CN113354833A - Method for extracting gutta-percha at ultralow temperature - Google Patents
Method for extracting gutta-percha at ultralow temperature Download PDFInfo
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- CN113354833A CN113354833A CN202110860511.0A CN202110860511A CN113354833A CN 113354833 A CN113354833 A CN 113354833A CN 202110860511 A CN202110860511 A CN 202110860511A CN 113354833 A CN113354833 A CN 113354833A
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Abstract
The invention provides a method for extracting gutta-percha at ultralow temperature. The method comprises the following steps: 1) soaking a pretreated raw material in an aqueous solution containing a surfactant for a preset time to obtain a soaking solution, wherein the pretreated raw material is any one or a combination of at least two of crushed eucommia leaves, eucommia bark and eucommia key fruit peels; 2) in the presence of an organic solvent, carrying out ultrasonic treatment, stirring, extraction and liquid separation on the soaking solution to obtain an organic phase containing gutta-percha, and carrying out solid-liquid separation on the organic phase to obtain a glue solution containing the gutta-percha; 3) and (4) freezing the glue solution to separate out gutta-percha. The method for extracting the gutta-percha at the ultralow temperature has the advantages of mild process conditions, high process safety, environmental protection and the like.
Description
Technical Field
The invention relates to a method for extracting natural products, in particular to a method for extracting gutta-percha at ultralow temperature.
Background
Eucommia ulmoides (Eucornia ulmoides) is a plant of the family of eucommia ulmoides, and is a unique rare medicinal material and woody oil plant in China. The root, stem, leaf, flower and fruit of eucommia ulmoides plant all contain a white filamentous substance, namely eucommia ulmoides gum, wherein the gum content in eucommia ulmoides leaf is 2-5%, the gum content in bark is 9-12%, and the gum content in seed peel is 15-25%.
The gutta-percha is one of natural rubber, can be developed into three functional materials of thermoplasticity, thermoelasticity and rubber elasticity, and has very wide application prospect. Since gutta-percha exists in specialized filamentous unicells among phloem parenchyma cells of eucommia ulmoides, and is low in gum content and high in viscosity, and cannot be directly collected by tapping like natural rubber, it is necessary to develop an extraction process of gutta-percha to obtain gutta-percha.
Because of the extensive existence of cellulose, lignin and other structures in plants, extraction of gutta-percha is not easy, and the extraction methods of gutta-percha at present mainly comprise a mechanical method, an alkaline leaching method, a solvent extraction method, a microbial fermentation method, an enzymolysis method and the like, and specifically comprise the following steps:
the mechanical method mainly utilizes high-speed stirring to break cell walls, so that the gutta-percha is separated out, and only crude gum can be prepared by the mechanical method, and the impurity content is more. The method is suitable for continuous large-scale production, but the severe breaking and washing can cause severe loss of the glue threads, and the yield is low.
The alkaline leaching method comprises washing folium Eucommiae or cortex Eucommiae, fermenting, steaming with sodium hydroxide aqueous solution, breaking cell wall lignin to expose gelatin silk, rinsing, breaking with hydraulic breaker, and sieving and rinsing to obtain gutta Percha. The alkaline leaching method consumes a large amount of sodium hydroxide, which causes high cost and environmental pollution, and the gutta percha silk has large loss and low yield.
The solvent method is to extract the gutta-percha by adopting different organic solvents, the common solvents comprise toluene, petroleum ether and other nonpolar solvents, the extraction temperature is generally slightly lower than the boiling temperature of the solvents, the petroleum ether with the boiling range of 60-90 ℃ is used, and the extraction temperature is usually 80-90 ℃. The solvent method has the disadvantages of small loss of the colloidal silk, high yield and higher purity, and needs long-time extraction or multiple times of extraction. In addition, the organic solvent commonly used at present is generally inflammable and has high toxicity. In addition, the impurities in the leaching solution are not evaporated in the distillation like the solvent such as petroleum ether, but are precipitated in the gutta percha, and the refining is difficult.
