CN104558258B - A kind of gutta-percha fractionation column and the method that gutta-percha is carried out series classification - Google Patents
A kind of gutta-percha fractionation column and the method that gutta-percha is carried out series classification Download PDFInfo
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- CN104558258B CN104558258B CN201410775569.5A CN201410775569A CN104558258B CN 104558258 B CN104558258 B CN 104558258B CN 201410775569 A CN201410775569 A CN 201410775569A CN 104558258 B CN104558258 B CN 104558258B
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Abstract
A kind of gutta-percha fractionation column and the method that gutta-percha is carried out series classification; the method of the present invention uses four sections of fractionation columns; can be by certain speed at addition precipitant at different levels; change the dissolubility of solvent continuously, carry out gutta-percha, once through fractionation column, obtaining the fraction that various molecular weights is interval simultaneously; coordinate the thermograde caused at each inter-stage; improve separation efficiency, effectively reduce precipitant usage amount, accomplish industrial scale classification.
Description
Technical field
The invention belongs to gutta-percha production field, a kind of gutta-percha fractionation column and gutta-percha is carried out series classification
Method.
Background technology
The Cortex Eucommiae (Eucommia ulmoides Olive) is that the Eucommiaceae Cortex Eucommiae belongs to deciduous tree, is specific to China
Rare medicinal herbs seeds, are also the important glue source plants that subject range is the widest in the world, belong to Chinese Second Class Key Protected Plant.The Cortex Eucommiae is removed
Beyond containing substantial amounts of medicinal ingredient, possibly together with substantial amounts of gutta-percha in the tissues such as leaf, bark, seed.Gutta-percha belongs to
Rigid rubber, is blended and deep processing by sulfide modifier or with other material, and gutta-percha can develop series of new merit
Energy material and industrial materials, especially have purposes widely in rubber, tire industry.There are some researches show: Du
Secondary glue and natural rubber blend composition, before reaching blending ratio 1:1, tensile strength, stretching strength, shore hardness, pull apart elongation
Rate has almost no change.Gutta-percha has more dynamic mechanical and low this excellent specific property is lost, the most suitable in using temperature range
The 1/ 5 of fourth glue, the 1/ 6 of natural rubber.Its anti-flex performance is excellent, makees rubber with it, under alternate stress, and material
Heat release reduces, and extends service life, and this is at rubber applications field tools such as tire industry, industrial conveyor-line, damping shock absorption parts
There is huge potential application value.
All containing gutta-percha in Eucommia Fruit, bark and blade, wherein gutta-percha content in samara is up to 10%～12%, bark
Gum content 6%～10%, blade gum content 1%～3%, the extraction of gutta-percha all can be extracted with the Cortex Eucommiae each position raw material.By
In having, the harvesting of Different Variation type, different times, different sources and the Cortex Eucommiae of different clones, its gum content and gutta-percha are special
Property all there are differences.Carry gluing method and have fermentation method, extraction and alkaline leaching and frozen glue method etc..Using different material, difference carries
The gutta-percha that access method extracts in purity, average molecular weight range and obvious difference is distributed, such as gutta-percha middle-molecular-weihydroxyethyl
Scope is from 10,000 to the highest close to 1,000,000, and the section that the gutta-percha molecular weight of separate sources is concentrated also has difference, and this is to gutta-percha
Real application research and industrialization bring difficulty, because the various mechanical properties of polymer and its molecular weight and molecular weight thereof
It is distributed closely related, is to determine its application performance and the important evidence of processing behavior, therefore to gutta-percha crude product, the most directly makes
The Gutta extraction liquid obtained with solvent extraction carries out precipitation fractionation, it is thus achieved that the product of various interval molecular weight is of practical significance.
The classification of polymer is to realize according to polymer difference of dissolubility in its good solvent and poor solvent, logical
Often low-molecular weight polymer part is relatively easily dissolved in a solvent, and high molecular weight moieties relatively indissoluble solution, it is usually in polymerization
The good solvent of thing adds poor solvent, first high molecular weight moieties be first precipitated out.So that this process is repeatedly
And reach better effects, but this technique is time-consuming, consumes quantity of solvent greatly, and the industrial cost that realizes is high, and organic volatilizable thing pollutes
Greatly, it not economic and environment-friendly method.
