CN1948410A - Method of extracting gutta percha by solvent circulation - Google Patents
Method of extracting gutta percha by solvent circulation Download PDFInfo
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- CN1948410A CN1948410A CN 200610051265 CN200610051265A CN1948410A CN 1948410 A CN1948410 A CN 1948410A CN 200610051265 CN200610051265 CN 200610051265 CN 200610051265 A CN200610051265 A CN 200610051265A CN 1948410 A CN1948410 A CN 1948410A
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- percha
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Abstract
This invention provides a solvent circulate extraction of gutta percha, and the ligarine is used for extraction of gutta percha from folium eucommiae or skin eucommiae. Its craft includes: (1)The raw material is through circulation drying in baking oven, and then shatterred by crusher, cribration. (2)The ligarine is added in accordance with dosage liquor ratio, refluxing in hot bath water. (3)Filtering as hot as possible, segregating its dregs and collecting the filtrate. (4)The filtrate is filtered after water cooling and hypothermy cold storage to reclaim gutta percha solid and filtrate separately. (5)The filtrate degelatinized mixes again with dregs, and then refluxing. (6)Crude product is obtained by combining gutta percha after conducting repetitive operation twice. (7)The ligarine reclaimed still can be used for extraction of gutta percha.
Description
Technical field
The present invention relates to a kind of extraction method of molding natural resins, extract the method for gutta-percha skin in particular to the employing solvent from the natural phant gutta-percha tree and the leaf.
Background technology
The bark of eucommia (Eucommia ulmoides Oliv) is the distinctive famous and precious economic tree of China, the white thread gutta-percha that is rich in its leaf, skin and the seed (Eucommia ulmoides gum, be called gutta-percha or balata), it is the isomers of natural para rubber, be trans-polyisoprene, and natural rubber is cis-polyisoprene, and structure is as follows:
Trans-polyisoprene cis-polyisoprene
One of gutta-percha tree important glue source plant that still subject range is the widest in the world all contains gutta-percha in its pericarp, bark, the blade.Gutta-percha has specific functions such as " rubber-plastics dual nature " and shape memory.Gutta-percha is present in containing in the cellula adhesiae of gutta-percha tree with a kind of orderly crystallization hard solid particulate, can not directly extract to obtain.
The existing extracting method of gutta-percha has dry method and wet method (solvent-extraction process) two classes.It is to destroy by the method for machinery to contain cellula adhesiae that dry method reclaims gutta-percha, and gutta-percha is come out, and obtains through separation again; Wet method is then as the solvent-extraction process of Chinese patent ZL00135831.6 grade, with low polar solvent, extract as chloroform, lower boiling sherwood oil, benzene class etc. that two keys are arranged, gutta-percha is dissolved out from vegetable cell, through adding methyl alcohol, ethanol, acetone, ethyl acetate isopolarity solvent colloid is separated out again, perhaps solvent evaporated obtains the gutta-percha solid matter.Dry method is carried the extraction yield height of glue not as wet method.But there is following shortcoming in wet method: the solvent species that 1. can dissolve gutta-percha is few, and the gutta-percha that is dissolved in the solvent is difficult to separate with solvent the recovery difficulty of glue; When 2. adopt changing solvent polarity and making the method that colloid separates out, then solvent can't utilize again, and solvent-oil ratio is big; 3. straight run distillation separates solvent and colloid, the impure amount height of the colloid that obtains; If 4. the pulverizing of raw material is abundant inadequately, colloid can not leach fully, and productive rate is affected; 5. the organic solvent volatility that boiling point is too low is big, and security is relatively poor.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts the single solvent circulation to extract gutta-percha, solvent can't utilize or the high defective of the impure amount of colloid again in the prior art to overcome.
