CN102850555A

CN102850555A - Method for preparing gutta-percha from eucommia bark

Info

Publication number: CN102850555A
Application number: CN2012103078992A
Authority: CN
Inventors: 夏琳; 辛振祥; 魏军生; 李银环
Original assignee: HENAN HENGRUIYUAN INDUSTRIAL CO LTD
Current assignee: HENAN HENGRUIYUAN INDUSTRIAL CO LTD
Priority date: 2012-08-28
Filing date: 2012-08-28
Publication date: 2013-01-02
Anticipated expiration: 2032-08-28
Also published as: CN102850555B

Abstract

A method for preparing gutta-percha from eucommia bark comprises the steps of: first cleaning the eucommia bark with clear water; drying until water content of the eucommia bark is less than 5%; crushing the eucommia bark into particles of 10-100 mum; putting the particles into an extracting tank; adding a single solvent petroleum ether for ultrasonic countercurrent extraction; then conducting stage filtering; and finally extracting gutta-percha by a low-temperature gutta-percha crystal precipitation method. The invention has advantages of simple process, little pollution, high yield and low cost; a micro-grinding pretreatment technology and the ultrasonic countercurrent extraction are employed to realize ideal effects with extraction rate higher than 95% and the gutta-percha content reaching 99.9%.

Description

A kind of method for preparing gutta-percha with Cortex Eucommiae

Technical field

The present invention relates to a kind of extracting method of natural product, is a kind of method for preparing gutta-percha with Cortex Eucommiae specifically.

Background technology

The bark of eucommia is the distinctive famous and precious economic tree of China, also is the widest important collagen plant of the scope of application in the world.All be rich in a kind of white rope---gutta-percha in the leaf of the bark of eucommia, bark and the pericarp.The Application Areas of gutta-percha has been opened up in the discovery of gutta-percha exclusive " rubber-plastics duplicity ".Its comprehensive development and utilization has caused the extensive concern of national departments concerned.

Compare with the applied research of gutta-percha aspect, the extraction process of natural Chinese gutta percha and the research and development of corresponding Showcase Production Line still were in than the primary stage, although gutta-percha can extract from eucommia bark, leaf and fruit thereof, but there is a lot of drawbacks in traditional extraction, such as: extraction time is many, and productive rate is low, pollute heavy, the shortcomings such as floor space is large, and cost is high, need waste residue to be processed is too many etc., these factors are unfavorable for extraction, development and the application of natural Chinese gutta percha.

At present all patent documentation of China and document mainly are divided into following several to the report of the pretreatment process in the natural Chinese gutta percha leaching process: milling and the pretreatment process of auxiliary dense NaOH infusion in the tight auspicious fragrant patent; Oldly increase in the ripple patent fermentation and with the 2%NaOH boiling, hydraulic engine is beaten the group, the force method of the collodion silk that dissociates; Horse Berlin method: 10%NaOH is at 90 ℃

Lower boiling, 40 ℃ of lower concentrated hydrochloric acids are processed the rhythm force methods: the Zhang Xuejun method: adopt multiple prozyme chicken roost Folium Eucommiae to carry out enzymolysis, make bark of eucommia silk free out etc.The shortcomings such as it is more serious that but these traditional pre-treatment force methods often exist the collodion silk damage, and blowdown flow rate is larger, and the product cycle is long.Therefore, the extraction process and the method that need a kind of natural Chinese gutta percha newly.

Summary of the invention

The invention provides a kind of method for preparing gutta-percha with Cortex Eucommiae, the method technique is simple, pollutes littlely, and more than the extraction rate reached to 95%, the content of gutta-percha reaches 99.9%.

A kind of method for preparing gutta-percha with Cortex Eucommiae adopts natural Cortex Eucommiae to make, the molecular weight 40000-300000 of gutta-percha, and its concrete preparation process is as follows:

Step 1, Cortex Eucommiae is put into clear water clean, dry, make the water content in the Cortex Eucommiae

Less than 5%, for subsequent use;

Step 2, with step 1 handle well Cortex Eucommiae send into supper micron mill, carry out micronizing, the particle after the pulverizing is floss, particle diameter is 10-100 μ m;

Step 3, the Cortex Eucommiae particle that step 2 is crushed are sent into ultrasonic extraction tank, carry out the ultrasonic vibration combination treatment, and concrete processing requirements is:

