CN102838756B - Ultrasound two-way gutta-percha preparation method - Google Patents
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Abstract
Provided is an ultrasound two-way gutta-percha preparation method. The material of gutta-percha preparation is one of natural eucommia skin or eucommia leaves or eucommia seeds. Molecular weight of produced gutta-percha is 40000-350000. The content of the gutta-percha is 99.9%. The method includes that the selected material is cleaned and dried to enable moisture content in the material to be less than 3%; the material is ground to particles with 10-400 micron particle diameter; the material particles are sent to an ultrasound spiral conveying pipe; the material particles are conveyed from A end of the ultrasound spiral conveying pipe to B end of the ultrasound spiral conveying pipe at a set conveying speed, and then enter a separation tank from the B end of the ultrasound spiral conveying pipe; and eventually gutta-percha crystals are precipitated at a low temperature, and the gutta-percha is produced. The preparation method is simple, little in pollution, high in yield rate, and low in cost; and the extraction rate can reach more than 95%, and the content of the gutta-percha reaches 99.9%.
Description
Technical field
The present invention relates to a kind of extracting method of natural product, is a kind of method of Ultrasound two-way gutta-percha preparation specifically.
Background technology
chinese gutta percha be uniquely have except para rubber (natural gum) in the world at present huge
The high-quality natural rubber resource of DEVELOPMENT PROSPECT, and China accounts for cosmopolitic species in the cultivated area of the bark of eucommia
Plant more than 99% of area, there is monopolistic resources advantage.More external developed countries, as Japan, give a long price for the Folium Eucommiae of China in a large number, accelerate the research and development to gutta-percha novel material.Therefore, the applicating and exploitation problem Dou Shi various countries of Chinese gutta percha concentrate the brainstorm subject of investigation.
But the development prospect cognition degree of current domestic industry to bark of eucommia industry is not high, does not have shape
Become the industrial chain of upstream and downstream Application and Development, therefore under this overall situation both domestic and external, China shuts out
The paces of secondary comprehensive utilization of resources need quickening badly, change Natural Rubber in The World Distribution Pattern, strengthen
The right of speech of China's natural rubber resource.China is that high-quality eucommia resource concentrates growing area, the bark of eucommia
The exploitation of glue, effectively will promote that this superior resources of China utilize, particularly military in China
The fields such as industry, tyre production industry.This project main body will strive driving the Changjiang river, the Yellow River middle and lower reaches
The bark of eucommia plant husbandry in area, makes it develop the new natural rubber treasure-house of formation one, Substitute For Partial
Natural rubber, part solves the phenomenon of natural rubber scarcity.The integrated application of natural Chinese gutta percha
And the tool of setting up of information-based key equipment Showcase Production Line is of great significance.Compared with the applied research of Chinese gutta percha aspect, the extraction process of natural Chinese gutta percha and the research and development of corresponding Showcase Production Line are still in the comparatively primary stage.There is a lot of drawback in traditional extraction, such as, extraction time is many, productive rate is low, pollution is heavy, high in cost of production, and therefore these factors are unfavorable for extraction, the development and apply of natural Chinese gutta percha, and become the bottleneck of the natural Chinese gutta percha development of restriction.
Through the scientific research and development of decades, although the extracting method of Chinese gutta percha has breakthrough,
That these extracting method all also exist drawback and are difficult to industrialization, the patent that current China is all and
Document mainly reports following natural Chinese gutta percha extracting method:
A. tight auspicious fragrant patent (Chinese Academy of Sciences chemistry institute): first, mill and expose collodion silk, toluene, benzene, ethylene dichloride extract, and add alcohol, ketone analyses thick glue; Secondly, the dense NaOH infusion hydrocellulose of raw material, pectin, the thick glue of organic solvent extraction.The shortcoming of this method is: collodion silk damage is serious, and physicals is poor, and solvent toxicity is large, and cannot reclaim, complex technical process, seriously polluted, cost is high.