The microbial fermentation or enzymolysis method is to degrade cellulose of cell walls to loosen the cell walls, so that the gutta-percha is dissolved out. The bacteria used in the microbial fermentation method include Pseudomonas, Bacillus in Bacillus, Bacillus subtilis, and lichen, and the fungi include mold, yeast, and Basidiomycetes; actinomycetes include Nocardia, Arthrobacter, Streptomyces, Thermoactinomyces, and Micromonospora, etc., which decompose cell walls mainly by secreting cellulase, hemicellulase, and ligninase.
Disclosure of Invention
The method for extracting the gutta-percha at the ultralow temperature provided by the embodiment of the invention has the advantages of mild process conditions, high process safety, environmental protection and the like. In order to achieve the above purpose, the embodiment of the present invention provides the following technical solutions:
the embodiment of the invention provides a method for extracting gutta-percha at ultralow temperature, which comprises the following steps:
1) soaking a pretreated raw material in an aqueous solution containing a surfactant for a preset time to obtain a soaking solution, wherein the pretreated raw material is any one or a combination of at least two of crushed eucommia leaves, eucommia bark and eucommia key fruit peels;
2) in the presence of an organic solvent, carrying out ultrasonic treatment, stirring, extraction and liquid separation on the soaking solution to obtain an organic phase containing gutta-percha, and carrying out solid-liquid separation on the organic phase to obtain a glue solution containing the gutta-percha;
3) and (4) freezing the glue solution to separate out gutta-percha.
In a specific embodiment, in step 1), the surfactant is any one of sodium dodecyl sulfate, polyethylene glycol p-isooctyl phenyl ether, polyethylene glycol ethyl phenyl ether or a combination of at least two thereof.
In a specific embodiment, the concentration of the surfactant in the aqueous solution is 0.1-2% by mass.
In a specific embodiment, in the step 1), the preset time is 15-120 min.
In a specific embodiment, the step 1) comprises:
crushing the raw materials to 0.5-5 cm to obtain pretreated raw materials, wherein the raw materials are any one or a combination of at least two of eucommia leaves, eucommia bark and eucommia key fruit peel;
mixing the pretreated feedstock and an aqueous solution containing a surfactant;
adjusting the pH value of the aqueous solution to be alkalescent by using an alkali solution;
and soaking the pretreated raw material in a weakly alkaline aqueous solution for the preset time to obtain the soaking solution.
In a specific embodiment, in the step 2), the temperature of the ultrasonic treatment is 20-40 ℃, and the time of the ultrasonic treatment is 5-30 min.
In a specific embodiment, the power of ultrasonic treatment is 300-3600 w.
In a specific embodiment, in the step 2), the temperature for stirring and extracting is 25-45 ℃, and the time for stirring and extracting is 20-60 min.
In a specific embodiment, in step 2), the organic solvent is any one of petroleum ether, benzene and toluene or a combination of at least two of petroleum ether, benzene and toluene.
In a specific embodiment, the freezing gel separation temperature for separating out the gutta-percha by freezing treatment is-20 to-10 ℃, and the freezing gel separation time is 2 to 3 hours.
Compared with the prior art, the invention has the following advantages and beneficial effects:
firstly, crushing raw materials, soaking the crushed raw materials into an aqueous solution containing a surfactant for treatment, destroying cell walls of cells containing gelatin, and adding an organic solvent for ultrasonic extraction; in this way, the ultrasonic treatment is carried out in a water-organic solvent two-phase system, and has the advantages that firstly, non-gutta percha impurities which can be dissolved in water are transferred into a water phase through a soaking process, so that the content of the impurities remained in the organic solvent is reduced; on the other hand, the density of the organic solvent is less than that of water and is positioned at the upper layer, the extracted gutta-percha is dissolved in the organic solvent, the extracted residue falls into the lower water phase, the residue and the gutta-percha can be separated only by simply carrying out liquid separation operation, and the efficiency of the subsequent organic phase solid-liquid separation process is improved.
And secondly, after the pretreated raw materials are soaked in the aqueous solution containing the surfactant for a preset time, the organic solvent can be directly added for the next operation, and the raw materials treated by the surfactant do not need to be filtered and dried, so that the production process steps can be reduced, and the production cost can be reduced.
