentrated, the resin absorption operation of nanofiltration membrane, with dry albumen and the polypeptide mixture of getting of liquid under microfiltration membrane concentrated solution and the resin absorption post.Resin elution can be got chlorogenic acid.
(3) extraction of gutta-percha: bark of eucommia mould-16 is inoculated in the centrifugal gained slag, carries out solid state fermentation at fermentation vat, solid-to-liquid ratio is 1: 2.5 (mass ratio, down together), and centrifugal after fermentation is finished, supernatant liquor drying, main component are polysaccharide and soluble substance.The thick glue of the bark of eucommia through fine laundering, refining obtain smart glue.
Wherein, albumen in the step (2) and the reuse of polypeptide mixture part are for solid state fermentation provides nitrogenous source.
Wherein, bark of eucommia mould-16 inoculum size 1～1.5% in the step (3), 35～40 ℃ of leavening temperatures, fermentation time 7d.
Wherein, the mixture part reuse of polysaccharide and soluble substance in the step (3) is for solid state fermentation provides carbon source.
Wherein, ferment when initial, press mass ratio and add carbon source and nitrogenous source at 3: 1.
The present invention has following beneficial effect:
1. Folium Eucommiae is carried out pre-treatment, the material treatment capacity when having reduced follow-up fermentation procedure, thus reduced capital cost.
2. sugar and the reuse of protein peptide part fermentation promotes fermented bacterium to grow fast, shortens fermentation time.
3. this production technique can be produced gutta-percha and chlorogenic acid simultaneously, saves cost, enhances productivity.
Description of drawings
Fig. 1 represents process flow sheet of the present invention
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1
The first step: pre-treatment.Get Folium Eucommiae 20kg, add 40kg water, with the steel defibrination, adding 120kg water and 0.1kg proteolytic enzyme again is 6 at pH, when temperature is 55 ℃, hydrolysis 2h is centrifugal.
Second step: nitrogenous source preparation.Supernatant liquor by the N100 micro-filtrate membrane filtration, is removed high molecular weight protein and suspended solid; See through liquid and concentrate through nanofiltration membrane, cycles of concentration is 6 times; Concentrated solution is by punching polymeric adsorbent absorption chlorogenic acid.Liquid under the post and micro-filtration concentrated solution is dry that albumen, polypeptide mix stand-by.
The 3rd step: the extraction of gutta-percha.Bark of eucommia mould-16 is inoculated in the centrifugal gained slag carries out solid state fermentation, inoculum size is 0.3kg, adds the nitrogenous source of previous step preparation and glucose as carbon source, the mass ratio of carbon source and nitrogenous source is 3: 1, add water and regulate that to make the solid-liquid mass ratio be 1: 2.5, leavening temperature is 37 ℃, and fermentation time is 7d.Centrifugal then that the supernatant liquor drying is obtained polysaccharide mixture is stand-by, and centrifugal slag is discharged rinse water through washing the back gently by rubbing with the hands, obtaining smart glue through refining again.
Embodiment 2
The first step: pre-treatment.Get Folium Eucommiae 20kg, add 40kg water, with the steel defibrination, adding 120kg water and 0.1kg proteolytic enzyme again is 6 at pH, when temperature is 55 ℃, hydrolysis 2h is centrifugal.
Second step: nitrogenous source preparation.Supernatant liquor by the N100 micro-filtrate membrane filtration, is removed high molecular weight protein and suspended solid; See through liquid and concentrate through nanofiltration membrane, cycles of concentration is 6 times; Concentrated solution is by punching polymeric adsorbent absorption chlorogenic acid.Liquid under the post and micro-filtration concentrated solution is dry that albumen, polypeptide mixture are stand-by.
The 3rd step: the extraction of gutta-percha.Bark of eucommia mould-16 is inoculated in the centrifugal gained slag carries out solid state fermentation, inoculum size is 0.3kg, the albumen, polypeptide mixture and the polysaccharide mixture that add preparation, the mass ratio that makes carbon source and nitrogenous source is 3: 1, add water and regulate that to make the solid-liquid mass ratio be 1: 2.5, leavening temperature is 35 ℃, and fermentation time is 7d.Centrifugal then that the supernatant liquor drying is obtained polysaccharide mixture is stand-by, and centrifugal slag is discharged rinse water through washing the back gently by rubbing with the hands, obtaining smart glue through refining again.
Claims (5)
1. method of utilizing biological process to extract gutta-percha from Folium Eucommiae comprises following processing step:
(1) pre-treatment: Folium Eucommiae adds 2 times of water (quality multiple, down together) defibrination, adds 6 times of water and 5 ‰ (in the cured leaf quality, down together) protease hydrolysis again, and wherein pH is 6, and temperature is 50～60 ℃, hydrolysis 1～2h, solid-liquid separation.
(2) preparation of nitrogenous source: enzymolysis solution is by micro-filtrate membrane filtration, concentrated, the resin absorption operation of nanofiltration membrane, with dry albumen and the polypeptide mixture of getting of liquid under microfiltration membrane concentrated solution and the resin absorption post.Resin elution can be got chlorogenic acid.
(3) extraction of gutta-percha: bark of eucommia mould-16 is inoculated in the centrifugal gained slag, carries out solid state fermentation at fermentation vat, solid-to-liquid ratio is 1: 2.5 (mass ratio, down together), and centrifugal after fermentation is finished, supernatant liquor drying, main component are polysaccharide and soluble substance.The thick glue of the bark of eucommia through fine laundering, refining obtain smart glue.
