CN103665392A - Method for separating out gutta-percha from solution - Google Patents

Method for separating out gutta-percha from solution Download PDF

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Publication number
CN103665392A
CN103665392A CN201310599288.4A CN201310599288A CN103665392A CN 103665392 A CN103665392 A CN 103665392A CN 201310599288 A CN201310599288 A CN 201310599288A CN 103665392 A CN103665392 A CN 103665392A
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China
Prior art keywords
percha
gutta
solution
water
solvent
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Application number
CN201310599288.4A
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Chinese (zh)
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CN103665392B (en
Inventor
张永康
李克刚
陈功锡
银永忠
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Jishou University
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Jishou University
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Publication of CN103665392B publication Critical patent/CN103665392B/en
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Abstract

The invention discloses a method for separating out gutta-percha from a solution. The operation steps are as follows: an ice water mixture is quickly added to the bottom, the middle and the top of the gutta-percha solution to be subjected to separation, and is quickly stirred to enable the temperature of the mixed solution to range from 0 DEG C to 4 DEG C, wherein the mass of the added ice water mixture is 1 to 5 times than that of the gutta-percha solution; at the moment, the ice water mixture and the gutta-percha solution are directly contacted to transfer heat and quickly cooled to crystallize; after crystallization is finished, the mixed solution stands still for stratification, wherein water is located on the bottommost layer, gutta-percha which is separated out is located on the middle layer, and a solvent after separation is located on the uppermost layer; the water, the solvent and the gutta-percha can be completely separated through centrifugation, filtration and liquid separation. The method shortens separation time, reduces solvent loss, obtains high-quality gutta-percha, and is convenient for implementation of industrialization.

Description

A kind of method that gutta-percha is resolved from solution
Technical field
The present invention relates to a kind of analytic method of gutta-percha, specifically refer to by freezing the method for gutta-percha separation from solution.
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.Conventionally adopt the non-polar solvents such as sherwood oil to extract from the plant tissue of the bark of eucommia, because gutta-percha is soluble in the hot non-polar solvents such as sherwood oil, in the cold non-polar solvents such as sherwood oil, solubleness is very low, therefore, to having extracted the solution of gutta-percha, carry out frozen cooling, gutta-percha can crystallization.
Present stage mainly adopts common dividing wall type frozen cooling or puts into refrigerator and lower the temperature, but dividing wall type frozen cooling or put into the method that refrigerator lowers the temperature and exist heat transmission resistance large, crystallization is problem slowly, particularly in the process of slow cooling, can cause soltion viscosity to promote rapidly, cannot transmission of heat by convection, heat transmission resistance can be therefore increasing, lower the temperature also more and more slower, the gutta-percha of now separating out can form gradually cotton-shaped suspended substance in solution, after crystallization completes, be difficult to completely separated with organic solvent, even if separation also easily causes the loss of a large amount of solvents reluctantly, not only waste resource but also contaminate environment, this has seriously perplexed the industrialization production process of gutta-percha.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art exactly, a kind of method that gutta-percha is resolved from solution is provided, use the method can overcome the impact of heat transmission resistance, shorten the crystallization time, effectively solve gutta-percha later separation trouble that slow cooling causes the problem of a large amount of solvents of loss.
Processing step of the present invention is: toward the bottom of gutta-percha solution to be resolved, middle part and top add fast mixture of ice and water and stir rapidly, make the temperature of mixed solution between 0 ℃-4 ℃, the quality that mixture of ice and water adds is 1-5 times of gutta-percha solution quality, now frozen water and gutta-percha solution carry out direct contact heat transfer and fast cooling crystallization, stratification after crystallization completes, now water is in the lowest layer, the gutta-percha of the resolving layer that mediates, and solvent after resolving occupy the superiors, again through centrifugal, filtration and separatory can be realized water, the complete separation of solvent and gutta-percha.
Compared with prior art, the invention has the beneficial effects as follows: utilize the non-polar solvents such as water and sherwood oil immiscible, the principle of meeting layering after standing, after frozen water, frozen water and gutta-percha solution carry out direct contact heat transfer, and gutta-percha fast cooling crystallization now efficiently solves cotton-shaped gutta-percha later separation trouble that slow cooling causes the problem of a large amount of solvents of loss, although method is simple, effect is very outstanding.The present invention, also due to the raising of heat exchange efficiency, has shortened the time of gutta-percha crystallization, has also saved the energy.
Because gutta-percha solubleness in the hot non-polar solvents such as sherwood oil is higher; and solubleness is very low in the non-polar solvents such as sherwood oil of 0 ℃-4 ℃; thereby; the resolution factor of gutta-percha is also very high; water after separation and solvent also can be realized and recycling very easily, and the loss of solvent is very low, and the gutta-percha that the method obtains is that bulk and quality are good; be convenient to carry out industrialization, mass-producing and Standardization Practice, have a extensive future.
Embodiment
Below the method that gutta-percha is resolved from solution is elaborated.
Embodiment 1
Bottom, middle part and top toward gutta-percha solution to be resolved add fast mixture of ice and water and stir rapidly, the temperature that makes mixed solution is 1 ℃, the quality that mixture of ice and water adds is 3 times of gutta-percha solution quality, now frozen water and gutta-percha solution carry out direct contact heat transfer and fast cooling crystallization, stratification after crystallization completes, now water is in the lowest layer, the gutta-percha of the resolving layer that mediates, and solvent after resolving occupy the superiors, more realize the complete separated of water, solvent and gutta-percha through centrifugal, filtration with separatory.
Embodiment 2
Bottom, middle part and top toward gutta-percha solution to be resolved add fast mixture of ice and water and stir rapidly, the temperature that makes mixed solution is 0 ℃, the quality that mixture of ice and water adds is 4 times of gutta-percha solution quality, now frozen water and gutta-percha solution carry out direct contact heat transfer and fast cooling crystallization, stratification after crystallization completes, now water is in the lowest layer, the gutta-percha of the resolving layer that mediates, and solvent after resolving occupy the superiors, more realize the complete separated of water, solvent and gutta-percha through centrifugal, filtration with separatory.
Embodiment 3
Bottom, middle part and top toward gutta-percha solution to be resolved add fast mixture of ice and water and stir rapidly, the temperature that makes mixed solution is 3.1 ℃, the quality that mixture of ice and water adds is 1.6 times of gutta-percha solution quality, now frozen water and gutta-percha solution carry out direct contact heat transfer and fast cooling crystallization, stratification after crystallization completes, now water is in the lowest layer, the gutta-percha of the resolving layer that mediates, and solvent after resolving occupy the superiors, more realize the complete separated of water, solvent and gutta-percha through centrifugal, filtration with separatory.