Thirdly, after the pretreated raw materials are treated by the surfactant and the ultrasonic waves, the dissolution of the gutta percha is facilitated, the extraction is carried out at ultralow temperature, the extraction rate can reach more than 95 percent (only one extraction is needed), and the extraction efficiency is high; in addition, the temperature of ultralow temperature extraction is 25-45 ℃ and is lower than the boiling point of the organic solvent, so that on one hand, the requirements of production equipment can be reduced, and a reflux device is not required to be configured; on the other hand, the ultralow extraction temperature can effectively reduce the volatilization and escape of the organic solvent, improve the safety of the production process, reduce the pollution of the solvent to the atmosphere, and has the advantages of mild process conditions, high process safety, environmental protection and the like.
Drawings
Fig. 1 is a flowchart illustrating steps of a method for extracting gutta percha at ultra-low temperature according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, an embodiment of the present invention provides a method for extracting gutta percha at ultra-low temperature, including the following steps:
step S1, soaking the pretreated raw material in a water solution containing a surfactant for a preset time to obtain a soaking solution, wherein the pretreated raw material is any one or the combination of at least two of crushed eucommia leaves, eucommia bark and eucommia key fruit peels;
preferably, the surfactant is any one of sodium dodecyl sulfate, polyethylene glycol p-isooctyl phenyl ether and polyethylene glycol ethyl phenyl ether or the combination of at least two of the above.
Preferably, the mass percentage concentration of the surfactant in the aqueous solution is 0.1-2%.
Preferably, the feed-liquid ratio of the pretreated raw material to the aqueous solution containing the surfactant is 1: (3-10).
Preferably, the preset time is 15-120 min.
Preferably, the step S1 further includes adding an alkali solution to the pretreated raw material after the pretreated raw material is placed in the aqueous solution containing the surfactant to adjust the pH value to be weakly alkaline; more preferably, the alkali solution is ammonia.
The step S1 specifically includes: drying raw materials including folium cortex eucommiae, cortex eucommiae and winged fruit peel, smashing to 0.5-5 cm to obtain a pretreated raw material, placing the pretreated raw material into an aqueous solution containing a surfactant (the mass percentage concentration of the surfactant is 0.1-2%), adding ammonia water to adjust the pH value to be alkalescent, soaking for 15-120 min to obtain a soaking solution, and then entering the next step.
In the embodiment of the invention, the pH value corresponding to weak alkalinity is 7-8.5.
More preferably, the pretreated raw materials are crushed to 0.5-1 cm, and the smaller the length of the pretreated raw materials is, the more favorable the dissolution of gutta-percha and other non-gutta-percha impurities is.
In the embodiment of the invention, the raw materials are mechanically crushed to 0.5-5 cm, in other embodiments, the pretreated raw materials can be directly purchased for extraction or manually crushed, and the invention is not limited.
Because the gutta-percha exists in the glue-containing cells, the cells are surrounded by the cellulose and the lignin, the glue-containing cells are exposed through preliminary smashing, and then the raw materials exposed out of the glue-containing cells are placed in the water solution containing the surfactant; therefore, on one hand, the surfactant has the function of cell lysis, and after cell lysis, the gutta percha is diffused and is easier to be extracted by an organic solvent; on the other hand, non-gutta percha impurities that can be dissolved in water can be transferred to the aqueous phase, reducing the content of impurities remaining in the organic solvent.
Step S2, in the presence of an organic solvent, subjecting the soaking solution to ultrasonic treatment, stirring, extracting and liquid separation to obtain an organic phase containing gutta-percha, and performing solid-liquid separation on the organic phase to obtain a glue solution containing gutta-percha;
preferably, the organic solvent is any one of petroleum ether, benzene and toluene or the combination of at least two of the petroleum ether, the benzene and the toluene.
Preferably, the feed-liquid ratio of the pretreated raw material to the organic solvent is 1: (3-15).
Preferably, the temperature of ultrasonic treatment is 20-40 ℃, and the time of ultrasonic treatment is 5-30 min.
Preferably, the power of ultrasonic treatment is 300-3600 w.
The ultrasonic treatment power is positively correlated with the mass of the pretreated raw material, and the larger the mass of the raw material to be treated is, the larger the ultrasonic treatment power is; normally, the greater the power of the sonication, the shorter the sonication time.