Wolf B A mentions the apparatus and method of Polymer Fractionation in patent DE3242130A1 and US5242594；Feng Ya
Above-mentioned Polymer Fractionation apparatus and method are improved in patent CN 161486777 B by triumphant grade, so that it is applicable to gather
The classification of urethane.The method of above-mentioned use has accomplished continuous operation, but polymer is once separated by fractionation column, final
A fraction with a lower molecular weight containing higher molecular weight can be obtained, if to high molecular or low-molecular-weight polymeric
If thing fraction needs further classification, in addition it is also necessary to above-mentioned fraction is realized by fractionation column classification again, adds precipitant
Consumption, and equipment, place investment and operation easier.
Summary of the invention
It is an object of the invention to provide a kind of gutta-percha fractionation column and use thermograde and precipitant concentration gradient to Du
Secondary glue carries out the method for series classification.The method of the present invention is realized by gutta-percha series classification post, the topmost of fractionation column
Being gutta-percha leaching liquid or crude product gutta-percha solution inlet, be divided into four sections inside post, one section is one-level, has porous between every section
Dividing plate separates, upper berth industrial filter cloth or industrial filter paper；Precipitant inlet and backflow entrance, every pars infrasegmentalis are arranged at every section of top
There is solution flow export after precipitation fractionation；Being with coolant jacket outside fractionation column, coolant enters from coolant jacket lower end；First order interface
Connect and have air compression plant, to provide the pressure needed for filtering；Run through series connection at different levels at fractionation column built with one to stir
Device, stirring power resources are in the motor of fractionation column foot.
A kind of method that gutta-percha is carried out series classification, is by unassorted to gutta-percha leaching liquid or gutta-percha crude product
Solution pumps into from fractionation column first order upper end entrance, pressurizes in the first order, and starts stirring motor holding moderate-speed mixer, and solution exists
After each section of fractionation column forms steady flow, open precipitant inlet, by precipitant by suitable gutta-percha solution/precipitant stream
Speed ratio pumps into, and the solution through precipitation fractionation flows out from the flow export of this section, and effluent is through being filtrated to get gutta-percha middle-molecular-weihydroxyethyl
The fraction of highest part, filtrate squeezes into this level through external pump from reflux inlet at different levels；Under pressure-driven, the first order molten
Liquid slow transit through lay industrial filter cloth dividing plate enter the second level, the precipitant the most slowly injected in the second level make this grade molten
The precipitant content relatively first order in liquid increases, and produces the level fractional precipitation relatively low compared with first order molecular weight, through the second level
Solution flow export flows out, and effluent is filtrated to get second fraction, and filtrate squeezes into this level through external pump；
Paragraphs below stage division is identical with this, from afterbody lower end flow export out be the level that molecular weight is minimum
Point, effluent filters after flowing out, and filtrate no longer pumps into afterbody.In classification process, open stirring motor, mixing speed control
System is between 50-120 rev/min so that the gutta-percha of precipitations at different levels can be uniformly dispersed, and does not deposits on dividing plates at different levels,
Open chuck refrigeration so that fractionation column forms step temperature difference, and lowermost temperature is at-10 DEG C to-20 DEG C, and upwards temperature is successively simultaneously
Improving, uppermost temperature is 5-10 DEG C of scope.
Use benzene, toluene, normal hexane, hexamethylene, gasoline, petroleum ether etc. nonpolar organic during general Gutta extraction
Solvent is as leaching agent, and extracting solution can be directly entered fractionation column and carry out classification, it is also possible to re-grading after being concentrated by extracting solution.For
Gutta-percha solid articles classification needs first to be dissolved into re-grading in above-mentioned non-polar organic solvent, non-polar organic solvent
Consumption use less, can dissolve completely, so can reduce precipitant consumption.Precipitant the having of low polarity in typically selecting
Machine solvent, such as methanol, ethanol or acetone etc., the last mixed solvent of precipitation fractionation can be separated by rectifying column, by non-
Polar solvent and precipitant are separately recovered, and recycle.