Claims (1)

1. the method that gutta-percha is resolved from solution, it is characterized in that: toward the bottom of gutta-percha solution to be resolved, middle part and top add fast mixture of ice and water and stir rapidly, make the temperature of mixed solution between 0 ℃-4 ℃, the quality that mixture of ice and water adds is 1-5 times of gutta-percha solution quality, now frozen water and gutta-percha solution carry out direct contact heat transfer and fast cooling crystallization, stratification after crystallization completes, water is in the lowest layer, the gutta-percha of the resolving layer that mediates, solvent after parsing occupy the superiors, again through centrifugal, filtration and separatory can be realized water, the complete separation of solvent and gutta-percha.
CN201310599288.4A 2013-11-25 2013-11-25 Method for separating out gutta-percha from solution Expired - Fee Related CN103665392B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310599288.4A CN103665392B (en) 2013-11-25 2013-11-25 Method for separating out gutta-percha from solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310599288.4A CN103665392B (en) 2013-11-25 2013-11-25 Method for separating out gutta-percha from solution

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CN103665392A true CN103665392A (en) 2014-03-26
CN103665392B CN103665392B (en) 2015-05-20

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103965489A (en) * 2014-06-02 2014-08-06 吉首大学 Continuous gutta-percha freezing-out device

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN103360275A (en) * 2012-03-30 2013-10-23 上海希迈医药科技有限公司 Method for preparing agomelatine I-type crystal

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN103360275A (en) * 2012-03-30 2013-10-23 上海希迈医药科技有限公司 Method for preparing agomelatine I-type crystal

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103965489A (en) * 2014-06-02 2014-08-06 吉首大学 Continuous gutta-percha freezing-out device

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