CN104558258A - Eucommia ulmoide gum fractionation column and method for continuously fractionating eucommia ulmoide gum - Google Patents
Eucommia ulmoide gum fractionation column and method for continuously fractionating eucommia ulmoide gum Download PDFInfo
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- CN104558258A CN104558258A CN201410775569.5A CN201410775569A CN104558258A CN 104558258 A CN104558258 A CN 104558258A CN 201410775569 A CN201410775569 A CN 201410775569A CN 104558258 A CN104558258 A CN 104558258A
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Abstract
The invention relates to a eucommia ulmoide gum fractionation column and a method for continuously fractionating eucommia ulmoide gum. According to the method, four sections of fractionation columns are adopted, a precipitating agent can be added in each fractionation column at a certain speed, the solubility of a solvent is continuously changed, eucommia ulmoide gum passes through the fractionation columns at one time, fractions with multiple molecular weight ranges are simultaneously obtained; by combining temperature gradient generated among fractionations, the separation efficiency is increased, the usage amount of the precipitating agent is effectively decreased and the industrial-grade large-scale fractionation is achieved.
Description
Technical field
The invention belongs to gutta-percha production field, particularly a kind of gutta-percha fractionation column and gutta-percha is carried out to the method for series classification.
Background technology
The bark of eucommia (Eucommia ulmoides Olive), for the Eucommiaceae bark of eucommia belongs to deciduous tree, is the specific rare medicinal herbs seeds of China, is also the important glue source plant that subject range is the widest in the world, belongs to Chinese Second Class Key Protected Plant.The bark of eucommia, except containing except a large amount of medicinal ingredientss, also contains a large amount of gutta-percha in the tissues such as leaf, bark, seed.Gutta-percha belongs to rigid rubber, and by sulfide modifier or the blended and deep processing with other material, gutta-percha can develop series of new functional materials and Industrial materials, especially in rubber item, tire industry, has purposes widely.There are some researches show: gutta-percha and natural rubber blend composition are before reaching blending ratio 1:1, and tensile strength, tensile modulus, shore hardness, tensile yield have almost no change.Gutta-percha has more dynamic mechanical loss this excellent specific property low, is only 1/ 5 of cis-butadiene cement, 1/ 6 of natural rubber within the scope of use temperature.Its anti-flex performance is excellent, makes rubber item with it, and under repeated stress, material exothermic reduces, and extend work-ing life, this is at tire industry, industrial conveyor-line, and the rubber applications fields such as damping shock absorption part have huge potential application value.
All containing gutta-percha in Eucommia Fruit, bark and blade, wherein gutta-percha content in samara can reach 10% ~ 12%, gutta-percha content in bark 6% ~ 10%, blade gum content 1% ~ 3%, and the extraction of gutta-percha all can be extracted by the bark of eucommia each position raw material.Owing to having, Different Variation type, different times are plucked, the bark of eucommia of Different sources and different clones, and its gum content and gutta-percha characteristic all there are differences.Carry gluing method and have fermentation method, extraction and alkaline leaching and frozen glue method etc.Use different material, the gutta-percha that Different Extraction Method is extracted is in purity, average molecular weight range and be distributed with obvious difference, as gutta-percha middle-molecular-weihydroxyethyl scope from 10,000 to the highest close to 1,000,000, the section that the gutta-percha molecular weight of different sources is concentrated also has difference, this brings difficulty to the real application research of gutta-percha and industrialization, because the various mechanical property of polymkeric substance and its molecular weight and molecular weight distribution closely related, it is the important evidence determining its application performance and processing behavior, therefore to gutta-percha crude product, the Gutta extraction liquid even directly using solvent extraction to obtain carries out precipitation fractionation, the product obtaining various interval molecular weight is of practical significance.
The classification of polymkeric substance realizes according to the difference of polymkeric substance solubleness in its good solvent and poor solvent, usual low-molecular weight polymer part is relatively easily dissolved in a solvent, and high molecular weight moieties comparatively indissoluble solution, be generally add poor solvent in the good solvent of polymkeric substance, first high molecular weight moieties is first precipitated out.This process can be made repeatedly to reach better effects, but this technique is consuming time, it is large to consume quantity of solvent, and industrial to realize cost high, and organic volatilizable thing pollutes large, is not the method for economic environmental protection.
Wolf B A mentions the apparatus and method of Polymer Fractionation in patent DE3242130A1 and US5242594; Feng Yakai etc. improve above-mentioned Polymer Fractionation apparatus and method in patent CN 161486777 B, with the classification making it be applicable to urethane.The method of above-mentioned use has accomplished continuous operation, but polymkeric substance is once separated by fractionation column, finally can only obtain one containing higher molecular weight with the fraction of a lower molecular weight, if need further classification to high molecular or low-molecular weight polymer fraction, above-mentioned fraction is also needed to be realized by fractionation column classification again, add the consumption of precipitation agent, and equipment, place investment and operation easier.
