CN107987186A - A kind of purifying process of the thick glue of the bark of eucommia - Google Patents
A kind of purifying process of the thick glue of the bark of eucommia Download PDFInfo
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- CN107987186A CN107987186A CN201810084401.8A CN201810084401A CN107987186A CN 107987186 A CN107987186 A CN 107987186A CN 201810084401 A CN201810084401 A CN 201810084401A CN 107987186 A CN107987186 A CN 107987186A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08C—TREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
- C08C2/00—Treatment of rubber solutions
- C08C2/06—Wining of rubber from solutions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08C—TREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
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- C08C2/02—Purification
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Abstract
The invention belongs to natural rubber technical field of purification, and in particular to a kind of purifying process of the thick glue of the bark of eucommia.The purifying process of the thick glue of the bark of eucommia, including following steps：（1）Thick peptization solution：Add solvent and dissolve thick glue；（2）It is refined：Flotation agent processing is added in by dissolved thick glue；（3）Cohesion：To step（2）In glue concentration, cooling and crystallization；（4）Dry and post processing：To step（3）In gutta-percha particle heating, dry, obtain finished product eucommia ulmoides refined glue.The thick blob of viscose of the bark of eucommia is handled by using dissolving, refined, cohesion and drying process, specifically the thick glue of the bark of eucommia is dissolved using specific solvent, then flotation agent is added to be refined to obtain the bark of eucommia glue of high-purity, then cohesion and drying process are passed through again, the eucommia ulmoides refined glue obtained, for its extraction rate reached to 99% or so, purity is 99% or so.
Description
Technical field
The invention belongs to natural rubber technical field of purification, and in particular to a kind of purifying process of the thick glue of the bark of eucommia.
Background technology
Exist on the purifying of gutta-percha, Xie Juanping, Li Wei et al.《Ankang University's journal》The 6th phase of volume 25 in December, 2013 delivers
's《The extraction of Eucommia ulmoides leaf glue and purifying research》Disclosed in one text：
Double bond in gutta-percha molecular structure is with certain polarity, the indissoluble in the organic solvent of extremely strong property and low polarity
Solution, and in the solvent chloroform of low polarity, petroleum ether, have the solubility in the benzene class equal solvent of double bond higher.But shut out in folium cortex eucommiae
Secondary glue comparision contents are low, and solvent-oil ratio is big during extraction, and pollution environment is serious, thus cannot be extensively using chloroform, petroleum ether etc.
Solvent, gasoline is a kind of common organic solvent, cheap and easy to get, is widely used in industry, therefore uses experiment of single factor, with second
Alcohol, petroleum ether, gasoline are solvent purification, select the best solvent of gutta-percha purification effect.
Purifying comprises the concrete steps that：The sample of drying is put into beaker, adds suitable petroleum ether, in 75 DEG C of water-baths
When middle extraction 2 is small, filters, extract 3 times, merging filtrate while hot, in -12 DEG C of refrigerators freezing place to there is white Filamentous precipitation,
Filtering, up to thick glue.Methanol rinses, up to smart glue.
By single factor test and experiment of many factor, it was therefore concluded that：Using petroleum ether as solvent, recovery rate highest；Gasoline takes second place,
It is not much different with the recovery rate of petroleum ether, during using ethanol as solvent, the recovery rate of gutta-percha is minimum, but the bark of eucommia of petroleum ether extraction
Glue is easy to purify than more loose, and the gutta-percha that using gasoline as solvent when extracts is relatively glutinous is unfavorable for purifying, and experiment proves Du
Secondary glue is soluble in the petroleum ether of heat, and solubility in ethanol is minimum.Maximum recovery rate is 2.17%.
Adopt and gutta-percha is purified with the aforedescribed process, the recovery rate of gutta-percha maximum is only 2.17%, its recovery rate
Still it is not high, and this low recovery rate limits the extensive use of gutta-percha.It is the bottleneck of gutta-percha large-scale production, therefore,
Need to be improved for above-mentioned method, design one kind can greatly improve Gutta extraction rate so that gutta-percha is extensive
Its input that is produced as widely use the purification process prepared.