B. old increasing ripple patent (chemistry institute of the Chinese Academy of Sciences): raw material destroys cell walls through fermentation, uses
2%NaOH boiling, hydraulic engine is smashed, and dissociate collodion silk.The shortcoming of this method is: boiling temperature is high, and collodion silk is destroyed, and pollute large, collodion silk purity is not high, and the production cycle is long.
C. Yang Zhen hall patent (special product institute of the Chinese Academy of Agricultural Sciences): cultivate wound healing tissue, dries and makes powder, benzene, trichloromethane lixiviate, methanol extraction, ether purification and recover.The shortcoming of this method is: mixed solvent cannot utilize, and cost is high, and wound healing tissue's regeneration period is long, and leather toxicity is large,
Collodion silk physicals is poor.
D. horse Berlin method: 10%NaOH boiling at 90 DEG C, at 40 DEG C, concentrated hydrochloric acid process obtains thick glue.The shortcoming of this method is: concentrated acid, concentrated base are seriously polluted, and blowdown flow rate is large, and alkali destroys serious to gutta-percha, physicals declines, and product is thick glue.
Draw, no matter be which kind of extracting method above in technique, all there is the defects such as extraction time is many, environmental pollution heavy, extraction efficiency is low according to above As-Is analysis.Therefore, the bottleneck realizing Chinese gutta percha extraction industrialization at present mainly processes the problem that extraction cost is high, extract poor accuracy.Therefore, the new extraction process of development is needed in the development of natural Chinese gutta percha industry badly, realizes the industrialization production that natural Chinese gutta percha extracts application, forms one and extract the Showcase Production Line driving its comprehensive utilization with natural Chinese gutta percha.
Summary of the invention
The invention provides a kind of method of Ultrasound two-way gutta-percha preparation, the method technique is simple, and pollute little, extraction rate reached is to more than 95%, and the content of gutta-percha reaches 99.9%.
A method for Ultrasound two-way gutta-percha preparation, adopt natural Cortex Eucommiae, Folium Eucommiae or Eucommia skin to make, the molecular weight 40000-350000 of gutta-percha, concrete preparation process is as follows:
A kind of method of Ultrasound two-way gutta-percha preparation, the material preparing gutta-percha adopts the one of natural Cortex Eucommiae, Folium Eucommiae or seed of bark of eucommia, the molecular weight 40000-350000 of the gutta-percha after making, the content 99.9% in gutta-percha, is characterized in that preparation process is as follows:
Step one, choose material used, the one namely in natural Cortex Eucommiae, Folium Eucommiae or Eucommia skin, first put into clear water and clean, dry, make the water content in material be less than 3%, for subsequent use;
Step 2, the material feeding pulverizer that will clean up, pulverize, the particle diameter of crushing rear material particle is 10-400 μm;
Step 3, the material particles crushed is sent into ultrasonic spiral conveying tube, material particles is delivered to the B end of ultrasonic spiral conveying tube from the A end of ultrasonic spiral conveying tube according to the transfer rate of setting, after enter extractor from the B end of ultrasonic spiral conveying tube;
The transfer rate of described material particles is: 0.04-0.5m
3/ h;
While holding convey materials particle from ultrasonic spiral conveying tube A, sherwood oil is added as solvent from the B end of ultrasonic spiral conveying tube, the A that sherwood oil flows to ultrasonic spiral conveying tube according to the speed of setting from the B end of ultrasonic spiral conveying tube holds, be dissolved in sherwood oil with material particles in ultrasonic spiral conveying tube after, be transported to extractor;
The flow speed of described sherwood oil is: 0.24-10m
3/ h;
Temperature in described ultrasonic spiral conveying tube is: 70-80 DEG C;
Step 4, the mixeding liquid temperature in extractor is remained on 50 DEG C, sends into 70-200 order filter sieve, filter, remove impurity, after deimpurity mixed solution will be gone to send into separating tank;
The temperature of separating tank controls at 10 DEG C, time length 1-24 hour, the colloid crystallization in mixed solution is precipitated completely after sending into separating tank by step 5, mixed solution;
After colloidal precipitation in step 6, separating tank, release and reclaim the liquid on colloid top layer, i.e. sherwood oil, recycles again, takes out colloid i.e. obtained a kind of natural gutta-percha.