In classification process, it is necessary to according to gutta-percha concentration in non-polar solven, the polarity of precipitant controls often
The precipitant of one-level and the velocity ratio of gutta-percha solution, to obtain preferable grading effect, in general, first order precipitant is used
Measure the most slightly larger, at least make the part of its highest weight reach the polarity scope of critical precipitation, thus first order precipitant with
The velocity ratio of gutta-percha solution controls between 1:2 ~ 1:4, and later precipitant at different levels control with the velocity ratio of gutta-percha solution
Between 1:3 ~ 1:8.
Advantages of the present invention: by the multi-level hierarchical post of design, can be by certain speed at addition precipitant at different levels, continuously
Change the dissolubility of solvent, carry out gutta-percha, once through fractionation column, obtaining the fraction that various molecular weights is interval simultaneously, coordinating
In the thermograde that each inter-stage causes, improve separation efficiency, effectively reduce precipitant usage amount, accomplish that industrial scale is divided
Level.
Accompanying drawing illustrates:
Fig. 1 is the gutta-percha series classification apparatus structure schematic diagram that the present invention uses.
1, solution inlet 2, precipitant inlet 3, backflow entrance 4, interface 5, coolant jacket 6, solution flow export 7,
Porous barrier 8, agitating device
Detailed description of the invention:
Embodiment 1
The western Hunan is produced seed of bark of eucommia uses benzene as the extract of Extraction solvent as raw material, straight to the gutta-percha in extracting solution
Tapping into row classification, before classification, weight average molecular weight is 22.3 ten thousand, molecular weight distributing index 1.61, and extracting solution solvent is benzene.
Gutta-percha grading plant post is high 2.0 meters, diameter 25cm, is divided into level Four, the high about 50cm of every one-level, first order temperature control
System is at 10 DEG C, and the second level controls at 0 DEG C, and the third level controls at-5 DEG C, and fourth stage temperature controls at-15 DEG C, and temperature controls error
Within 2 DEG C；Starting stirring, stir speed (S.S.) controls at 50 ~ 60 revs/min
Gutta extraction liquid is pumped into from fractionation column upper entrance (1), flow velocity between 60 ~ 120 L/h, preferably 60 ~
Between 80 L/h, open the precipitant inlet (2) of the first order, pump into precipitation agent methanol, flow-control at 30 ~ 60 L/h, first
Level precipitation agent methanol is 1:2 with the velocity ratio of Gutta extraction liquid, and fractional precipitation gutta-percha out is through first order flow export
(6) flowing out, obtain first the highest fraction of molecular weight after filtering, filtrate is back to the first order through transport pump；
First order mixed liquor is through 1, and the filter cloth of 2 liang of inter-stages enters the second level, and it is 15 ~ 30 that the second level pumps into the flow velocity of methanol
L/h, i.e. second level precipitation agent methanol are 1:4 with the velocity ratio of Gutta extraction liquid, at second level dicyandiamide solution to gutta-percha
Dissolubility declines further, and precipitation fractionation gutta-percha float out flows out through second level flow export (6), obtains through filtering
The gutta-percha that molecular weight is more lower, filtrate is back to the second level through transport pump；The third level is similar with fourth stage operational approach,
It is 10 ~ 20 L/h that the third level and the fourth stage pump into the flow velocity of methanol.Fourth stage effluent filters after obtaining last fraction, filter
Liquid is no longer back to this level.One is the results are shown in Table after classification.
Molecular weight after classification and distribution thereof in table one embodiment 1
Embodiment 2
To the western Hunan produce Folium Eucommiae extract as raw material, the gutta-percha in extracting solution is directly carried out classification, classification
Front weight average molecular weight is 7.3 ten thousand, molecular weight distributing index 5.5, and extracting solution solvent is benzene.