The content of the invention
In order to solve above-mentioned technical problem, the present invention provides a kind of thick glue purification technique of the high bark of eucommia of recovery rate.
The purifying process of the thick glue of the bark of eucommia provided by the present invention, including following steps：
（1）Thick peptization solution：Add solvent and dissolve thick glue；
（2）It is refined：Flotation agent processing is added in by dissolved thick glue；
（3）Cohesion：To step（2）In glue concentration, cooling and crystallization；
（4）Dry and post processing：To step（3）In gutta-percha particle heating, dry, obtain finished product eucommia ulmoides refined glue.
Preferably, the thick glue of the bark of eucommia is the thick glue obtained by raw material of Folium Eucommiae or is obtained by raw material of eucommia bark thick
Glue.
It is furthermore preferred that the thick glue of the bark of eucommia is to digest the thick glue that folium cortex eucommiae or/and eucommia bark obtain with biological enzyme.The present invention
The thick glue of the bark of eucommia being applicable in, is not limited to the thick glue of the bark of eucommia obtained using specific biology enzyme enzymolysis, as long as all can make the bark of eucommia
Leaf or eucommia bark argillization, the thick glue product containing gutta-percha for disintegrating and smoothly digesting acquisition, the guarantor in the present invention
Within the scope of shield, i.e., located using the thick glue of abiotic enzymic degradation acquisition, the same technique for being also applied for the present invention to purify
Reason, such replacement are also fallen within the scope and spirit of the invention.
Preferably, step（1）In, the thick glue of the bark of eucommia and antioxidant are added in dissolution kettle, adds solvent, heats thing
Material, dissolves, and filtering, obtains the thick sol solution of the bark of eucommia.
In solvent at least containing carbon atom number be 5-30 compound, and the compound include neopentane, n-hexane,
Any of hexamethylene, petroleum ether, benzene and benzene homologues.
Preferably, step（2）In, in step（1）Flotation agent is added in the thick sol solution of the bark of eucommia of gained, heats and stirs,
Sedimentation.
Contain acrylic acid and acrylamide copolymer in flotation agent.
Step（3）In, the temperature of glue concentration is 60-80 DEG C, and vacuum is -0.95- -0.98MPa during concentration.
Step（4）In, dry under vacuum, drying temperature is less than or equal to 90 DEG C.
More specifically, technique of the invention includes following steps：
Dissolving：
（1）In dissolution kettle, solvent is added, then adds the thick glue of the bark of eucommia and antioxidant, opens stirring；In the solvent at least
Containing a kind of carbon atom number be 5-30 compound, the compound include neopentane, n-hexane, hexamethylene, petroleum ether,
Any of benzene and benzene homologues；
（2）Heating stepses（1）In material reach 50-90 DEG C, when dissolving 2-8 is small；
（3）The thick sol solution of the bark of eucommia is obtained after coarse filtration, refined filtration double-filtration successively；
It is refined：
（4）Flotation agent is added in the thick glue of the bark of eucommia by dissolving；The addition of flotation agent is the weight of the thick glue of the bark of eucommia
0.01-0.1%；
（5）Heating makes step（4）The temperature of middle material is maintained at 60-70 DEG C, and stirs, speed of agitator 300-500rpm；
（6）After when stirring 1-3 is small, when sedimentation 3-8 is small, the glue after must refining；
Cohesion：
（7）Glue after will be refined adds concentration kettle, stirs and is heated to 60-80 DEG C, mixing speed 100-150rpm, vacuum
Partial solvent is steamed under degree -0.95-0.98MPa；
（8）Cooling：Glue after concentration enters the kettle that cools down, and opens stirring, mixing speed 100-150rpm, and addition accounts for refined rear glue
The dispersant of liquid gross weight 0.01-0.1%, 6-10 DEG C of cooling rate/h, glue enters crystallization kettle after being cooled to 24-27 DEG C；
（9）Crystallization：Glue stirs in crystallization kettle, progressively cools down, and mixing speed 50rpm, 5-7 DEG C of cooling velocity/h, is cooled to
0 DEG C of cooling temperature, gutta-percha is separated out from solvent；Particle solution after cohesion is filtered by centrifuge；
It is dry：
（10）The gutta-percha particle heating produced to cohesion process, dry removing solvent, obtains eucommia ulmoides refined glue under vacuum.