Summary of the invention
The object of this invention is to provide a kind of gutta-percha fractionation column and use temperature gradient and precipitant concentration gradient and the method for series classification is carried out to gutta-percha.Method of the present invention is realized by gutta-percha series classification post, the topmost of fractionation column is gutta-percha leaching liquid or crude product gutta-percha solution inlet, and post inside is divided into four sections, and one section is one-level, porous barrier is had to separate between every section, upper berth industrial filter cloth or industrial filter paper; Precipitant inlet and phegma entrance are arranged at every section of top, and after every pars infrasegmentalis has precipitation fractionation, solution stream exports; Outside fractionation column, be with cooling jacket, cooling fluid enters from cooling jacket lower end; First step interface is connected with air compression plant, to provide the pressure needed for filtration; Run through series connection whipping appts at different levels at fractionation column built with one, stir power resources in the motor of fractionation column foot.
A kind of method of gutta-percha being carried out to series classification, that gutta-percha leaching liquid or the unassorted crude product solution of gutta-percha are pumped into from end entrance the fractionation column first step, pressurize in the first step, and start agitator motor maintenance moderate-speed mixer, after solution forms steady flow in each section of fractionation column, open precipitant inlet, precipitation agent is pumped into by suitable gutta-percha solution/precipitation agent velocity ratio, solution through precipitation fractionation flows out from the spout of this section, effluent obtains the fraction that gutta-percha middle-molecular-weihydroxyethyl highest portion is divided after filtration, filtrate squeezes into the corresponding levels through external pump from reflux inlet at different levels, under pressure-driven, the solution of the first step slow transits through the dividing plate laying industrial filter cloth and enters the second stage, the precipitation agent constantly slowly injected in the second stage make the precipitation agent content of solution at the corresponding levels comparatively the first step increase, produce the level fractional precipitation lower compared with first step molecular weight, solution stream outlet through the second stage is flowed out, effluent obtains second fraction through filtration, and filtrate squeezes into the corresponding levels through external pump,
Following section of stage division is identical therewith, from last step lower end spout out be the fraction that molecular weight is minimum, effluent liquid flow out after filter, filtrate no longer pumps into last step.In classification process, open agitator motor, stirring velocity controls between 50-120 rev/min, the gutta-percha of precipitation at different levels is can be uniformly dispersed, and does not deposit on dividing plate at different levels, open chuck refrigeration simultaneously, fractionation column is made to form step temperature difference, lowermost temperature is at-10 DEG C to-20 DEG C, and upwards temperature improves successively, and uppermost temperature is 5-10 DEG C of scope.
Use the non-polar organic solvents such as benzene, toluene, normal hexane, hexanaphthene, gasoline, sherwood oil as leaching agent in general Gutta extraction process, extracting solution directly can enter fractionation column and carry out classification, classification again after also extracting solution can being concentrated.Need first to be dissolved into classification again in above-mentioned non-polar organic solvent for the classification of gutta-percha solid articles, non-polar organic solvent consumption lacks use as far as possible, can dissolve completely, can reduce precipitation agent consumption like this.The organic solvent of precipitation agent low polarity in generally selecting, as methyl alcohol, ethanol or acetone etc., the last mixed solvent of precipitation fractionation can be separated by rectifying column, non-polar solvent and precipitation agent is reclaimed respectively, recycles.
In classification process, must according to the concentration of gutta-percha in non-polar solvent, the polarity of precipitation agent controls the precipitation agent of every one-level and the velocity ratio of gutta-percha solution, to obtain good grading effect, in general, first step precipitation agent consumption should be slightly larger, the part of its highest weight is at least made to reach the polarity scope of critical precipitation, so the velocity ratio of first step precipitation agent and gutta-percha solution controls between 1:2 ~ 1:4, the velocity ratio of later precipitation agent at different levels and gutta-percha solution controls between 1:3 ~ 1:8.
Advantage of the present invention: by the multi-level hierarchical post of design; precipitation agent can be added at different levels by certain speed; continuously change the solvability of solvent; carry out once through fractionation column to gutta-percha; obtain the fraction in various molecular weights interval simultaneously, be engaged in the thermograde that each inter-stage causes, improve separation efficiency; effective minimizing precipitation agent usage quantity, accomplishes industrial scale classification.