After the cells of the raw material are cracked by the surfactant, the glue-containing cells can be further destroyed through ultrasonic treatment, specifically, on one hand, the cellulose and lignin are destroyed by the mechanical impact of the cavitation action of the glue-containing cells, so that more glue-containing cells can be exposed; on the other hand, the cell structure is destroyed by ultrasonic waves, so that the gutta percha is diffused out of the cell structure. To achieve this, the power of the sonication needs to be greater than 300 w.
Preferably, the temperature for stirring and extracting is 25-45 ℃, and the time for stirring and extracting is 20-60 min.
In the embodiment of the invention, the solid-liquid separation mode is filtration.
The step S2 specifically includes: adding an organic solvent into the soaking solution, carrying out ultrasonic treatment for 5-30 min at the temperature of 20-40 ℃ under the condition of 300-3600 w in a water-organic solvent two-phase solvent, then stirring for 20-60 min at the temperature of 25-45 ℃, obtaining a water phase containing residues and an organic phase containing gutta-percha after liquid separation, and filtering the organic phase to obtain a glue-containing solution.
The prior art only adopts organic solvent for extraction at present, and the organic phase contains both gutta-percha and residue, so that the filtering efficiency is low because the gutta-percha is easy to separate out and blocks the filtering cloth in the form of sticky substances when the residue is filtered and separated. The invention is based on water phase-organic phase extraction, the extracted gutta-percha is dissolved in an organic solvent, the extracted residue falls into the lower layer water phase, the residue and the gutta-percha can be separated by liquid separation, and then the organic phase is filtered to obtain the liquid containing solution, thereby greatly improving the filtering efficiency.
And step S3, freezing the glue solution to separate out gutta-percha.
Preferably, the freezing gel separation temperature for separating out the gutta-percha through freezing treatment is-20 to-10 ℃, and the freezing gel separation time is 2 to 3 hours.
When the freezing time is less than 2 hours, the yield of the product gutta-percha is influenced, the freezing time is too long, the influence is basically avoided, the production cost is considered, and the freezing gel separation time is 2-3 hours.
According to the invention, after cell walls of raw materials are destroyed by a pretreatment process, the raw materials are soaked into an aqueous solution containing a surfactant for treatment, an organic solvent is added for ultrasonic extraction, the eucommia ulmoides gum can be easily diffused from the raw material cells by the combination of the soaking of the surfactant solution and the ultrasonic extraction, so that the extraction temperature is reduced, the extraction temperature of the solvent method in the prior art is 80-90 ℃, the extraction temperature of the method is 25-45 ℃ and is lower than the boiling point (60-90 ℃) of the organic solvent, on the one hand, the requirements of production equipment can be reduced, and a reflux device is not required; on the other hand, the ultralow extraction temperature can effectively reduce the precipitation of the organic solvent, improves the safety of the production process, also reduces the pollution of the solvent to the atmosphere, and has the advantages of mild process conditions, high process safety, environmental protection and the like.
Example 1
Crushing 500g of dried eucommia key fruit peel to 0.5-1 cm, placing the crushed eucommia key fruit peel into an aqueous solution containing 0.2% of lauryl sodium sulfate (the material-liquid ratio of the eucommia key fruit peel to the aqueous solution is 1: 3), adding ammonia water to adjust the pH value to be alkalescent, soaking for 15 minutes, and then adding the mixture into a water tank according to the weight ratio of 1: 6, adding petroleum ether (with a boiling range of 60-90 ℃) into a water-petroleum ether two-phase solvent, performing ultrasonic treatment for 10min at 30 ℃ by using 300w power ultrasound, then stirring for 30min at 25 ℃, separating liquid to obtain an organic phase and a water phase, filtering the organic phase to obtain a liquid containing glue, freezing the liquid containing glue below-10 ℃ for 2 hours to separate out gutta-percha, and recovering and extracting the gutta-percha with an extraction rate of 95.7%.
