CN103588979A - Vacuum pulsing type method for extracting gutta-percha in eucommia ulmoides seed shells - Google Patents
Vacuum pulsing type method for extracting gutta-percha in eucommia ulmoides seed shells Download PDFInfo
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- CN103588979A CN103588979A CN201310599072.8A CN201310599072A CN103588979A CN 103588979 A CN103588979 A CN 103588979A CN 201310599072 A CN201310599072 A CN 201310599072A CN 103588979 A CN103588979 A CN 103588979A
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Abstract
The invention discloses a vacuum pulsing type method for extracting gutta-percha in eucommia ulmoides seed shells. The method comprises the following steps: (1) pretreatment of the raw materials: separating nuts in eucommia ulmoides samara with a mechanical method to obtain a percha-extracting raw material, namely the eucommia ulmoides seed shells; (2) extraction of gutta-percha: using petroleum ether with the boiling range being 60-90 DEG C as a solvent, and carrying out dynamic countercurrent extraction on the gutta-percha in the eucommia ulmoides seed shells, wherein the extraction temperature is 40-60 DEG C, and the extraction time is 1-10 hours; in the extraction process, carrying out intermittent vacuum pumping and vacuum breaking on an extracting tank, and utilizing vacuum pulsing to strengthen mass transfer; after the extraction is finished, carrying out freezing crystallization and separation on a gutta-percha petroleum ether solution to obtain the gutta-percha. According to the method, dynamic countercurrent extraction is combined with vacuum pulsing to strengthen mass transfer, so that the extraction efficiency is increased, the operation steps are reduced, and the cost is reduced. The method is also convenient for industrial application and has a wide prospect.
Description
Technical field
The present invention relates to a kind of extracting method of gutta-percha, specifically refer to adopt vacuum pulsation from bark of eucommia shell, to extract the method for gutta-percha.
Background technology
Gutta-percha is a kind of emerging functional materials, after sulfuration, not only can present rubbery state but also can present different plastics states, and its market application foreground is boundless.Gutta-percha is present in Cortex Eucommiae, leaf and fruit, and wherein in bark of eucommia shell, gel content can reach 15-20%, be the highest position of bark of eucommia gel content, and Eucommia Fruit is renewable every year, is the desirable feedstock of extracting gutta-percha.
Gutta-percha is soluble in the non-polar solvents such as sherwood oil, generally can only adopt the non-polar solvents such as sherwood oil to extract, but non-polar solvent is to Mierocrystalline cellulose, the penetrance of the hydroaropic substance such as pectin and xylogen is poor, collodion silk in bark of eucommia shell is again by with Mierocrystalline cellulose, the plant cell tissue that pectin and xylogen are main component is wrapped up and is gathered, thereby with there being very large resistance to mass transfer in the non-polar solvent extract processes such as sherwood oil, solvent is difficult to remove to dissolve gutta-percha through plant cell tissue, the solution that has dissolved gutta-percha is also difficult to discharge, extraction time is long and efficiency is low, the shell of having carried after glue still remains more gutta-percha.
For reducing resistance to mass transfer, prior art adopts enzymolysis or alkaline solution to carrying out pre-treatment in raw material mostly, with plant cell tissues such as zymin or etched with alkali solution Mierocrystalline cellulose, pectin and xylogen, to strengthen the penetrance of solvent, but enzymolysis lifetime is long, cost is high and the problem of weak effect, alkaline purification meeting produces a large amount of waste liquids, and serious environment pollution cannot adapt to the needs that gutta-percha industrialization is produced.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art exactly, and a kind of method of extracting gutta-percha in Eucommia shell is provided, and uses the method can overcome the impact of resistance to mass transfer, reduce gutta-percha residual quantity, and shorten extraction time, and save cost, improve extraction efficiency.
The present invention includes following step:
(1) pre-treatment of raw material, uses mechanical process after the kernel separation in Eucommia, must carry collagen material bark of eucommia shell.In the separated Eucommia seed by mechanical process, also some pectin in bark of eucommia shell, Mierocrystalline cellulose and xylogen can be removed, reduce foreign matter content, reduce resistance to mass transfer, be conducive to the extraction of gutta-percha.