2. a kind of method of utilizing biological process to extract gutta-percha from Folium Eucommiae according to claim 1 is characterized in that albumen and the reuse of polypeptide mixture part in the step (2), for solid state fermentation provides nitrogenous source.
3. a kind of method of utilizing biological process from Folium Eucommiae, to extract gutta-percha according to claim 1, bark of eucommia mould-16 inoculum size 1～1.5% in it is characterized in that, 35～40 ℃ of leavening temperatures, fermentation time 7d.
4. a kind of method of utilizing biological process to extract gutta-percha from Folium Eucommiae according to claim 1 is characterized in that the mixture part reuse of middle polysaccharide of step (3) and soluble substance, for solid state fermentation provides carbon source.
5. a kind of method of utilizing biological process to extract gutta-percha from Folium Eucommiae according to claim 1 is characterized in that fermenting when initial, presses mass ratio and adds carbon source and nitrogenous source at 3: 1.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827412A (en) * | 2012-09-11 | 2012-12-19 | 沈阳化工大学 | Preparation method for natural gutta rubber-toughened plastic resin |
| CN103585421A (en) * | 2013-09-24 | 2014-02-19 | 牛玲 | Liver-nourishing and kidney-tonifying eucommia and preparation method thereof |
| CN103755976A (en) * | 2014-01-10 | 2014-04-30 | 吉首大学 | Eucommia ulmoides key fruit hull treating method beneficial to extraction of gutta-percha |
| CN103798520A (en) * | 2014-01-22 | 2014-05-21 | 唐忠海 | Feed additive for substituting antibiotics and preparation method thereof |
| CN104368171A (en) * | 2014-11-26 | 2015-02-25 | 国家林业局泡桐研究开发中心 | Gutta-percha washing and extracting equipment |
| CN105524287A (en) * | 2016-02-01 | 2016-04-27 | 吉首大学 | Method for extracting eucommia ulmoides gum from eucommia ulmoides shells through combination of fermentation and leaching |
| CN106084252A (en) * | 2016-08-12 | 2016-11-09 | 曹蕊 | A kind of method extracting gutta-percha in Folium Eucommiae skin |
| CN108948375A (en) * | 2018-08-29 | 2018-12-07 | 湖北中鑫生物科技有限公司 | A kind of preparation method of filament gutta-percha |
| CN113426156A (en) * | 2021-07-19 | 2021-09-24 | 李保刚 | Method for large-scale continuous production of eucommia rubber by using eucommia leaves |
| CN113801341A (en) * | 2020-06-15 | 2021-12-17 | 广州中国科学院先进技术研究所 | Method for extracting, concentrating and recovering organic solvent from gutta-percha |
-
2011
- 2011-04-27 CN CN2011101059672A patent/CN102276849A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827412A (en) * | 2012-09-11 | 2012-12-19 | 沈阳化工大学 | Preparation method for natural gutta rubber-toughened plastic resin |
| CN102827412B (en) * | 2012-09-11 | 2015-08-26 | 沈阳化工大学 | A kind of preparation method of natural Chinese gutta percha toughened thermoplastic resin |
| CN103585421A (en) * | 2013-09-24 | 2014-02-19 | 牛玲 | Liver-nourishing and kidney-tonifying eucommia and preparation method thereof |
| CN103585421B (en) * | 2013-09-24 | 2016-05-11 | 牛玲 | Bark of eucommia processed product of a kind of liver-kidney tonifying and preparation method thereof |
| CN103755976A (en) * | 2014-01-10 | 2014-04-30 | 吉首大学 | Eucommia ulmoides key fruit hull treating method beneficial to extraction of gutta-percha |
| CN103798520A (en) * | 2014-01-22 | 2014-05-21 | 唐忠海 | Feed additive for substituting antibiotics and preparation method thereof |
| CN104368171B (en) * | 2014-11-26 | 2016-03-16 | 国家林业局泡桐研究开发中心 | Gutta-percha equipment is extracted in washing |
| CN104368171A (en) * | 2014-11-26 | 2015-02-25 | 国家林业局泡桐研究开发中心 | Gutta-percha washing and extracting equipment |
| CN105524287A (en) * | 2016-02-01 | 2016-04-27 | 吉首大学 | Method for extracting eucommia ulmoides gum from eucommia ulmoides shells through combination of fermentation and leaching |
| CN105524287B (en) * | 2016-02-01 | 2017-12-19 | 吉首大学 | Fermentation leaching combines the method that gutta-percha is extracted from bark of eucommia shell |
| CN106084252A (en) * | 2016-08-12 | 2016-11-09 | 曹蕊 | A kind of method extracting gutta-percha in Folium Eucommiae skin |
| CN108948375A (en) * | 2018-08-29 | 2018-12-07 | 湖北中鑫生物科技有限公司 | A kind of preparation method of filament gutta-percha |
| CN113801341A (en) * | 2020-06-15 | 2021-12-17 | 广州中国科学院先进技术研究所 | Method for extracting, concentrating and recovering organic solvent from gutta-percha |
| CN113426156A (en) * | 2021-07-19 | 2021-09-24 | 李保刚 | Method for large-scale continuous production of eucommia rubber by using eucommia leaves |
| CN113426156B (en) * | 2021-07-19 | 2022-08-12 | 李保刚 | Method for large-scale continuous production of eucommia rubber by using eucommia leaves |
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Application publication date: 20111214 |