The beneficial effects of the present invention are carry out the thick blob of viscose of the bark of eucommia by using dissolving, refined, cohesion and drying process
Processing, is specifically dissolved the thick glue of the bark of eucommia using specific solvent, and then addition flotation agent is refined high-purity to obtain
The bark of eucommia glue of degree, then again by cohesion and drying process, the eucommia ulmoides refined glue obtained, its extraction rate reached to 99% or so,
Purity is 99% or so.
Embodiment
The present invention is further described with reference to specific embodiment, so that those skilled in the art knows more about
The present invention, but be not intended to limit the present invention.
Embodiment 1
The thick glue purification of the bark of eucommia obtains the technique of eucommia ulmoides refined glue, including following steps：
Dissolving：
（1）In dissolution kettle, solvent pentane is added, then adds the thick glue of the bark of eucommia and antioxidant BHT（Bis- tertiary fourths of 2,6-
Base -4- methylphenols）, open agitating device；
The mass ratio of the thick glue of the bark of eucommia and pentane is 1：12；Antioxidant is BHT, its dosage is the 0.3% of the thick glue weight of the bark of eucommia；
（2）Using chuck heating stepses（1）In material reach 70 DEG C, when dissolving 5 is small, mixing speed is during dissolving
150rpm or so；
（3）Successively the thick sol solution of the bark of eucommia is obtained after 200 mesh coarse filtration, 1000 mesh refined filtration double-filtrations；
（4）Filter residue repeats dissolving 3 times, repeat step（1）-（3）Course of dissolution（The weight ratio of filter residue and pentane is 1：
12）；
It is refined：
（5）It will be sent into purification kettle by the thick glue glue of the bark of eucommia dissolved, then add in the thick glue glue of the bark of eucommia by dissolving
Enter flotation agent；Flotation agent is specially acrylic acid and acrylamide copolymer and the mixture of glycerine；Acrylic acid and acrylamide
The weight ratio of copolymer and glycerine is 2：1；The addition of whole flotation agent is the 0.05% of the weight of the thick glue glue of the bark of eucommia；
（6）Using the method for chuck heating to step（5）In purification kettle in material heat, hot water temperature's control in chuck
System is at 85 DEG C or so, rate-determining steps（5）The temperature of middle material is maintained at 65 DEG C or so, and stirs, speed of agitator 400rpm；
（7）Stir 12 it is small when after, when sedimentation 5 is small, then will contain impurity, flotation agent part and be separated from bottom, the clean glue in top
Optionally repetitive decontamination is several times for liquid；
Cohesion：
（8）Concentration：Glue after will be refined adds concentration kettle, opens and stirs and be heated to 70 DEG C or so of heating-up temperature, stirring speed
130rpm is spent, steams partial solvent under vacuum -0.95--0.98MPa, condensation recycling design removes dissolution process；
（9）Cooling：Glue after concentration enters cooling kettle, opens stirring, mixing speed 130rpm, adds dividing for 0.01-0.1%
Powder, dispersant are calcium stearate, and 8 DEG C/h of cooling rate, glue enters crystallization kettle after being cooled to 25 DEG C；
（10）Crystallization：Glue is in crystallization kettle, under stirring state, progressively cools down, mixing speed 50rpm, 6 DEG C/h of cooling velocity,
0 DEG C or so of cooling temperature is cooled to, gutta-percha is progressively separated out from solvent；Particle solution after cohesion is filtered through centrifuge；
It is dry：
（11）The gutta-percha particle containing 15% or so solvent that cohesion process is produced, into double-cone dryer, 60 DEG C of temperature,
Vacuum -0.95 under the conditions of -0.98MPa it is dry 4 it is small when, product volatile matter<0.5%.
Solvent condensation recycling, dried micelle enters screw elevator or fluidized bed drying case is aeration-cooling to room
Temperature.Automatically weigh, pack, obtain finished product eucommia ulmoides refined glue.