A, elder generation put into petroleum ether solution in ultrasonic extraction tank, the Cortex Eucommiae particle that rear adding crushes, and the weight ratio that Cortex Eucommiae particle and petroleum ether solution add is: 1:6-16;

The ultrasonic vibration device of B, unlatching ultrasonic extraction tank, it is 2.4-3.6KW that power is set, and shakes time 30-60 minute, temperature: 50-75 ℃, makes the object in the extractor form the colloid mixed solution;

Step 4, the colloid mixed solution that step 3 is formed are sent into dregs and liquor separation device, carry out classified filtering, make its temperature remain on 50 ℃, cross first 1000 order filter sieve, then being 500 order filter sieve, then is less than 200 order filter sieve, will go at last deimpurity colloid mixed solution to send into separating tank;

After step 5, colloid mixed solution are sent into separating tank, the temperature of separating tank is controlled at 10 ℃, time length 2-16 hour, the colloid in the separating tank is precipitated fully;

After the colloidal precipitation in the step 6, separating tank, emit and reclaim the liquid on the colloid top layer, take out colloid, or with below the greenhouse cooling to 10 of separating tank ℃, take out after making the colloid crystallization, namely make a kind of natural gutta-percha.

Beneficial effect

1, the present invention adopts the micronizing preconditioning technique that Cortex Eucommiae is carried out pre-treatment, it is ground into small particle, and the different components that is conducive to crushed material extracts, after micronizing, outside more natural Chinese gutta percha component is exposed to, for the dissolving of next step organic solvent ready.And the micronizing preconditioning technique also can be realized continuous, efficient, the green preprocessing process of the bark of eucommia, can reduce the volume of extraction equipment, reduces the usage quantity of organic solvent, the extraction efficiency of Effective Raise natural rubber;

2, leaching process adopts the solvent of single ether conduct, and the characteristics of this solvent low toxicity, environmental protection use this solvent to extract without discharge cycle, and are capable of reducing energy consumption, do not relate to the separated from solvent problem, can improve the solvent utilising efficiency, reduce production costs, free from environmental pollution;

3, adopt classified filtering, avoid stopping up, make filter effect better, improve filtration efficiency, save the technological operation time;

4, adopted advanced ultrasound countercurrent extraction technique, compare with conventional mechanical method, ultrasonic wave is a kind of uniform sphere mechanical wave, can produce judder, high acceleration, strong cavatition and stirring action, the mass transfer of acceleration system, the processes such as heat transfer, when therefore being used for the solvent assisted extraction, can accelerate gutta-percha and enter solvent, thereby shorten extraction time, save solvent, make its extraction yield more than 95%, the content of gutta-percha reaches 99.9%, whole separation carry the glue process have pollute low, productive rate is high, the characteristics that cost is low can realize the classification of gutta-percha, rapid extraction.

Description of drawings

Fig. 1 is the scanning electron microscope picture through eucommia bark after the micronizing pre-treatment;

Fig. 2 is not for passing through the scanning electron microscope picture of the pretreated eucommia bark of micronizing;

From Fig. 1 and Fig. 2, can find out, Fig. 1 and Fig. 2 contrast, can observe the eucommia bark of processing through ultra micro among Fig. 2, there is the Chinese gutta percha component outside more being exposed to around its micron-sized vegetable fibre, the condition that the micronizing preconditioning technique is provided convenience for next step organic solvent extraction work is described, is conducive to the extraction of gutta-percha.

Fig. 3 is the nmr spectrum of the natural rubber that extracts.

Embodiment

Embodiment 1

Less than 5%, for subsequent use;

Step 2, with step 1 handle well Cortex Eucommiae send into supper micron mill, carry out micronizing, the particle after the pulverizing is floss, particle diameter is 10 μ m;

A, elder generation put into petroleum ether solution in ultrasonic extraction tank, the Cortex Eucommiae particle that rear adding crushes, and the weight ratio that Cortex Eucommiae particle and petroleum ether solution add is: 1:6;

The ultrasonic vibration device of B, unlatching ultrasonic extraction tank, it is 2.4KW that power is set, 30 minutes vibrations time, temperature: 50 ℃, make the object in the extractor form the colloid mixed solution;

Step 4, the colloid mixed solution that step 3 is formed are sent into dregs and liquor separation device, carry out classified filtering, make its temperature remain on 50 ℃, cross first 1000 order filter sieve, then being 500 order filter sieve, then is 100 order filter sieve, will go at last deimpurity colloid mixed solution to send into separating tank;