Beneficial effect
1, the present invention adopts micronizing preconditioning technique to carry out pre-treatment to Cortex Eucommiae, be ground into small particle, the different components being conducive to pulverizing nothing extracts, after micronizing, outside more natural Chinese gutta percha component is exposed to, for the dissolving of next step organic solvent is ready.Further, micronizing preconditioning technique also can realize continuous, efficient, the green preprocessing process of the bark of eucommia.
2, leaching process adopt single ether as solvent, the feature of this solvent low toxicity, environmental protection, uses this solvent to extract without discharge cycle, capable of reducing energy consumption, does not relate to separated from solvent problem, can improve solvent utilising efficiency, reduce production cost, free from environmental pollution.
3, have employed advanced ultrasound countercurrent extraction technique, compare by conventional mechanical method, ultrasonic wave is a kind of uniform sphere mechanical wave, judder can be produced, high acceleration, strong cavatition and stirring action, the mass transfer of acceleration system, the processes such as heat transfer, therefore time for solvent assisted extraction, gutta-percha can be accelerated and enter solvent, thus shorten extraction time, save solvent, make its extraction yield more than 95%, the content of gutta-percha reaches 99.9%, whole separation carry glue process have pollute low, the feature that productive rate is high, the classification of gutta-percha can be realized, rapid extraction.
4. obtain gutta-percha collodion silk long, tension, the physical property intensity of anti tear is high, can Application Areas wide.
Accompanying drawing explanation
Fig. 1 is the nmr spectrum of extracted natural rubber;
Embodiment
embodiment 1
A kind of method of Ultrasound two-way gutta-percha preparation, the material preparing gutta-percha adopts the one of natural Cortex Eucommiae, Folium Eucommiae or seed of bark of eucommia, the molecular weight 40000-350000 of the gutta-percha after making, the content 99.9% in gutta-percha, is characterized in that preparation process is as follows:
Step one, choose material used, the one namely in natural Cortex Eucommiae, Folium Eucommiae or Eucommia skin, first put into clear water and clean, dry, make the water content in material be less than 3%, for subsequent use;
Step 2, the material feeding pulverizer that will clean up, pulverize, the particle diameter of crushing rear material particle is 10 μm;
Step 3, the material particles crushed is sent into ultrasonic spiral conveying tube, material particles is delivered to the B end of ultrasonic spiral conveying tube from the A end of ultrasonic spiral conveying tube according to the transfer rate of setting, after enter extractor from the B end of ultrasonic spiral conveying tube;
The transfer rate of described material particles is: 0.04m
3/ h;
While holding convey materials particle from ultrasonic spiral conveying tube A, sherwood oil is added as solvent from the B end of ultrasonic spiral conveying tube, the A that sherwood oil flows to ultrasonic spiral conveying tube according to the speed of setting from the B end of ultrasonic spiral conveying tube holds, be dissolved in sherwood oil with material particles in ultrasonic spiral conveying tube after, be transported to extractor;
The flow speed of described sherwood oil is: 0.24m
3/ h;
Temperature in described ultrasonic spiral conveying tube is: 70 DEG C;
Step 4, the mixeding liquid temperature in extractor is remained on 50 DEG C, sends into 70 order filter sieve, filter, remove impurity, after deimpurity mixed solution will be gone to send into separating tank;
The temperature of separating tank controls at 10 DEG C, 1 hour time length, the colloid crystallization in mixed solution is precipitated completely after sending into separating tank by step 5, mixed solution;
After colloidal precipitation in step 6, separating tank, release and reclaim the liquid on colloid top layer, i.e. sherwood oil, recycles again, takes out colloid i.e. obtained a kind of natural gutta-percha.
