CN102838758A

CN102838758A - Method of preparing gutta-percha with eucommia leaves

Info

Publication number: CN102838758A
Application number: CN2012103079891A
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: 2012-12-26
Anticipated expiration: 2032-08-28
Also published as: CN102838758B

Abstract

Provided is a method of preparing gutta-percha with eucommia leaves. The eucommia leaves are placed into clear water to be cleaned and then dried to enable moisture content inside eucommia skin to be less than 5%. The eucommia leaves are ground into particles with 10-500 micron particle diameter. Based on the eucommia leave granules and petroleum ether solutions in a weight ratio of 1:6-1:8, the petroleum ether is added. Under the temperature of 50-75 DEG C, ultrasound vibration is carried out for 30-120 minutes, and substances in an ultrasonic extraction tank form glue mixed liquor. The glue mixed liquor is sent to a filter sieve with 30-200 meshes and filtered, impurities are eliminated, and the glue mixed liquor with the impurities eliminated is sent to a separation tank. Eventually the gutta-percha is extracted through the method that gutta-percha crystals are precipitated at a low temperature. The method is simple in process, little in pollution, and low in cost; and micro-grinding pretreatment techniques and ultrasonic countercurrent extraction are adopted, the effect is ideal, the extraction rate can reach more than 95%, and the gutta-percha content reaches 99.9%.

Description

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

Technical field

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

Background technology

In China the research and utilization of the bark of eucommia is only limited to Cortex Eucommiae traditionally; Being used as medicine with skin exactly of Chinese medicine middle finger; But it is unfavorable to the growth of tree that gutta-percha tree is got skin for a long time, and the technologies of orbicular decorticating of getting skin requires also higherly, not so very easily causes the death of setting; After getting skin, the regeneration of skin also needs long process.Therefore, from the angle that raw material is learned, be not a good method.

Many scholars' big quantity research shows since the eighties: though there is the difference of different regions and Different Harvesting Time; But Folium Eucommiae and skin on chemical ingredients except that indivedual compositions; Most chemical ingredients basically identical; Have equal effect, the utilization of the bark of eucommia is had very high feasibility with leaf for leatherware.In addition from raw material; The bark of eucommia is a deciduous trees, and the utilization of leaf can be described as utilization of waste material, and this provides more wider advantages for research; Because it is bigger to the demand of herbal medicine; Traditional bark of eucommia medicinal part is a bark, and the bark resource is obviously not enough, with leaf for micromicro to remedy the deficiency of this respect.

Summary of the invention

The present invention provides a kind of and prepares the method for gutta-percha with Folium Eucommiae, adopts natural Folium Eucommiae to process, the molecular weight 40000-60000 of gutta-percha, and the content of gutta-percha: 99.9%, more than the extraction rate reached to 95%.

A kind ofly prepare the method for gutta-percha with Folium Eucommiae, its concrete preparation process is following:

Step 1, Folium Eucommiae put into clear water clean, dry, make in the leaf water cut less than

5%, subsequent use;

Step 2, with step 1 handle well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after the pulverizing is a floss, particle diameter is 10-500 μ m;

Step 3, the Folium Eucommiae particle that step 2 is crushed are sent into the ultrasonic extraction jar, extract, and concrete processing requirements is:

A, elder generation put into petroleum ether solution in the ultrasonic extraction jar, the back adds the Folium Eucommiae particle that crushes, and the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:6-18;

B, open ultrasonic shaking device, shake time 30-120 minute, temperature: 50-75 ℃, make the object in the ultrasonic extraction jar form the colloid mixed solution;

Step 4, the colloid mixeding liquid temperature that step 3 is formed remain on 50 degrees centigrade, send into 30-200 order filter sieve, filter, and remove impurity, after will remove impurity the colloid mixed solution 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 1-12 hour, makes the complete crystalline deposit of colloid in the separating tank;

After the colloidal precipitation in step 6, the separating tank, emit and reclaim the liquid on the colloid top layer, promptly sherwood oil recycles once more, takes out colloid and promptly makes 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 helps crushed material extracts, after micronizing; Outside more natural Chinese gutta percha component is exposed to, for the dissolving of next step organic solvent is got 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 the equipment that extracts, and reduces the usage quantity of organic solvent, effectively improves the extraction efficiency of tree elastomer;

2, leaching process adopts the solvent of single ether conduct, and the characteristics of this solvent low toxicity, environmental protection are used this solvent not have discharge cycle and extracted, 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, adopted advanced ultrasound countercurrent extraction technology, realized high efficiency extraction making its extraction yield more than 95%, the content of gutta-percha reaches 99.9%, and whole separation is put forward the glue process and had and pollute lowly, and the characteristics that productive rate is high realize classification, the rapid extraction of gutta-percha.