Embodiment 2
The thick glue purification of the bark of eucommia obtains the technique of eucommia ulmoides refined glue, including following steps：
Dissolving：
（1）In dissolution kettle, solvent 2- methybutanes are added, then add the thick glue of the bark of eucommia and antioxidant, open stirring；
The mass ratio of the thick glue of the bark of eucommia and 2- methybutanes is 1：10；Antioxidant is WH1520A（2- n-octylthiomethylene -4,
6- DI-tert-butylphenol compounds）, its dosage is the 0.3% of the thick glue weight of the bark of eucommia；
（2）Using chuck heating stepses（1）In material reach 70 DEG C, when dissolving 5 is small, mixing speed is during dissolving
150rpm or so；
（3）The thick sol solution of the bark of eucommia is obtained after coarse filtration, refined filtration double-filtration；Cross 200 mesh during coarse filtration, when refined filtration crosses 1000 mesh；
（4）Filter residue repeats to dissolve 3 times, and the weight ratio of filter residue and 2- methybutanes is 1：10；
It is refined：
（5）It will be sent into purification kettle by the thick glue glue of the bark of eucommia dissolved, then add in the thick glue glue of the bark of eucommia by dissolving
Enter flotation agent；Flotation agent is specially the mixture of acrylic acid and acrylamide copolymer and acetic acid butanediol ester；Acrylic acid and third
The weight ratio of acrylamide copolymer and acetic acid butanediol ester is 2：1；The addition of whole flotation agent is the weight of the thick glue glue of the bark of eucommia
The 0.03% of amount；
（6）Using the method for chuck heating to step（5）In purification kettle in material heat, hot water temperature's control in chuck
System is at 80 DEG C, rate-determining steps（5）The temperature of middle material is maintained at 60 DEG C, and stirs, speed of agitator 300rpm；
（7）Stir 1.5 it is small when after, when sedimentation 4 is small, then will contain impurity, flotation agent part and be separated from bottom.Glue after refined
Liquid carries out treating agglomeration process process into glue storage tank.
Cohesion：
（8）Concentration：Glue after will be refined adds concentration kettle, opens and stirs and be heated to 70 DEG C of heating-up temperature, mixing speed
130rpm, steams partial solvent under vacuum -0.95 to -0.98MPa, and condensation recycling design removes dissolution process；
（9）Cooling：Glue after concentration enters cooling kettle, opens stirring, mixing speed 130rpm, adds dividing for 0.01-0.1%
Powder, dispersant are calcium stearate, and 8 DEG C/h of cooling rate, glue enters crystallization kettle after being cooled to 25 DEG C；
（10）Crystallization：Glue is in crystallization kettle, under stirring state, progressively cools down, mixing speed 50rpm, 6 DEG C/h of cooling velocity,
0 DEG C or so of cooling temperature is cooled to, gutta-percha is progressively separated out from solvent；Particle solution after cohesion is filtered through centrifuge；
It is dry：
（11）The gutta-percha particle containing 15% or so solvent that cohesion process is produced, into double-cone dryer, 60 DEG C of temperature,
Vacuum -0.95 is to when dry 3-6 is small under the conditions of -0.98MPa, product volatile matter<0.5%.Solvent condensation recycling, it is dry
Micelle afterwards enters screw elevator or fluidized bed drying case is aeration-cooling to room temperature.Automatically weigh, pack, obtain finished product bark of eucommia essence
Glue.
Embodiment 3
The thick glue purification of the bark of eucommia obtains the technique of eucommia ulmoides refined glue, including following steps：
Dissolving：
（1）In dissolution kettle, solvent octane is added, then adds the thick glue of the bark of eucommia and antioxidant, opens stirring；The thick glue of the bark of eucommia
Mass ratio with octane is 1：10；Antioxidant is BHT, its dosage is the 0.3% of the thick glue weight of the bark of eucommia；
（2）Using chuck heating stepses（1）In material reach 75 DEG C, when dissolving 5 is small, mixing speed is during dissolving
150rpm or so；
（3）The thick sol solution of the bark of eucommia is obtained after coarse filtration, refined filtration double-filtration；Cross 200 mesh during coarse filtration, when refined filtration crosses 1000 mesh；
（4）Filter residue repeats to dissolve 3 times, and the weight ratio of filter residue and octane is 1：10.