embodiment 2
A kind of method of Ultrasound two-way gutta-percha preparation, the material preparing gutta-percha adopts the one of natural Cortex Eucommiae, Folium Eucommiae or seed of bark of eucommia, the molecular weight 40000-350000 of the gutta-percha after making, the content 99.9% in gutta-percha, is characterized in that preparation process is as follows:
Step one, choose material used, the one namely in natural Cortex Eucommiae, Folium Eucommiae or Eucommia skin, first put into clear water and clean, dry, make the water content in material be less than 3%, for subsequent use;
Step 2, the material feeding pulverizer that will clean up, pulverize, the particle diameter of crushing rear material particle is 100 μm;
Step 3, the material particles crushed is sent into ultrasonic spiral conveying tube, material particles is delivered to the B end of ultrasonic spiral conveying tube from the A end of ultrasonic spiral conveying tube according to the transfer rate of setting, after enter extractor from the B end of ultrasonic spiral conveying tube;
The transfer rate of described material particles is: 0.2m
3/ h;
While holding convey materials particle from ultrasonic spiral conveying tube A, sherwood oil is added as solvent from the B end of ultrasonic spiral conveying tube, the A that sherwood oil flows to ultrasonic spiral conveying tube according to the speed of setting from the B end of ultrasonic spiral conveying tube holds, be dissolved in sherwood oil with material particles in ultrasonic spiral conveying tube after, be transported to extractor;
The flow speed of described sherwood oil is: 5m
3/ h;
Temperature in described ultrasonic spiral conveying tube is: 75 DEG C;
Step 4, the mixeding liquid temperature in extractor is remained on 50 DEG C, sends into 100 order filter sieve, filter, remove impurity, after deimpurity mixed solution will be gone to send into separating tank;
The temperature of separating tank controls at 10 DEG C, 15 hours time length, the colloid crystallization in mixed solution is precipitated completely after sending into separating tank by step 5, mixed solution;
After colloidal precipitation in step 6, separating tank, release and reclaim the liquid on colloid top layer, i.e. sherwood oil, recycles again, takes out colloid i.e. obtained a kind of natural gutta-percha.
embodiment 3
A kind of method of Ultrasound two-way gutta-percha preparation, the material preparing gutta-percha adopts the one of natural Cortex Eucommiae, Folium Eucommiae or seed of bark of eucommia, the molecular weight 40000-350000 of the gutta-percha after making, the content 99.9% in gutta-percha, is characterized in that preparation process is as follows:
Step one, choose material used, the one namely in natural Cortex Eucommiae, Folium Eucommiae or Eucommia skin, first put into clear water and clean, dry, make the water content in material be less than 3%, for subsequent use;
Step 2, the material feeding pulverizer that will clean up, pulverize, the particle diameter of crushing rear material particle is 400 μm;
Step 3, the material particles crushed is sent into ultrasonic spiral conveying tube, material particles is delivered to the B end of ultrasonic spiral conveying tube from the A end of ultrasonic spiral conveying tube according to the transfer rate of setting, after enter extractor from the B end of ultrasonic spiral conveying tube;
The transfer rate of described material particles is: 0.5m
3/ h;
While holding convey materials particle from ultrasonic spiral conveying tube A, sherwood oil is added as solvent from the B end of ultrasonic spiral conveying tube, the A that sherwood oil flows to ultrasonic spiral conveying tube according to the speed of setting from the B end of ultrasonic spiral conveying tube holds, be dissolved in sherwood oil with material particles in ultrasonic spiral conveying tube after, be transported to extractor;
The flow speed of described sherwood oil is: 10m
3/ h;
Temperature in described ultrasonic spiral conveying tube is: 80 DEG C;
Step 4, the mixeding liquid temperature in extractor is remained on 50 DEG C, sends into 200 order filter sieve, filter, remove impurity, after deimpurity mixed solution will be gone to send into separating tank;
The temperature of separating tank controls at 10 DEG C, 24 hours time length, the colloid crystallization in mixed solution is precipitated completely after sending into separating tank by step 5, mixed solution;
After colloidal precipitation in step 6, separating tank, release and reclaim the liquid on colloid top layer, i.e. sherwood oil, recycles again, takes out colloid i.e. obtained a kind of natural gutta-percha.