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, phegma entrance 4, interface 5, cooling jacket 6, solution stream outlet 7, porous barrier 8, whipping appts
embodiment:
Embodiment 1
Produce seed of bark of eucommia to the western Hunan and use benzene as the extract of Extraction solvent as raw material, directly carry out classification to the gutta-percha in extracting solution, 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 sorting equipment post is high 2.0 meters, and diameter 25cm, is divided into level Four, every one-level height about 50cm, and first step temperature controls at 10 DEG C, and the second stage controls at 0 DEG C, and the third stage controls at-5 DEG C, and fourth stage temperature controls at-15 DEG C, and temperature control error is within 2 DEG C; Start 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 is between 60 ~ 120 L/h, preferably between 60 ~ 80 L/h, open the precipitant inlet (2) of the first step, pump into precipitation agent methanol, flow control is at 30 ~ 60 L/h, the velocity ratio of first step precipitation agent methanol and Gutta extraction liquid is 1:2, fractionation precipitation gutta-percha out flows out through first step spout (6), and obtain first fraction that molecular weight is the highest after filtering, filtrate is back to the first step through pump delivery;
First step mixed solution is through 1, the filter cloth of 2 liang of inter-stages enters the second stage, the flow velocity that the second stage pumps into methyl alcohol is 15 ~ 30 L/h, namely the velocity ratio of second stage precipitation agent methanol and Gutta extraction liquid is 1:4, decline further in the solubleness of second stage solvent system to gutta-percha, precipitation fractionation gutta-percha suspended substance out flows out through second stage spout (6), and obtain the lower gutta-percha of molecular weight through filtering, filtrate is back to the second stage through pump delivery; The third stage and fourth stage working method similar, the flow velocity that the third stage and the fourth stage pump into methyl alcohol is 10 ~ 20 L/h.After fourth stage effluent liquid filters and obtains last fraction, filtrate is no longer back to this level.One is the results are shown in Table after classification.
Molecular weight in table one embodiment 1 after classification and distribution thereof
Embodiment 2
Produce the extract of Folium Eucommiae as raw material to the western Hunan, directly carry out classification to the gutta-percha in extracting solution, before classification, weight-average molecular weight is 7.3 ten thousand, molecular weight distributing index 5.5, and extracting solution solvent is benzene.
Gutta-percha sorting equipment post is high 2.0 meters, and diameter 25cm, is divided into level Four, every one-level height about 50cm, and first step temperature controls at 10 DEG C, and the second stage controls at 0 DEG C, and the third stage controls at-5 DEG C, and fourth stage temperature controls at-15 DEG C, and temperature control error is within 2 DEG C; Start 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 is between 60 ~ 120 L/h, preferably between 60 ~ 80 L/h, open the precipitant inlet (2) of the first step, pump into precipitation agent methanol, flow control is at 20 ~ 40 L/h, the velocity ratio of first step precipitation agent methanol and Gutta extraction liquid is 1:3, fractionation precipitation gutta-percha out flows out through first step spout (6), and obtain first fraction that molecular weight is the highest after filtering, filtrate is back to the first step through pump delivery;
First step mixed solution is through 1, the filter cloth of 2 liang of inter-stages enters the second stage, the flow velocity that the second stage pumps into methyl alcohol is 20 ~ 40 L/h, namely the velocity ratio of second stage precipitation agent methanol and Gutta extraction liquid is 1:3, decline further in the solubleness of second stage solvent system to gutta-percha, precipitation fractionation gutta-percha suspended substance out flows out through second stage spout (6), and obtain the lower gutta-percha of molecular weight through filtering, filtrate is back to the second stage through pump delivery; The third stage and fourth stage working method similar, the flow velocity that the third stage and the fourth stage pump into methyl alcohol is 20 ~ 40 L/h.After fourth stage effluent liquid filters and obtains last fraction, filtrate is no longer back to this level.One is the results are shown in Table after classification.
Molecular weight in table two embodiment 2 after classification and distribution thereof
Embodiment 3
Produce the extract of eucommia bark as raw material to the western Hunan, directly carry out classification to the gutta-percha in extracting solution, before classification, weight-average molecular weight is 193000, molecular weight distributing index 1.95.Extraction solvent is sherwood oil (boiling range 60 ~ 90 DEG C).
Gutta-percha sorting equipment post is high 2.0 meters, and diameter 25cm, is divided into level Four, every one-level height about 50cm, and first step temperature controls at 10 DEG C, and the second stage controls at 0 DEG C, and the third stage controls at-5 DEG C, and fourth stage temperature controls at-15 DEG C, and temperature control error is within 2 DEG C; Start stirring, stir speed (S.S.) controls at 90 ~ 100 revs/min; Precipitation agent is ethanol.
Gutta extraction liquid is pumped into from fractionation column upper entrance (1), flow velocity is between 60 ~ 120 L/h, preferably between 60 ~ 80 L/h, open the precipitant inlet (2) of the first step, pump into precipitation agent ethanol alcohol, flow control is at 20 ~ 40 L/h, the velocity ratio of first step precipitation agent ethanol and Gutta extraction liquid is 1:3, fractionation precipitation gutta-percha out flows out through first step spout (6), obtain first fraction that molecular weight is the highest after filtering, filtrate is back to the first step through pump delivery.