As will be further removed pectin, Mierocrystalline cellulose and the xylogen in shell, further reduce the resistance to mass transfer in Gutta extraction process, can be by the bark of eucommia shell obtaining by patent documentation CN 103360612A(number of patent application: 201310341063.9, patentee: University Of Jishou, contriver: Chen Gongxi, Zhang Yongkang, silver are forever loyal etc.) shown in Eucommia shell adhesive supplier play glue and process, further remove impurity and minimizing resistance to mass transfer.
(2) extraction of gutta-percha, take boiling range as 60 ℃ of-90 ℃ of sherwood oils be solvent, gutta-percha in bark of eucommia shell is carried out to dynamic countercurrent extraction, extracting temperature is 40 ℃-60 ℃, extraction time 1-10 hour, carries out step vacuumizing and vacuum breaker to extractor in leaching process, utilizes vacuum pulsation reinforcing mass transfer, after extraction completes, gutta-percha petroleum ether solution is carried out to freezing crystallization separated, obtain gutta-percha.
The mechanism of vacuum pulsation reinforcing mass transfer is: because sherwood oil is the organic solvent that volatility is stronger, sherwood oil while vacuumizing in plant cell tissue can gasify because of decompression, cause plant cell tissue's internal pressure to be greater than outside plant tissue cell, the sherwood oil that has dissolved gutta-percha can be forced through plant cell tissue under differential pressure action; When vacuum breaker, plant tissue cell's external pressure is greater than in plant tissue cell and presses, sherwood oil outside plant tissue cell enters rapidly plant tissue cell inside and removes to dissolve gutta-percha because of differential pressure action, alternately changing and strengthened sherwood oil and be dissolved in the gutta-percha mass transfer in sherwood oil of this plant tissue cell external and internal pressure, reduces extraction efficiency raising, gutta-percha residual rate.
Compared with prior art, the invention has the beneficial effects as follows: by dynamic countercurrent, extract in conjunction with vacuum pulsation reinforcing mass transfer, improved extraction efficiency, shortened extraction time, reduced the residual rate of gutta-percha, through evidence, the method can make the residual rate of gutta-percha in shell be reduced to below 0.5%, extraction time shortens 30%-50%, and the gutta-percha residual rate of common extracting method is 0.7%-1%, the present invention has also saved alkaline solution or the pretreated processing step of zymin, reduced cost, do not carrying out in pretreated situation, still having obtained desirable extraction effect.
The present invention arranges and extracts temperature is 40 ℃-60 ℃; in this temperature range, can guarantee that sherwood oil has higher solubleness to gutta-percha; can not cause due to the violent agitation of sherwood oil again malleation leakage and affect vacuum pulsed operation; the method is also convenient to carry out industrialization, mass-producing and Standardization Practice, has a extensive future.
Embodiment
Below the method for gutta-percha in vacuum pulsating extraction bark of eucommia shell is elaborated.
Embodiment 1
(1) pre-treatment of raw material, uses mechanical process after the kernel separation in Eucommia, must carry collagen material bark of eucommia shell, then bark of eucommia shell is beaten to glue by the Eucommia shell adhesive supplier shown in patent documentation CN 103360612A and process, and further removes impurity.
(2) extraction of gutta-percha, take boiling range as 60 ℃ of-90 ℃ of sherwood oils be solvent, gutta-percha in bark of eucommia shell is carried out to dynamic countercurrent extraction, extracting temperature is 45 ℃, 1.5 hours extraction times, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker, utilize vacuum pulsation reinforcing mass transfer, after extraction completes, gutta-percha petroleum ether solution is carried out to freezing crystallization separated, obtain gutta-percha.
Embodiment 2
(1) pre-treatment of raw material, uses mechanical process after the kernel separation in Eucommia, must carry collagen material bark of eucommia shell.
(2) extraction of gutta-percha, take boiling range as 60 ℃ of-90 ℃ of sherwood oils be solvent, gutta-percha in bark of eucommia shell is carried out to dynamic countercurrent extraction, extracting temperature is 50 ℃, 9 hours extraction times, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker, utilize vacuum pulsation reinforcing mass transfer, after extraction completes, gutta-percha petroleum ether solution is carried out to freezing crystallization separated, obtain gutta-percha.