Natural rubber magnetic resonance detection is tested:
Magnetic resonance detection has been carried out to extracted natural rubber, result is as Fig. 1, HNMR collection of illustrative plates display in Fig. 1, at the peak-to-peak signal l.60ppm located than stronger, this peak is trans-1, the proton peak of 4 structure methyl, 1.67ppm place does not almost have signal, shows hardly containing cis-l in natural Chinese gutta percha, the proton peak on 4 structure methyl, also just illustrate in the natural Chinese gutta percha extracted hardly containing cis-l, 4-polyisoprene.The signal at 2.03 ppm and 1.96 ppm two places is shown to be the proton peak of two methylene radical.The signal at 5.10 ppm places is proton peak of double bond in Isosorbide-5-Nitrae structure.1 is not had, 2 structures and 3, the signal of H in 4 structures in figure.The long-pending calculating by peak, the anti-form-1 characterized in figure, the trans-Isosorbide-5-Nitrae structural content of 4-polyisoprene is 99.9%, and cis-Isosorbide-5-Nitrae-polyisoprene structure is 0.1%.
Claims (1)
1. a method for Ultrasound two-way gutta-percha preparation, is characterized in that: the ultrasonic wave of employing is a kind of uniform sphere mechanical wave, and material is with 0.04-0.5m
3the speed of/h is delivered to B end from the A end of ultrasonic spiral conveying tube, and solvent is with 0.24-10m
3the speed of/h flows to A end from the B end of ultrasonic spiral conveying tube, under the judder of sphere mechanical wave, cavitation and stirring action, Accelerative mass transfer, heat transfer process, accelerate gutta-percha enter solvent and obtain gutta-percha mixed solution, gutta-percha filament length after separation and Extraction, tension, tearing toughness are high, the molecular weight 40000-300000 of the gutta-percha after making, content 99.9% in gutta-percha, preparation process is as follows:
Step one, choose material used, the one namely in natural Cortex Eucommiae, Folium Eucommiae or Eucommia skin, first put into clear water and clean, dry, make the water content in material be less than 3%, for subsequent use;
Step 2, the material feeding pulverizer that will clean up, pulverize, the particle diameter of crushing rear material particle is 400 μm;
Step 3, the material particles crushed is sent into ultrasonic spiral conveying tube, material particles is according to 0.04-0.5m
3the transfer rate of/h is delivered to the B end of ultrasonic spiral conveying tube from the A end of ultrasonic spiral conveying tube, after enter extractor from the B end of ultrasonic spiral conveying tube;
While holding convey materials particle from ultrasonic spiral conveying tube A, add sherwood oil as solvent from the B end of ultrasonic spiral conveying tube, sherwood oil is according to 0.24-10m
3the speed of/h flows to the A end of ultrasonic spiral conveying tube from the B end of ultrasonic spiral conveying tube, after being dissolved in sherwood oil, be transported to extractor in ultrasonic spiral conveying tube with material particles;
Temperature in described ultrasonic spiral conveying tube is: 70-80 DEG C;
Step 4, the mixeding liquid temperature in extractor is remained on 50 DEG C, sends into 70-200 order filter sieve, filter, remove impurity, after deimpurity mixed solution will be gone to send into separating tank;
The temperature of separating tank controls at 10 DEG C, time length 1-24 hour, the colloid crystallization in mixed solution is precipitated completely after sending into separating tank by step 5, mixed solution;
After colloidal precipitation in step 6, separating tank, release and reclaim the liquid on colloid top layer, i.e. sherwood oil, recycles again, takes out colloid i.e. obtained a kind of natural gutta-percha.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1948410A (en) * | 2006-11-08 | 2007-04-18 | 贵州大学 | Method of extracting gutta percha by solvent circulation |
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| CN1948410A (en) * | 2006-11-08 | 2007-04-18 | 贵州大学 | Method of extracting gutta percha by solvent circulation |
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| "连续逆流螺旋超声波浸取设备的研究";刘玉德等;《食品与机械》;20090531;第25卷(第3期);第62-64页 * |
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