Example 2
Crushing 500g of dried mixture of the key fruit peel and the leaves of the eucommia ulmoides into 0.5-5 cm, placing the mixture into an aqueous solution containing 0.5% of polyethylene glycol p-isooctyl phenyl ether (the material-liquid ratio of the mixture of the key fruit peel and the leaves of the eucommia ulmoides to the aqueous solution is 1: 5), adding ammonia water to adjust the pH value to be alkalescent, soaking for 15 minutes, and then adding the mixture into a container according to the weight ratio of 1: 8, adding petroleum ether (the boiling range is 60-90 ℃) into a water-petroleum ether two-phase solvent, performing ultrasonic treatment for 5min at 40 ℃ by using 1.6KW power ultrasound, then stirring for 30min at 45 ℃, separating liquid to obtain an organic phase and a water phase, filtering the organic phase to obtain a liquid containing glue solution, freezing the liquid containing glue solution below-10 ℃ for 2.5 hours to separate out gutta-percha, and recovering and extracting the gutta-percha with the recovery rate of 96.2%.
Example 3
Crushing 1000g of dried eucommia key fruit peel to 0.5-1 cm, placing the crushed eucommia key fruit peel into a water solution containing 2% polyethylene glycol ethyl phenyl ether (the material-liquid ratio of the eucommia key fruit peel to the water solution is 1: 6), adding ammonia water to adjust the pH value to be alkalescent, soaking for 15 minutes, and then adding the mixture into a water tank according to the weight ratio of 1: 8, adding benzene into a water-benzene two-phase solvent, performing ultrasonic treatment for 15min at 20 ℃ by using 1.6KW power ultrasound, then stirring for 45min at 35 ℃, separating liquid to obtain an organic phase and a water machine, filtering the organic phase to obtain a liquid containing glue, freezing the liquid containing glue below-10 ℃ for 3 hours to separate out gutta-percha, and recovering and extracting the gutta-percha with the recovery rate of 96.3 percent.
Example 4
Crushing 1000g of dried mixture of the winged fruit pericarp and the bark of the eucommia ulmoides tree to 0.5-5 cm, placing the mixture into a water solution containing 2% of polyethylene glycol ethyl phenyl ether (the material-liquid ratio of the mixture of the winged fruit pericarp and the bark of the eucommia ulmoides tree to the water solution is 1: 5), adding ammonia water to adjust the pH value to be alkalescent, soaking for 15 minutes, and then adding the mixture into a container according to the weight ratio of 1: 10, adding toluene into a water-toluene two-phase solvent, performing ultrasonic treatment for 25min at 35 ℃ by using 1.5KW power ultrasound, then stirring for 30min at 45 ℃, separating liquid to obtain an organic phase and a water phase, filtering the organic phase to obtain a liquid containing glue solution, freezing the liquid containing glue solution below-10 ℃ for 2 hours to separate out the gutta-percha, wherein the recovery extraction rate of the gutta-percha is 95.8%.
Example 5
Crushing 1000g of dried bark of eucommia ulmoides tree to 1-5 cm primarily, then placing the bark of eucommia ulmoides tree in an aqueous solution containing 1% of polyethylene glycol ethyl phenyl ether (the material-liquid ratio of the bark of eucommia ulmoides tree to the aqueous solution is 1: 3), adding ammonia water to adjust the pH value to be alkalescent, soaking for 60 minutes, and then adding 1: 3, adding petroleum ether (with a boiling range of 60-90 ℃) into a water-petroleum ether two-phase solvent, performing ultrasonic treatment for 30min at 32 ℃ by using 3.6KW power ultrasound, then stirring for 60min at 40 ℃, obtaining an organic phase and a water phase by liquid separation, filtering the organic phase to obtain a liquid containing glue solution, freezing the liquid containing glue solution below-10 ℃ for 2.5 hours to separate out gutta-percha, and recovering and extracting the gutta-percha with the extraction rate of 95.4%.