It is refined：
The technique that the thick glue of the bark of eucommia refines, including following steps：
（5）It will be sent into purification kettle by the thick glue glue of the bark of eucommia dissolved, then add in the thick glue glue of the bark of eucommia by dissolving
Enter flotation agent；Flotation agent is specially acrylic acid and acrylamide copolymer and glycerine, the mixture of acetic acid butanediol ester；Propylene
The weight ratio of acid and acrylamide copolymer and glycerine, acetic acid butanediol ester is 2：0.5：0.5；The addition of whole flotation agent
For the 0.03% of the weight of the thick glue glue of the bark of eucommia；
（6）Using the method for chuck heating to step（5）In purification kettle in material heat, hot water temperature's control in chuck
System is at 80 DEG C, rate-determining steps（5）The temperature of middle material is maintained at 60 DEG C, and stirs, speed of agitator 300rpm；
（7）Stir 1.5 it is small when after, when sedimentation 4 is small, then will contain impurity, flotation agent part and be separated from bottom, the clean glue in top
Optionally repetitive decontamination is several times for liquid；
Cohesion：
（8）Concentration：Glue after will be refined adds concentration kettle, opens and stirs and be heated to 70 DEG C of heating-up temperature, mixing speed
130rpm, steams partial solvent under vacuum -0.95 to -0.98MPa, and condensation recycling design removes dissolution process；
（9）Cooling：Glue after concentration enters cooling kettle, opens stirring, mixing speed 130rpm, adds dividing for 0.01-0.1%
Powder, dispersant are calcium stearate, and 8 DEG C/h of cooling rate, glue enters crystallization kettle after being cooled to 25 DEG C；
（10）Crystallization：Glue is in crystallization kettle, under stirring state, progressively cools down, mixing speed 50rpm, 6 DEG C/h of cooling velocity,
0 DEG C or so of cooling temperature is cooled to, gutta-percha is progressively separated out from solvent；Particle solution after cohesion is filtered through centrifuge；
It is dry：
（11）The gutta-percha particle containing 15% or so solvent that cohesion process is produced, into double-cone dryer, 60 DEG C of temperature,
Vacuum -0.95 is to when dry 3-6 is small under the conditions of -0.98MPa, product volatile matter<0.5%.Solvent condensation recycling, it is dry
Micelle afterwards enters screw elevator or fluidized bed drying case is aeration-cooling to room temperature.Automatically weigh, pack, obtain finished product bark of eucommia essence
Glue.
Embodiment 4
The thick glue purification of the bark of eucommia obtains the technique of eucommia ulmoides refined glue, including following steps：
Dissolving：
（1）In dissolution kettle, solvent n-heptane is added, then adds the thick glue of the bark of eucommia and antioxidant, opens stirring；The bark of eucommia is thick
The mass ratio of glue and normal heptane is 1：10；Antioxidant is BHT, its dosage is the 0.8% of the thick glue weight of the bark of eucommia；
（2）Using chuck heating stepses（1）In material reach 75 DEG C, when dissolving 5 is small, mixing speed is during dissolving
200rpm；
（3）The thick sol solution of the bark of eucommia is obtained after coarse filtration, refined filtration double-filtration；Cross 200 mesh during coarse filtration, when refined filtration crosses 1000 mesh；
（4）Filter residue repeats to dissolve 3 times, and the weight ratio of filter residue and normal heptane is 1：10.