Description of drawings

Fig. 1 is the polarizing microscope photo of Folium Eucommiae;

Fig. 1 is not for passing through the polarizing microscope photo of the pretreated Folium Eucommiae of micronizing;

Fig. 2 is the polarizing microscope photo through Folium Eucommiae after the micronizing pre-treatment;

Can find out that from Fig. 1 and Fig. 2 compared to Figure 1 Fig. 2 can observe through Folium Eucommiae after the micronizing pre-treatment and expose the natural Chinese gutta percha of a large amount of crystalline, the micronizing preconditioning technique helps the extraction of gutta-percha.

Fig. 3 is the nmr spectrum of the tree elastomer that extracted.

Embodiment

Embodiment 1

A kind ofly prepare the method for gutta-percha, adopt natural Folium Eucommiae to process with Folium Eucommiae, the molecular weight 40000-60000 of gutta-percha, the content of gutta-percha: 99.9%, its preparation process is following:

5%, subsequent use;

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

A, elder generation put into petroleum ether solution in the ultrasonic extraction jar, the back adds the Folium Eucommiae particle that crushes, and the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:6;

B, open ultrasonic shaking device, 30 minutes vibrations time, temperature: 50 ℃, make the object in the ultrasonic extraction jar form the colloid mixed solution;

Step 4, the colloid mixeding liquid temperature that step 3 is formed remain on 50 degrees centigrade, send into 30 order filter sieve, filter, and remove impurity, after will remove impurity the colloid mixed solution send into separating tank;

After step 5, colloid mixed solution are sent into separating tank, the temperature of separating tank is controlled at 10 ℃, 1 hour time length, makes the complete crystalline deposit of colloid in the separating tank;

Embodiment 2

5%, subsequent use;

Step 2, with step 1 handle well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after the pulverizing is a floss, particle diameter is 300 μ m;

A, elder generation put into petroleum ether solution in the ultrasonic extraction jar, the back adds the Folium Eucommiae particle that crushes, and the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:10;

B, open ultrasonic shaking device, 80 minutes vibrations time, temperature: 60 ℃, make the object in the ultrasonic extraction jar form the colloid mixed solution;

Step 4, the colloid mixeding liquid temperature that step 3 is formed remain on 50 degrees centigrade, send into 100 order filter sieve, filter, and remove impurity, after will remove impurity the colloid mixed solution send into separating tank;

After step 5, colloid mixed solution are sent into separating tank, the temperature of separating tank is controlled at 10 ℃, 6 hours time length, makes the complete crystalline deposit of colloid in the separating tank;

Embodiment 3

5%, subsequent use;

Step 2, with step 1 handle well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after the pulverizing is a floss, particle diameter is 500 μ m;

A, elder generation put into petroleum ether solution in the ultrasonic extraction jar, the back adds the Folium Eucommiae particle that crushes, and the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:18;

B, open ultrasonic shaking device, 120 minutes vibrations time, temperature: 75 ℃, make the object in the ultrasonic extraction jar form the colloid mixed solution;

Step 4, the colloid mixeding liquid temperature that step 3 is formed remain on 50 degrees centigrade, send into 200 order filter sieve, filter, and remove impurity, after will remove impurity the colloid mixed solution send into separating tank;

After step 5, colloid mixed solution are sent into separating tank, the temperature of separating tank is controlled at 10 ℃, 12 hours time length, makes the complete crystalline deposit of colloid in the separating tank;

The experiment of tree elastomer magnetic resonance detection:

Tree elastomer to being extracted has carried out magnetic resonance detection, result such as Fig. 3, and the HNMR collection of illustrative plates shows among Fig. 3; Peak-to-peak signal l.60ppm locating is stronger, and this peak is the proton peak of anti--1,4 structure methyl; 1.67ppm locate almost not have signal, be illustrated in and contain suitable-l in the natural Chinese gutta percha hardly, the proton peak on the 4 structure methyl; Also just explanation contains suitable-l, the 4-TR 301 hardly in the natural Chinese gutta percha that extracts.2.03 the signal indicating at ppm and 1.96 ppm, two places is proton peak of two methylene radical.5.10 the signal at ppm place is the proton peak of two keys in 1,4 structure.The signal that does not have H in 1,2 structure and 3,4 structures among the figure.Amass calculating through the peak, the anti-form-1 that is characterized among the figure, anti--1,4 structural content of 4-TR 301 is 99.9%, cis-1,4-TR 301 structure is 0.1%.

Claims

1. one kind prepares the method for gutta-percha with Folium Eucommiae, adopts natural Folium Eucommiae to process, the molecular weight 40000-60000 of gutta-percha, and the content of gutta-percha: 99.9%, it is characterized in that preparation process is following:

5%, subsequent use;

Step 4, the colloid mixed solution that step 3 is formed are sent into 30-200 order filter sieve, filter, and remove impurity, after will remove impurity the colloid mixed solution 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 1-12 hour, the colloid crystallization in the separating tank is precipitated fully;