In a large amount of experiments and research process, the contriver finds that boiling range is that 60-90 ℃ hot sherwood oil has good dissolving power to gutta-percha; Coexist with α type and β type just because of the gutta-percha crystal, fusing point is respectively 65 ℃ and 55 ℃, be difficult to dissolve at normal temperatures, so when under being higher than 65 ℃ temperature condition, refluxing, the molten state gutta-percha easily is dissolved in the sherwood oil, and the sol solution that contains that heat filtering obtains is cooled off, and gutta-percha is just separated out so that white is cotton-shaped, below-20 ℃, the colloidal amount of separating out reaches the highest.
For gutta-percha being extracted from Cortex Eucommiae, leaf, pericarp with sherwood oil, and higher extraction yield arranged, the contriver has also carried out a large amount of experiments with regard to the technic index of extracting gutta-percha, has determined to separate out preferably temperature, solid-liquid ratio, raw material pulverizing particle diameter, extraction time, backflow extraction temperature.
Based on above-mentioned achievement in research, the method that gutta-percha is extracted in the circulation that the contriver provides is solvent with the sherwood oil, extracts gutta-percha from Folium Eucommiae or Cortex Eucommiae, and this technology may further comprise the steps:
(1) Folium Eucommiae or Cortex Eucommiae are descended air seasoning 3～4h about 50 ℃ in baking oven, pulverize, sieve through pulverizer;
(2) in pulverize the ratio of dry material quality with solvent volume be 1: 10～15 ratio to add the boiling range temperature be 60～90 ℃ petroleum ether solvent, 2h refluxes in 75～85 ℃ hot water bath;
(3) filter with the above stainless (steel) wire of 100 orders while hot, separate the discharging slag, and collection is dissolved with the filtrate of gutta-percha;
(4) filtrate of waiting to be dissolved with gutta-percha through water-cooled, be lower than-20 ℃ deepfreeze after, filter with 100 order stainless (steel) wires, reclaim gutta-percha solid of separating out and the filtrate of having sloughed gutta-percha respectively;
(5) filtrate of having sloughed gutta-percha is mixed and backflow 1.5h with the material slag again;
(6) look the situation of gutta-percha stripping in Cortex Eucommiae or the Folium Eucommiae, repetitive operation step (3), (4) and (5) merge the gutta-percha that all filtrations obtain more than twice or twice, are thick product;
(7) reclaim the sherwood oil filtrate that obtains and be used further to new Folium Eucommiae (perhaps Cortex Eucommiae) raw material continuation extraction gutta-percha; In case of necessity, by weight/volume ratio, replenish a spot of fresh sherwood oil.
The contriver points out: the Folium Eucommiae of pulverizing or Cortex Eucommiae are thick excessively, and it is incomplete to carry glue; Cross the detailed rules and regulations collodion silk and destroy seriously, so sieve in the first step and can be the 60-80 order, 60 orders are advisable most.
The contriver learns through experiment, and 1: 10 above solid-liquid ratio is the gutta-percha in the stripping leaf more completely, and the ratio of therefore determining to pulverize in second step dry material quality and solvent volume is 1: 10～15, and wherein be good at 1: 10.
It is as shown in the table that solid-liquid ratio is deposited the influence under the condition in 2 hours to the rate of recovery at-20 ℃:
| Reflux temperature | Return time | 60 order leaves (g) | Sherwood oil amount (ml) | Solid-liquid ratio | Extract thick glue and reclaim (%) |
| 80 ℃ (stirring) | 2h | 60 | 420 | 1∶7 | 2.121 |
| 60 | 480 | 1∶8 | 2.401 | ||
| 60 | 600 | 1∶10 | 2.508* | ||
| 80 | 800 | 1∶10 | 2.498* | ||
| 60 | 800 | 1∶13 | 2.495 | ||
| 40 | 400 | 1∶10 | 2.448* | ||
| 60 | 960 | 1∶16 | 2.524 |
The contriver points out that temperature raises and helps the mass transfer diffusion, and the extraction temperature of determining for second step can obtain comparatively ideal result at 75～85 ℃ more than 80 ℃; With this understanding, reflux extracting time is advisable with 1～3h.
Emphasizing filtered while hot in the 3rd step, is to prevent that gutta-percha from precipitateing in the material slag, reduces extraction yield.