After step 5, colloid mixed solution are sent into separating tank, the temperature of separating tank is controlled at 10 ℃, 2 hours time length, the colloid in the separating tank is precipitated fully;

Embodiment 2

Less than 5%, for subsequent use;

Step 2, with step 1 handle well Cortex Eucommiae send into supper micron mill, carry out micronizing, the particle after the pulverizing is floss, particle diameter is 50 μ m;

A, elder generation put into petroleum ether solution in ultrasonic extraction tank, the Cortex Eucommiae particle that rear adding crushes, and the weight ratio that Cortex Eucommiae particle and petroleum ether solution add is: 1:10;

The ultrasonic vibration device of B, unlatching ultrasonic extraction tank, it is 3.0KW that power is set, 40 minutes vibrations time, temperature: 60 ℃, make the object in the extractor form the colloid mixed solution;

Step 4, the colloid mixed solution that step 3 is formed are sent into dregs and liquor separation device, carry out classified filtering, make its temperature remain on 50 ℃, cross first 1000 order filter sieve, then being 500 order filter sieve, then is 150 order filter sieve, will go at last deimpurity colloid mixed solution to send into separating tank;

After step 5, colloid mixed solution are sent into separating tank, the temperature of separating tank is controlled at 10 ℃, 8 hours time length, the colloid in the separating tank is precipitated fully;

Embodiment 3

Less than 5%, for subsequent use;

Step 2, with step 1 handle well Cortex Eucommiae send into supper micron mill, carry out micronizing, the particle after the pulverizing is floss, particle diameter is 100 μ m;

A, elder generation put into petroleum ether solution in ultrasonic extraction tank, the Cortex Eucommiae particle that rear adding crushes, and the weight ratio that Cortex Eucommiae particle and petroleum ether solution add is: 1:16;

The ultrasonic vibration device of B, unlatching ultrasonic extraction tank, it is 3.6KW that power is set, 60 minutes vibrations time, temperature: 75 ℃, make the object in the extractor form the colloid mixed solution;

Step 4, the colloid mixed solution that step 3 is formed are sent into dregs and liquor separation device, carry out classified filtering, make its temperature remain on 50 ℃, cross first 1000 order filter sieve, then being 500 order filter sieve, then is 200 order filter sieve, will go at last deimpurity colloid mixed solution to send into separating tank;

After step 5, colloid mixed solution are sent into separating tank, the temperature of separating tank is controlled at 10 ℃, 16 hours time length, the colloid in the separating tank is precipitated fully;

The experiment of natural rubber magnetic resonance detection:

The natural rubber that extracts has been carried out magnetic resonance detection, result such as Fig. 3, the HNMR collection of illustrative plates shows among Fig. 3, and is stronger at the peak-to-peak signal of l.60ppm locating, and this peak is anti--1, the proton peak of 4 structure methyl, 1.67ppm locate almost not have signal, show and in natural Chinese gutta percha, contain hardly suitable-l, the proton peak on the 4 structure methyl, do not contain suitable-Isosorbide-5-Nitrae polyisoprene in the natural rubber that also just explanation is extracted.2.03 the signal at ppm and 1.96 ppm, two places shows it is the proton peak of two methylene radical.5.10 the signal at ppm place is the proton peak of two keys in the Isosorbide-5-Nitrae structure.The signal that does not have H in 1,2 structure and 3,4 structures among the figure.Amass calculating by the peak, the anti-form-1 that characterizes among the figure, the 4-polyisoprene anti--the Isosorbide-5-Nitrae structural content is 99.9%, cis-Isosorbide-5-Nitrae-polyisoprene structure is 0.1%.

Claims

1. a method for preparing gutta-percha with Cortex Eucommiae adopts natural Cortex Eucommiae to make, the molecular weight 40000-300000 of gutta-percha, and the content of gutta-percha: 99.9%, it is characterized in that preparation process is as follows:

Less than 5%, for subsequent use;

Step 4, the colloid mixed solution that step 3 is formed are sent into dregs and liquor separation device, make its temperature remain on 50 ℃, carry out classified filtering, will go deimpurity colloid mixed solution to send into separating tank;

2. a kind of method for preparing gutta-percha with Cortex Eucommiae as claimed in claim 1 is characterized in that: described classified filtering is, crosses first 1000 order filter sieve, after 500 order filter sieve, then is less than 200 order filter sieve.