First step mixed solution is through 1, the filter cloth of 2 liang of inter-stages enters the second stage, the flow velocity that the second stage pumps into methyl alcohol is 10 ~ 20 L/h, namely the velocity ratio of second stage precipitation agent ethanol and Gutta extraction liquid is 1:6, decline further in the solubleness of second stage solvent system to gutta-percha, precipitation fractionation gutta-percha suspended substance out flows out through second stage spout (6), and obtain the lower gutta-percha of molecular weight through filtering, filtrate is back to the second stage through pump delivery; The third stage and fourth stage working method similar, the flow velocity that the third stage and the fourth stage pump into ethanol is 10 ~ 20 L/h.After fourth stage effluent liquid filters and obtains last fraction, filtrate is no longer back to this level.The results are shown in Table three after classification.
Molecular weight in table three embodiment 3 after classification and distribution thereof
Conbined usage thermograde and precipitant concentration gradient method, obtain the method for the gutta-percha of the interval molecular weight of multiple difference by scalping operation.
Claims (7)
1. a gutta-percha series classification post, is characterized in that post inside is divided into four sections, and one section is one-level, has porous barrier (7) to separate between every section; Precipitant inlet (2) and phegma entrance (3) are arranged at every section of top, and after every pars infrasegmentalis has precipitation fractionation, solution stream exports (6); Outside fractionation column, be with cooling jacket (5), cooling fluid enters from cooling jacket (5) lower end; First step interface is connected with air compression plant; Run through series connection whipping appts (8) at different levels at fractionation column built with one, stir power resources in the motor of fractionation column foot.
2. gutta-percha series classification post according to claim 1, is characterized in that porous barrier (7) is covered with industrial filter cloth or industrial filter paper.
3. one kind is carried out the method for series classification to gutta-percha, gutta-percha leaching liquid or the unassorted crude product solution of gutta-percha is it is characterized in that to pump into from above-mentioned fractionation column first step entrance (1), and start agitator motor maintenance moderate-speed mixer, after solution forms steady flow in each section of fractionation column, open precipitant inlet (2), precipitation agent is pumped into by suitable gutta-percha solution/precipitation agent velocity ratio, fraction through precipitation fractionation flows out from the spout (6) of this section, effluent obtains the fraction that gutta-percha middle-molecular-weihydroxyethyl highest portion is divided after filtration, filtrate squeezes into the corresponding levels through external pump from reflux inlet (3) at different levels, under pumping pressure drives, the solution of the first step enters the second stage by the dividing plate of industrial filter cloth, the level fractional precipitation that the precipitation agent constantly injected in the second stage makes generation at the corresponding levels lower compared with first step molecular weight, solution stream through the second stage exports (6) and flows out, effluent obtains second fraction through filtration, and filtrate squeezes into the corresponding levels through external pump, following section of stage division is identical therewith, from last step lower end spout out be the fraction that molecular weight is minimum, effluent liquid flow out after filter, filtrate no longer pumps into last step, in classification process, open cooling jacket (5), make the first step arrive the thermograde of last step formation 10 ~-20 DEG C.
4. method of gutta-percha being carried out to series classification according to claim 3, is characterized in that precipitation agent is methyl alcohol, ethanol or acetone.
5. method of gutta-percha being carried out to series classification according to claim 3, it is characterized in that the velocity ratio of first step precipitation agent and gutta-percha solution is 1:2 ~ 1:4, the velocity ratio of later precipitation agent at different levels and gutta-percha solution controls between 1:3 ~ 1:8.
6. method of gutta-percha being carried out to series classification according to claim 3, is characterized in that agitator motor mixing speed controls at 50 ~ 120 revs/min.
7. method of gutta-percha being carried out to series classification according to claim 3, it is characterized in that making fractionation column form step 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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Citations (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 |
| US5242594A (en) * | 1991-02-14 | 1993-09-07 | Pluess-Staufer Ag | Process and apparatus for industrial fractionation of polymers |
| CN101486777A (en) * | 2009-02-17 | 2009-07-22 | 天津大学 | Continuous precipitation grading plant and method for polymer |
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- 2014-12-17 CN CN201410775569.5A patent/CN104558258B/en not_active Expired - Fee Related
Patent Citations (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 |
| US5242594A (en) * | 1991-02-14 | 1993-09-07 | Pluess-Staufer Ag | Process and apparatus for industrial fractionation of polymers |
| CN101486777A (en) * | 2009-02-17 | 2009-07-22 | 天津大学 | Continuous precipitation grading plant and method for polymer |
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