The temperature of separating out of gutta-percha is tested definite in the 4th step through the contriver, experimental result shows, freezing 40min can make the gutta-percha precipitating of the overwhelming majority come out under-20 ℃ condition, refrigeration 0.5～2h, substantially gutta-percha can be separated out fully, so the deepfreeze time is defined as 0.5～2h.
The backflow in the 5th step is to expect that as far as possible the gutta-percha that contains in the slag reclaims.
" method of extracting gutta percha by solvent circulation " of the present invention simplified original gutta-percha widely and reclaimed technology, and the solvent of the lixiviate gutta-percha that reclaims, and can be used as to carry peptizing agent and recycle, and realizes the solvent closed circulation, do not discharge; Owing to adopted the low temperature separation method, the volatilization loss amount of solvent is little, and is less to the pollution of ambient air, and impurity still is retained in the solution, the purity height of the gutta-percha of recovery; Easy, the safety of operating procedure.
Description of drawings
Fig. 1 is the influence of backflow extraction temperature under 1: 10 condition for solid-liquid ratio, and Fig. 2 is the influence that return time reclaims the lixiviate of glue, and Fig. 3 is the influence to the gutta-percha amount of separating out of the temperature of cooled and stored.
Embodiment
Embodiment is a raw material with commercially available Cortex Eucommiae, is that 60～90 ℃ sherwood oil is a solvent with the boiling range temperature.Cortex Eucommiae is descended air seasoning 3～4h about 50 ℃ in baking oven, pulverize, cross 60 mesh sieves through pulverizer; In pulverizing the ratio of dry material quality with solvent volume is that 1: 10 ratio adds petroleum ether solvent, and 2h refluxes in 75～85 ℃ hot water bath; Filter with the above stainless (steel) wire of 100 orders while hot, separate the discharging slag, and collection is dissolved with the filtrate of gutta-percha in tool plug triangular flask; Treat filtrate through water-cooled, be lower than-20 ℃ deepfreeze 1h after, filter with 100 order stainless (steel) wires, reclaim gutta-percha solid of separating out and the filtrate of having sloughed gutta-percha respectively; Having sloughed the filtrate of gutta-percha mixes and backflow 1.5h with the material slag again; Repeat aforesaid operations step twice, merge the gutta-percha that all filtrations obtain, promptly obtain thick product.The sherwood oil filtrate that recovery obtains is used further to the extraction once more of Cortex Eucommiae or Folium Eucommiae raw material, perhaps is used for the extraction of new Folium Eucommiae raw material, and what the maximum of realization solvent reclaimed recycles.The gutta-percha extraction yield that obtains by this operation can reach 100%.
Claims (4)
1 one kinds of methods that adopt the one-component extracting gutta percha by solvent circulation are solvent with the sherwood oil, extract gutta-percha from Folium Eucommiae or Cortex Eucommiae, it is characterized in that this technology may further comprise the steps:
(1) Folium Eucommiae or Cortex Eucommiae are descended air seasoning 3～4h about 50 ℃ in baking oven, pulverize, sieve through pulverizer;
(2) in pulverize the ratio of dry material quality with solvent volume be 1: 10～15 ratio to add the boiling range temperature be 60～90 ℃ petroleum ether solvent, in 75～85 ℃ hot water bath, reflux;
(3) filter with the above stainless (steel) wire of 100 orders while hot, separate the discharging slag, and collection is dissolved with the filtrate of gutta-percha;
(4) filtrate of waiting to be dissolved with gutta-percha is filtered the filtrate of reclaiming the gutta-percha solid respectively and having sloughed gutta-percha through after the water cooling, again in being lower than under-20 ℃ the condition behind the deepfreeze with 100 order stainless (steel) wires;
(5) filtrate of having sloughed gutta-percha is mixed and backflow 1.5h with the material slag again;
(6) look the situation of gutta-percha stripping, repetitive operation step (3), (4) and (5) merge the gutta-percha that all filtrations obtain more than twice or twice, are thick product;
(7) reclaim the sherwood oil filtrate that obtains and be used for Folium Eucommiae or Cortex Eucommiae raw material extraction gutta-percha once more; In case of necessity, replenish fresh sherwood oil.