It is refined：
（5）It will be sent into purification kettle by the thick glue glue of the bark of eucommia dissolved, then add in the thick glue glue of the bark of eucommia by dissolving
Enter flotation agent；Flotation agent is specially the mixture of acrylic acid and acrylamide copolymer and acetic acid butanediol ester；Acrylic acid and third
The weight ratio of acrylamide copolymer and acetic acid butanediol ester is 2：1；The addition of whole flotation agent is the weight of the thick glue glue of the bark of eucommia
The 0.03% of amount；
（6）Using the method for chuck heating to step（5）In purification kettle in material heat, hot water temperature's control in chuck
System is at 80 DEG C, rate-determining steps（5）The temperature of middle material is maintained at 60 DEG C, and stirs, speed of agitator 300rpm；
（7）Stir 1.5 it is small when after, when sedimentation 4 is small, then will contain impurity, flotation agent part and be separated from bottom；
Cohesion：
（8）Concentration：Glue after will be refined adds concentration kettle, opens and stirs and be heated to 70 DEG C of heating-up temperature, mixing speed
130rpm, steams partial solvent under vacuum -0.95 to -0.98MPa, and condensation recycling design removes dissolution process；
（9）Cooling：Glue after concentration enters cooling kettle, opens stirring, mixing speed 130rpm, adds dividing for 0.01-0.1%
Powder, dispersant are calcium stearate, and 8 DEG C/h of cooling rate, glue enters crystallization kettle after being cooled to 25 DEG C；
（10）Crystallization：Glue is in crystallization kettle, under stirring state, progressively cools down, mixing speed 50rpm, 6 DEG C/h of cooling velocity,
0 DEG C or so of cooling temperature is cooled to, gutta-percha is progressively separated out from solvent；Particle solution after cohesion is filtered through centrifuge；
It is dry：
（11）The gutta-percha particle containing 15% or so solvent that cohesion process is produced, into double-cone dryer, 60 DEG C of temperature,
Vacuum -0.95 is to when dry 3-6 is small under the conditions of -0.98MPa, product volatile matter<0.5%.Solvent condensation recycling, it is dry
Micelle afterwards enters screw elevator or fluidized bed drying case is aeration-cooling to room temperature.Automatically weigh, pack, obtain finished product bark of eucommia essence
Glue.
The detection method of finished product eucommia ulmoides refined glue obtained in embodiment 1-4, its recovery rate and purity is as follows：
Contained gutta-percha × 100% in the weight of the eucommia ulmoides refined glue of recovery rate %=acquisition/bark of eucommia glue；
In purity %=products obtained therefrom in the thick glue of eucommia ulmoides refined glue/bark of eucommia total gutta-percha content × 100%；
Specific detection method is as follows：With reference to gel content analysis method in butadiene rubber< SH/T1050-1991》；
By calculating, the recovery rate and purity of the eucommia ulmoides refined glue in embodiment 1-4 are as shown in the table：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Recovery rate % | 99.05 | 99.32 | 99.13 | 99.19 |
| Purity % | 99.24 | 99.11 | 99.27 | 99.26 |
The technique that can be seen that the present invention from the data in above table handles the thick glue of the bark of eucommia, its recovery rate and purity
Reach more than 99%, relative to the technique provided in documents 1, the present invention has significant progress, thick for the bark of eucommia
The production and application of the large-scale of glue provide technical support.
Claims (10)
1. the purifying process of the thick glue of the bark of eucommia, including following steps：
（1）Thick peptization solution：Add solvent and dissolve thick glue；
（2）It is refined：Flotation agent processing is added in by dissolved thick glue；
（3）Cohesion：To step（2）In glue concentration, cooling and crystallization；
（4）Dry and post processing：To step（3）In gutta-percha particle heating, dry, obtain finished product eucommia ulmoides refined glue.
2. the purifying process of the thick glue of the bark of eucommia as claimed in claim 1, it is characterised in that the thick glue of the bark of eucommia is using Folium Eucommiae as original
Expect the thick glue obtained or the thick glue obtained using eucommia bark as raw material.
3. the purifying process of the thick glue of the bark of eucommia as claimed in claim 1, it is characterised in that the thick glue of the bark of eucommia is to be digested with biological enzyme
The thick glue that folium cortex eucommiae or/and eucommia bark obtain.
4. the purifying process of the thick glue of the bark of eucommia as claimed in claim 1, it is characterised in that step（1）In, added in dissolution kettle
The thick glue of the bark of eucommia and antioxidant, add solvent, and heated material, dissolves, and filtering, obtains the thick sol solution of the bark of eucommia.
5. the purifying process of the thick glue of the bark of eucommia as claimed in claim 4, it is characterised in that at least contain carbon atom number in solvent
For the compound of 5-30, and the compound does not include appointing in neopentane, n-hexane, hexamethylene, petroleum ether, benzene and benzene homologues
It is a kind of.