Example 6
Crushing 1000g of dried eucommia ulmoides leaves to 0.5-1 cm primarily, then placing the crushed eucommia ulmoides leaves into an aqueous solution containing 0.3% of lauryl sodium sulfate (the material-liquid ratio of the eucommia ulmoides leaves to the aqueous solution is 1: 10), adding ammonia water to adjust the pH value to be alkalescent, soaking for 30 minutes, and then adding 1: 15 of petroleum ether (boiling range is 60-90 ℃), performing ultrasonic treatment for 20min at 30 ℃ by using 1KW power ultrasound in a water-petroleum ether two-phase solvent, then stirring for 30min at 40 ℃, obtaining an organic phase and a water phase by liquid separation, filtering the organic phase to obtain a liquid containing glue, freezing the liquid containing glue below-10 ℃ for 3 hours to separate out gutta-percha, and recovering and extracting the gutta-percha with the extraction rate of 97.1%.
In the present invention, the unit of the feed-to-liquid ratio is g/ml.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
All the embodiments in the present specification are described in a related manner, and the same and similar parts among the embodiments may be referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. The method for extracting gutta percha at ultralow temperature is characterized by comprising the following steps:
1) soaking a pretreated raw material in an aqueous solution containing a surfactant for a preset time to obtain a soaking solution, wherein the pretreated raw material is any one or a combination of at least two of crushed eucommia leaves, eucommia bark and eucommia key fruit peels;
2) in the presence of an organic solvent, carrying out ultrasonic treatment, stirring, extraction and liquid separation on the soaking solution to obtain an organic phase containing gutta-percha, and carrying out solid-liquid separation on the organic phase to obtain a glue solution containing the gutta-percha;
3) and (4) freezing the glue solution to separate out gutta-percha.
2. The method for extracting gutta-percha at ultra-low temperature as claimed in claim 1, wherein said surfactant is any one or a combination of at least two of sodium dodecyl sulfate, polyethylene glycol p-isooctyl phenyl ether, and polyethylene glycol ethyl phenyl ether in step 1).
3. The method for extracting gutta percha at ultra-low temperature as claimed in claim 2, wherein the concentration of the surfactant in the aqueous solution is 0.1-2% by mass.
4. The method for extracting gutta percha at ultra-low temperature as in claim 1, wherein said predetermined time is 15-120 min in step 1).
5. The method for extracting gutta percha at ultra-low temperature as set forth in any one of claims 1 to 4, wherein said step 1) comprises:
crushing the raw materials to 0.5-5 cm to obtain pretreated raw materials, wherein the raw materials are any one or a combination of at least two of eucommia leaves, eucommia bark and eucommia key fruit peel;
mixing the pretreated feedstock and an aqueous solution containing a surfactant;
adjusting the pH value of the aqueous solution to be alkalescent by using an alkali solution;
and soaking the pretreated raw material in a weakly alkaline aqueous solution for the preset time to obtain the soaking solution.
6. The method for extracting gutta percha at ultra-low temperature as claimed in claim 1, wherein the temperature of the ultrasonic treatment in the step 2) is 20 to 40 ℃ and the time of the ultrasonic treatment is 5 to 30 min.
7. The method for extracting gutta percha at ultra-low temperature as claimed in claim 6, wherein the power of ultrasonic treatment is 300-3600 w.
8. The method for extracting gutta percha at ultra-low temperature as in claim 1 or 6, wherein the temperature of the stirring extraction in the step 2) is 25 to 45 ℃ and the time of the stirring extraction is 20 to 60 min.
9. The method for extracting gutta percha at ultra-low temperature as claimed in claim 1, wherein said organic solvent is any one or a combination of at least two of petroleum ether, benzene and toluene in the step 2).
10. The method for extracting gutta-percha at ultra-low temperature as in claim 1, wherein the freezing and gel-separating temperature for separating gutta-percha by freezing treatment in the step 3) is-20 to-10 ℃, and the freezing and gel-separating time is 2 to 3 hours.
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| CN110423361A (en) * | 2019-08-20 | 2019-11-08 | 贵州大学 | A kind of natural gutta-percha lotion |
| CN110467734A (en) * | 2019-08-29 | 2019-11-19 | 贵州大学 | A kind of method of the thick glue solution purifying preparation eucommia ulmoides refined glue of Cortex Eucommiae seed peel |
| CN112724420A (en) * | 2021-02-01 | 2021-04-30 | 福州大学 | Method for efficiently extracting high-purity gutta-percha based on ionic liquid and organic solvent biphase |
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