2 the method for claim 1 is characterized in that it is 60 orders that the first step crushed material is crossed sieve aperture.
3 the method for claim 1, the extraction temperature that it is characterized in that for second step is under 75～85 ℃ of conditions, and reflux extracting time is 1～3h.
4 the method for claim 1 is characterized in that the deepfreeze time is 0.5～2h in the 4th step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610051265XA CN100457846C (en) | 2006-11-08 | 2006-11-08 | Method of extracting gutta percha by solvent circulation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610051265XA CN100457846C (en) | 2006-11-08 | 2006-11-08 | Method of extracting gutta percha by solvent circulation |
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| CN1948410A true CN1948410A (en) | 2007-04-18 |
| CN100457846C CN100457846C (en) | 2009-02-04 |
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| CNB200610051265XA Expired - Fee Related CN100457846C (en) | 2006-11-08 | 2006-11-08 | Method of extracting gutta percha by solvent circulation |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009113425A1 (en) * | 2008-03-14 | 2009-09-17 | 日立造船株式会社 | Biopolymer originating in eucommia ulmoides |
| CN102838756A (en) * | 2012-08-28 | 2012-12-26 | 河南恒瑞源实业有限公司 | Ultrasound two-way gutta-percha preparation method |
| CN102838759A (en) * | 2012-09-21 | 2012-12-26 | 汉中永杨医药科技发展有限公司 | Method and device for extracting eucommia ulmoides gum from insect excrement of insect eating eucommia ulmoides |
| CN102838758A (en) * | 2012-08-28 | 2012-12-26 | 河南恒瑞源实业有限公司 | Method of preparing gutta-percha with eucommia leaves |
| CN102850555A (en) * | 2012-08-28 | 2013-01-02 | 河南恒瑞源实业有限公司 | Method for preparing gutta-percha from eucommia bark |
| CN103131024A (en) * | 2011-11-28 | 2013-06-05 | 湘西老爹生物有限公司 | Method for extracting eucommia ulmoides refined glue |
| CN103131026A (en) * | 2011-12-01 | 2013-06-05 | 湘西老爹生物有限公司 | Concentration rubber-separating method in eucommia rubber extraction process |
| CN103131025A (en) * | 2011-11-28 | 2013-06-05 | 湘西老爹生物有限公司 | Method for extracting gutta percha from eucommia ulmoides nutshell |
| CN101157827B (en) * | 2007-09-27 | 2014-03-05 | 贵州大学 | Method for extracting filament gutta-percha from eucommia leaf and skin |
| CN103881116A (en) * | 2014-04-13 | 2014-06-25 | 吉首大学 | Method for extracting gutta-percha from plant tissues |
| CN104448346A (en) * | 2014-11-28 | 2015-03-25 | 河南恒瑞源实业有限公司 | Extraction method of eucommia ulmoides gum |
| CN108047356A (en) * | 2018-01-29 | 2018-05-18 | 山东贝隆杜仲生物工程有限公司 | A kind of method of the thick glue of refined Cortex Eucommiae |
| CN112300406A (en) * | 2020-10-22 | 2021-02-02 | 西北农林科技大学 | Method for pretreating eucommia ulmoides leaves before extracting gutta-percha from eucommia ulmoides leaves |
| CN113426156A (en) * | 2021-07-19 | 2021-09-24 | 李保刚 | Method for large-scale continuous production of eucommia rubber by using eucommia leaves |
Family Cites Families (3)
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| CN1036724C (en) * | 1992-12-24 | 1997-12-17 | 中国科学院化学研究所 | Extracting method for gutta-percha |
| CN1212272A (en) * | 1998-08-31 | 1999-03-31 | 贵阳黔人中药材种植发展有限责任公司 | Process for extracting raw rubber from bark of eucommia |