6. the purifying process of the thick glue of the bark of eucommia as claimed in claim 1, it is characterised in that step（2）In, in step（1）Gained
The thick sol solution of the bark of eucommia in add flotation agent, heat and stir, settle.
7. the purifying process of the thick glue of the bark of eucommia as claimed in claim 6, it is characterised in that contain acrylic acid and propylene in flotation agent
Amide copolymer.
8. the purifying process of the thick glue of the bark of eucommia as claimed in claim 1, it is characterised in that step（3）In, the temperature of glue concentration
For 60-80 DEG C, vacuum is -0.95- -0.98MPa during concentration.
9. the purifying process of the thick glue of the bark of eucommia as claimed in claim 1, it is characterised in that step（4）In, it is dry under vacuum, do
Dry temperature is less than or equal to 90 DEG C.
10. the purifying process of the thick glue of the bark of eucommia as claimed in claim 1, it is characterised in that including following steps：
Dissolving：
（1）In dissolution kettle, solvent is added, then adds the thick glue of the bark of eucommia and antioxidant, opens stirring；In the solvent at least
Containing a kind of carbon atom number be 5-30 compound, the compound include neopentane, n-hexane, hexamethylene, petroleum ether,
Any of benzene and benzene homologues；
（2）Heating stepses（1）In material reach 50-90 DEG C, when dissolving 2-8 is small；
（3）The thick sol solution of the bark of eucommia is obtained after coarse filtration, refined filtration double-filtration successively；
It is refined：
（4）Flotation agent is added in the thick glue of the bark of eucommia by dissolving；The addition of flotation agent is the weight of the thick glue of the bark of eucommia
0.01-0.1%；
（5）Heating makes step（4）The temperature of middle material is maintained at 60-70 DEG C, and stirs, speed of agitator 300-500rpm；
（6）After when stirring 1-3 is small, when sedimentation 3-8 is small, the glue after must refining；
Cohesion：
（7）Glue after will be refined adds concentration kettle, stirs and is heated to 60-80 DEG C, mixing speed 100-150rpm, vacuum
Partial solvent is steamed under degree -0.95-0.98MPa；
（8）Cooling：Glue after concentration enters the kettle that cools down, and opens stirring, mixing speed 100-150rpm, and addition accounts for refined rear glue
The dispersant of liquid gross weight 0.01-0.1%, 6-10 DEG C of cooling rate/h, glue enters crystallization kettle after being cooled to 24-27 DEG C；
（9）Crystallization：Glue stirs in crystallization kettle, progressively cools down, and mixing speed 50rpm, 5-7 DEG C of cooling velocity/h, is cooled to
0 DEG C of cooling temperature, gutta-percha is separated out from solvent；Particle solution after cohesion is filtered by centrifuge；
It is dry：
（10）The gutta-percha particle heating produced to cohesion process, dry removing solvent, obtains eucommia ulmoides refined glue under vacuum.
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| CN111621067A (en) * | 2020-06-17 | 2020-09-04 | 西北农林科技大学 | Method for extracting and separating gutta-percha from eucommia ulmoides Mengni armyworm larva dung |
| CN112142878A (en) * | 2020-11-04 | 2020-12-29 | 山东贝隆杜仲生物工程有限公司 | Condensation process of gutta-percha |
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| CN104231281A (en) * | 2014-09-26 | 2014-12-24 | 西北农林科技大学 | Method for extracting and separating eucommia ulmoides rubber |
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| CN111621067A (en) * | 2020-06-17 | 2020-09-04 | 西北农林科技大学 | Method for extracting and separating gutta-percha from eucommia ulmoides Mengni armyworm larva dung |
| CN111621067B (en) * | 2020-06-17 | 2022-06-14 | 西北农林科技大学 | Method for extracting and separating gutta-percha from eucommia ulmoides Mengni armyworm larva dung |
| CN112142878A (en) * | 2020-11-04 | 2020-12-29 | 山东贝隆杜仲生物工程有限公司 | Condensation process of gutta-percha |
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