Gutta-percha grading plant post is high 2.0 meters, diameter 25cm, is divided into level Four, the high about 50cm of every one-level, first order temperature control
System is at 10 DEG C, and the second level controls at 0 DEG C, and the third level controls at-5 DEG C, and fourth stage temperature controls at-15 DEG C, and temperature controls error
Within 2 DEG C；Starting stirring, stir speed (S.S.) controls at 60 ~ 80 revs/min
Gutta extraction liquid is pumped into from fractionation column upper entrance (1), flow velocity between 60 ~ 120 L/h, preferably 60 ~
Between 80 L/h, open the precipitant inlet (2) of the first order, pump into precipitation agent methanol, flow-control at 20 ~ 40 L/h, first
Level precipitation agent methanol is 1:3 with the velocity ratio of Gutta extraction liquid, and fractional precipitation gutta-percha out is through first order flow export
(6) flowing out, obtain first the highest fraction of molecular weight after filtering, filtrate is back to the first order through transport pump；
First order mixed liquor is through 1, and the filter cloth of 2 liang of inter-stages enters the second level, and it is 20 ~ 40 that the second level pumps into the flow velocity of methanol
L/h, i.e. second level precipitation agent methanol are 1:3 with the velocity ratio of Gutta extraction liquid, at second level dicyandiamide solution to gutta-percha
Dissolubility declines further, and precipitation fractionation gutta-percha float out flows out through second level flow export (6), obtains through filtering
The gutta-percha that molecular weight is more lower, filtrate is back to the second level through transport pump；The third level is similar with fourth stage operational approach,
It is 20 ~ 40 L/h that the third level and the fourth stage pump into the flow velocity of methanol.Fourth stage effluent filters after obtaining last fraction, filter
Liquid is no longer back to this level.One is the results are shown in Table after classification.
Molecular weight after classification and distribution thereof in table two embodiment 2
Embodiment 3
To the western Hunan produce eucommia bark extract as raw material, the gutta-percha in extracting solution is directly carried out classification, classification
Front weight average molecular weight is 193000, molecular weight distributing index 1.95.Extraction solvent is petroleum ether (boiling range 60 ~ 90 DEG C).
Gutta-percha grading plant post is high 2.0 meters, diameter 25cm, is divided into level Four, the high about 50cm of every one-level, first order temperature control
System is at 10 DEG C, and the second level controls at 0 DEG C, and the third level controls at-5 DEG C, and fourth stage temperature controls at-15 DEG C, and temperature controls error
Within 2 DEG C；Starting stirring, stir speed (S.S.) controls at 90 ~ 100 revs/min；Precipitant is ethanol.
Gutta extraction liquid is pumped into from fractionation column upper entrance (1), flow velocity between 60 ~ 120 L/h, preferably 60 ~
Between 80 L/h, open the precipitant inlet (2) of the first order, pump into precipitant ethanol alcohol, flow-control at 20 ~ 40 L/h, the
One-level precipitant ethanol is 1:3 with the velocity ratio of Gutta extraction liquid, and fractional precipitation gutta-percha out flows out through the first order
Mouth (6) flows out, and obtains first the highest fraction of molecular weight after filtering, and filtrate is back to the first order through transport pump.
First order mixed liquor is through 1, and the filter cloth of 2 liang of inter-stages enters the second level, and it is 10 ~ 20 that the second level pumps into the flow velocity of methanol
L/h, i.e. second level precipitant ethanol are 1:6 with the velocity ratio of Gutta extraction liquid, at second level dicyandiamide solution to gutta-percha
Dissolubility declines further, and precipitation fractionation gutta-percha float out flows out through second level flow export (6), obtains through filtering
The gutta-percha that molecular weight is more lower, filtrate is back to the second level through transport pump；The third level is similar with fourth stage operational approach,
It is 10 ~ 20 L/h that the third level and the fourth stage pump into the flow velocity of ethanol.Fourth stage effluent filters after obtaining last fraction, filter
Liquid is no longer back to this level.The results are shown in Table three after classification.
Molecular weight after classification and distribution thereof in table three embodiment 3
Thermograde and precipitant concentration gradient method are used in combination, are obtained by scalping operation multiple different interval
The method of the gutta-percha of molecular weight.