| CN1183955C (en) * | 2003-04-09 | 2005-01-12 | 李保刚 | Method of continuously producing eucommia extract powder, gutta percha, eucommia resin and organic fertilizer using eucommia leaf |
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2006
- 2006-11-08 CN CNB200610051265XA patent/CN100457846C/en not_active Expired - Fee Related
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157827B (en) * | 2007-09-27 | 2014-03-05 | 贵州大学 | Method for extracting filament gutta-percha from eucommia leaf and skin |
| JP2009221306A (en) * | 2008-03-14 | 2009-10-01 | Hitachi Zosen Corp | Biopolymer originating in eucommia ulmoides |
| US8093338B2 (en) | 2008-03-14 | 2012-01-10 | Hitachi Zosen Corporation | Biopolymer originating in Eucommia ulmoides |
| WO2009113425A1 (en) * | 2008-03-14 | 2009-09-17 | 日立造船株式会社 | Biopolymer originating in eucommia ulmoides |
| CN103131024A (en) * | 2011-11-28 | 2013-06-05 | 湘西老爹生物有限公司 | Method for extracting eucommia ulmoides refined glue |
| CN103131025A (en) * | 2011-11-28 | 2013-06-05 | 湘西老爹生物有限公司 | Method for extracting gutta percha from eucommia ulmoides nutshell |
| CN103131026A (en) * | 2011-12-01 | 2013-06-05 | 湘西老爹生物有限公司 | Concentration rubber-separating method in eucommia rubber extraction process |
| CN102838758A (en) * | 2012-08-28 | 2012-12-26 | 河南恒瑞源实业有限公司 | Method of preparing gutta-percha with eucommia leaves |
| CN102850555B (en) * | 2012-08-28 | 2015-04-29 | 河南恒瑞源实业有限公司 | Method for preparing gutta-percha from eucommia bark |
| CN102838756A (en) * | 2012-08-28 | 2012-12-26 | 河南恒瑞源实业有限公司 | Ultrasound two-way gutta-percha preparation method |
| CN102850555A (en) * | 2012-08-28 | 2013-01-02 | 河南恒瑞源实业有限公司 | Method for preparing gutta-percha from eucommia bark |
| CN102838758B (en) * | 2012-08-28 | 2015-04-29 | 河南恒瑞源实业有限公司 | Method of preparing gutta-percha with eucommia leaves |
| CN102838756B (en) * | 2012-08-28 | 2015-04-15 | 河南恒瑞源实业有限公司 | Ultrasound two-way gutta-percha preparation method |
| CN102838759A (en) * | 2012-09-21 | 2012-12-26 | 汉中永杨医药科技发展有限公司 | Method and device for extracting eucommia ulmoides gum from insect excrement of insect eating eucommia ulmoides |
| CN102838759B (en) * | 2012-09-21 | 2014-10-15 | 汉中永杨医药科技发展有限公司 | Method and device for extracting eucommia ulmoides gum from insect excrement of insect eating eucommia ulmoides |
| CN103881116A (en) * | 2014-04-13 | 2014-06-25 | 吉首大学 | Method for extracting gutta-percha from plant tissues |
| CN104448346A (en) * | 2014-11-28 | 2015-03-25 | 河南恒瑞源实业有限公司 | Extraction method of eucommia ulmoides gum |
| CN104448346B (en) * | 2014-11-28 | 2020-11-13 | 河南恒瑞源实业有限公司 | Extraction method of gutta-percha |
| CN108047356A (en) * | 2018-01-29 | 2018-05-18 | 山东贝隆杜仲生物工程有限公司 | A kind of method of the thick glue of refined Cortex Eucommiae |
| CN108047356B (en) * | 2018-01-29 | 2020-06-16 | 山东贝隆杜仲生物工程有限公司 | Method for refining eucommia ulmoides crude glue solution |
| CN112300406A (en) * | 2020-10-22 | 2021-02-02 | 西北农林科技大学 | Method for pretreating eucommia ulmoides leaves before extracting gutta-percha from eucommia ulmoides leaves |
| 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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