Embodiment 3
(1) pre-treatment of raw material, uses mechanical process after the kernel separation in Eucommia, must carry collagen material bark of eucommia shell.
(2) extraction of gutta-percha, take boiling range as 60 ℃ of-90 ℃ of sherwood oils be solvent, gutta-percha in bark of eucommia shell is carried out to dynamic countercurrent extraction, extracting temperature is 56 ℃, 6 hours extraction times, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker, utilize vacuum pulsation reinforcing mass transfer, after extraction completes, gutta-percha petroleum ether solution is carried out to freezing crystallization separated, obtain gutta-percha.
Claims (2)
1. vacuum pulsating extracts a method for gutta-percha in bark of eucommia shell, it is characterized in that comprising following step:
(1) pre-treatment of raw material, uses mechanical process after the kernel separation in Eucommia, must carry collagen material bark of eucommia shell;
(2) extraction of gutta-percha, take boiling range as 60 ℃ of-90 ℃ of sherwood oils be solvent, gutta-percha in bark of eucommia shell is carried out to dynamic countercurrent extraction, extracting temperature is 40 ℃-60 ℃, extraction time 1-10 hour, in leaching process, extractor is carried out to step vacuumizing and vacuum breaker, after having extracted, gutta-percha petroleum ether solution is carried out to freezing crystallization separated, obtain gutta-percha.
2. vacuum pulsating according to claim 1 extracts the method for gutta-percha in bark of eucommia shell, it is characterized in that: the bark of eucommia shell that separation of hull from kernel is obtained is played glue by the Eucommia shell adhesive supplier shown in patent documentation CN 103360612A and processed.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310599072.8A CN103588979A (en) | 2013-11-25 | 2013-11-25 | Vacuum pulsing type method for extracting gutta-percha in eucommia ulmoides seed shells |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310599072.8A CN103588979A (en) | 2013-11-25 | 2013-11-25 | Vacuum pulsing type method for extracting gutta-percha in eucommia ulmoides seed shells |
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| CN103588979A true CN103588979A (en) | 2014-02-19 |
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| CN201310599072.8A Pending CN103588979A (en) | 2013-11-25 | 2013-11-25 | Vacuum pulsing type method for extracting gutta-percha in eucommia ulmoides seed shells |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670001A (en) * | 2016-01-25 | 2016-06-15 | 吉首大学 | Method for extracting eucommia ulmoides gum from eucommia ulmoides shell |
Citations (5)
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|---|---|---|---|---|
| CN101138686A (en) * | 2007-07-23 | 2008-03-12 | 沈军 | Method for extracting active ingredient of natural product and uses thereof |
| CN101946848A (en) * | 2010-08-27 | 2011-01-19 | 中国农业大学 | Method for processing preserved apricot |
| CN102977380A (en) * | 2012-12-21 | 2013-03-20 | 吉首大学 | Method for extracting high-purity gutta-percha from cortex eucommiae key fruit |
| 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 |
| CN103360612A (en) * | 2013-08-07 | 2013-10-23 | 吉首大学 | Gum collector for eucommia ulmoides samara husks |
-
2013
- 2013-11-25 CN CN201310599072.8A patent/CN103588979A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101138686A (en) * | 2007-07-23 | 2008-03-12 | 沈军 | Method for extracting active ingredient of natural product and uses thereof |
| CN101946848A (en) * | 2010-08-27 | 2011-01-19 | 中国农业大学 | Method for processing preserved apricot |
| 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 |
| CN102977380A (en) * | 2012-12-21 | 2013-03-20 | 吉首大学 | Method for extracting high-purity gutta-percha from cortex eucommiae key fruit |
| CN103360612A (en) * | 2013-08-07 | 2013-10-23 | 吉首大学 | Gum collector for eucommia ulmoides samara husks |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670001A (en) * | 2016-01-25 | 2016-06-15 | 吉首大学 | Method for extracting eucommia ulmoides gum from eucommia ulmoides shell |
| CN105670001B (en) * | 2016-01-25 | 2018-04-20 | 吉首大学 | A kind of method that gutta-percha is extracted in the shell from the bark of eucommia |
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Application publication date: 20140219 |