Claims (7)
1. a gutta-percha series classification post, it is characterised in that be divided into four sections inside post, one section is one-level, has porous between every section
Dividing plate (7) separates；Precipitant inlet (2) and backflow entrance (3) are arranged at every section of top, and every pars infrasegmentalis has solution after precipitation fractionation
Flow export (6)；Being with coolant jacket (5) outside fractionation column, coolant enters from coolant jacket (5) lower end；First order interface connects to be had
Air compression plant；Running through series connection agitating device (8) at different levels at fractionation column built with one, stirring power resources are in fractionation column
The motor of foot.
Gutta-percha series classification post the most according to claim 1, it is characterised in that porous barrier is covered with industrial filter cloth on (7)
Or industrial filter paper.
3. method gutta-percha being carried out series classification, is characterized in that unassorted to gutta-percha leaching liquid or gutta-percha
Crude product solution pumps into from the first order entrance (1) of the gutta-percha series classification post described in claim 1, and starts stirring motor guarantor
Hold moderate-speed mixer, after solution forms steady flow in each section of fractionation column, open precipitant inlet (2), by precipitant and the Cortex Eucommiae
The velocity ratio of sol solution is that 1:2 ~ 1:4 pumps into precipitant, and the fraction through precipitation fractionation flows out from the flow export (6) of this section, stream
Go out thing through being filtrated to get the fraction of gutta-percha middle-molecular-weihydroxyethyl highest part, filtrate through external pump from backflow entrance at different levels
(3) this level is squeezed into；Under pump pressure drives, the solution of the first order enters the second level by the dividing plate of industrial filter cloth, in the second level
The precipitant constantly injected makes this grade produce the level fractional precipitation relatively low compared with first order molecular weight, through the solution flow export of the second level
(6) flowing out, effluent is filtrated to get second fraction, and filtrate squeezes into this level through external pump；Paragraphs below stage division
Identical with this, from afterbody lower end flow export out be the fraction that molecular weight is minimum, effluent flow out after filter, filtrate is not
Pump into afterbody again；In classification process, open coolant jacket (5) so that the first order to afterbody forms 10 ~-20 DEG C
Thermograde.
The method that gutta-percha is carried out series classification the most according to claim 3, is characterized in that precipitant is methanol, ethanol
Or acetone.
The method that gutta-percha is carried out series classification the most according to claim 3, is characterized in that first order precipitant and Du
The velocity ratio of secondary sol solution is 1:2 ~ 1:4, the velocity ratio of later precipitant at different levels and gutta-percha solution control 1:3 ~ 1:8 it
Between.
The method that gutta-percha is carried out series classification the most according to claim 3, is characterized in that stirring motor speed of agitator
Control at 50 ~ 120 revs/min.
The method that gutta-percha is carried out series classification the most according to claim 3, is characterized in that making fractionation column form ladder
The temperature difference, lowermost temperature is at-10 DEG C to-20 DEG C, and upwards temperature improves successively, and uppermost temperature controls 5-10 DEG C of scope.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410775569.5A CN104558258B (en) | 2014-12-17 | 2014-12-17 | A kind of gutta-percha fractionation column and the method that gutta-percha is carried out series classification |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410775569.5A CN104558258B (en) | 2014-12-17 | 2014-12-17 | A kind of gutta-percha fractionation column and the method that gutta-percha is carried out series classification |
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| Publication Number | Publication Date |
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| CN104558258A CN104558258A (en) | 2015-04-29 |
| CN104558258B true CN104558258B (en) | 2016-08-24 |
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3242130A1 (en) * | 1982-11-13 | 1984-08-02 | Heinz Dipl.-Chem. 6082 Mörfelden Geerissen | Process for the continuous fractionation of polymers |
| DE4104573A1 (en) * | 1991-02-14 | 1992-08-20 | Pluss Stauffer Ag | METHOD AND DEVICE FOR TECHNICAL FRACTIONATION OF POLYMERS |
| CN101486777B (en) * | 2009-02-17 | 2010-12-29 | 天津大学 | Continuous precipitation grading plant and method for polymer |
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