CN102838758B - Method of preparing gutta-percha with eucommia leaves - Google Patents

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 Folium Eucommiae prepares the method for gutta-percha

Technical field

The present invention relates to a kind of extracting method of natural product, is a kind of method that Folium Eucommiae prepares gutta-percha specifically.

Background technology

Research and utilization in China to the bark of eucommia is only limitted to Cortex Eucommiae traditionally, being used as medicine with skin exactly of Chinese medicine middle finger, but it is unfavorable to the growth of setting to get skin for a long time to gutta-percha tree, and the technologies of orbicular decorticating getting skin requires also higher, not so the death of setting very easily is caused, after getting skin, the regeneration of skin also needs a longer process.Therefore, from the angle of raw material, be not a good method.

Since the eighties, the large quantity research of many scholars shows: although there is the difference of different geographical and Different Harvesting Time, but Folium Eucommiae and skin in chemical composition except individual components, most chemical composition is basically identical, there is equivalent efficacy, have very high feasibility with leaf for leatherware to the utilization of the bark of eucommia.In addition from raw material, the bark of eucommia is deciduous trees, utilization of waste material be can be described as to the utilization of leaf, this provides more wider advantages for studying, due to larger to the demand of herbal medicine, traditional bark of eucommia medicinal part is bark, and bark resource is obviously not enough, with leaf for micromicro to make up the deficiency of this respect.

Summary of the invention

The invention provides a kind of method that Folium Eucommiae prepares gutta-percha, adopt natural Folium Eucommiae to make, the molecular weight 40000-60000 of gutta-percha, the content of gutta-percha: 99.9%, extraction rate reached is to more than 95%.

Folium Eucommiae prepares a method for gutta-percha, and its concrete preparation process is as follows:

Step one, Folium Eucommiae put into clear water and clean, dry, the water content in leaf is less than

5%, for subsequent use;

Step 2, step one is handled well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after pulverizing is floss, and particle diameter is 10-500 μm;

Step 3, Folium Eucommiae particle step 2 crushed send into ultrasonic extraction tank, and extract, concrete processing requirements is:

A, first in ultrasonic extraction tank, put into petroleum ether solution, after add the Folium Eucommiae particle crushed, the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:6-18;

B, unlatching ultrasonic vibration device, vibrations time 30-120 minute, temperature: 50-75 DEG C, makes the object in ultrasonic extraction tank form colloid mixed solution;

Step 4, the colloid mixeding liquid temperature that step 3 is formed is remained on 50 degrees Celsius, sends into 30-200 order filter sieve, filter, remove impurity, after deimpurity colloid mixed solution will be gone to send into separating tank;

The temperature of separating tank controls at 10 DEG C, time length 1-12 hour, makes the complete crystalline deposit of the colloid in separating tank after sending into separating tank by step 5, colloid 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 crushed material 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, can reduce the volume of extraction equipment, reduces the usage quantity of organic solvent, effectively improves the extraction efficiency of natural rubber;

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, realize high efficiency extraction, 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, realizes the classification of gutta-percha, rapid extraction.

Accompanying drawing explanation

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

Fig. 1 is the polarizing microscope photo without the pretreated Folium Eucommiae of micronizing;

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

As can be seen from Fig. 1 and Fig. 2, compared to Figure 1 Fig. 2 can observe the natural Chinese gutta percha that Folium Eucommiae after micronizing pre-treatment exposes a large amount of crystallizations, and micronizing preconditioning technique is conducive to the extraction of gutta-percha.

Fig. 3 is the nmr spectrum of extracted natural rubber.

Embodiment

embodiment 1

Folium Eucommiae prepares a method for gutta-percha, adopts natural Folium Eucommiae to make, the molecular weight 40000-60000 of gutta-percha, the content of gutta-percha: 99.9%, and its preparation process is as follows:

Step one, Folium Eucommiae put into clear water and clean, dry, the water content in leaf is less than

5%, for subsequent use;

Step 2, step one is handled well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after pulverizing is floss, and particle diameter is 10 μm;

Step 3, Folium Eucommiae particle step 2 crushed send into ultrasonic extraction tank, and extract, concrete processing requirements is:

A, first in ultrasonic extraction tank, put into petroleum ether solution, after add the Folium Eucommiae particle crushed, the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:6;

B, unlatching ultrasonic vibration device, the 30 minutes time of vibrations, temperature: 50 DEG C, makes the object in ultrasonic extraction tank form colloid mixed solution;

Step 4, by step 3 formed colloid mixeding liquid temperature remain on 50 degrees Celsius, send into 30 order filter sieve, filter, remove impurity, after will go deimpurity colloid mixed solution send into separating tank;

The temperature of separating tank controls at 10 DEG C, 1 hour time length, makes the complete crystalline deposit of the colloid in separating tank after sending into separating tank by step 5, colloid 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

Folium Eucommiae prepares a method for gutta-percha, adopts natural Folium Eucommiae to make, the molecular weight 40000-60000 of gutta-percha, the content of gutta-percha: 99.9%, and its preparation process is as follows:

Step one, Folium Eucommiae put into clear water and clean, dry, the water content in leaf is less than

5%, for subsequent use;

Step 2, step one is handled well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after pulverizing is floss, and particle diameter is 300 μm;

Step 3, Folium Eucommiae particle step 2 crushed send into ultrasonic extraction tank, and extract, concrete processing requirements is:

A, first in ultrasonic extraction tank, put into petroleum ether solution, after add the Folium Eucommiae particle crushed, the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:10;

B, unlatching ultrasonic vibration device, the 80 minutes time of vibrations, temperature: 60 DEG C, makes the object in ultrasonic extraction tank form colloid mixed solution;

Step 4, by step 3 formed colloid mixeding liquid temperature remain on 50 degrees Celsius, send into 100 order filter sieve, filter, remove impurity, after will go deimpurity colloid mixed solution send into separating tank;

The temperature of separating tank controls at 10 DEG C, 6 hours time length, makes the complete crystalline deposit of the colloid in separating tank after sending into separating tank by step 5, colloid 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

Folium Eucommiae prepares a method for gutta-percha, adopts natural Folium Eucommiae to make, the molecular weight 40000-60000 of gutta-percha, the content of gutta-percha: 99.9%, and its preparation process is as follows:

Step one, Folium Eucommiae put into clear water and clean, dry, the water content in leaf is less than

5%, for subsequent use;

Step 2, step one is handled well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after pulverizing is floss, and particle diameter is 500 μm;

Step 3, Folium Eucommiae particle step 2 crushed send into ultrasonic extraction tank, and extract, concrete processing requirements is:

A, first in ultrasonic extraction tank, put into petroleum ether solution, after add the Folium Eucommiae particle crushed, the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:18;

B, unlatching ultrasonic vibration device, the 120 minutes time of vibrations, temperature: 75 DEG C, makes the object in ultrasonic extraction tank form colloid mixed solution;

Step 4, by step 3 formed colloid mixeding liquid temperature remain on 50 degrees Celsius, send into 200 order filter sieve, filter, remove impurity, after will go deimpurity colloid mixed solution send into separating tank;

The temperature of separating tank controls at 10 DEG C, 12 hours time length, makes the complete crystalline deposit of the colloid in separating tank after sending into separating tank by step 5, colloid 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. 3, HNMR collection of illustrative plates display in Fig. 3, 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. prepare a method for gutta-percha with Folium Eucommiae, adopt natural Folium Eucommiae to make, the molecular weight 40000-60000 of gutta-percha, the content of gutta-percha: 99.9%, is characterized in that preparation process is as follows:

Step one, Folium Eucommiae put into clear water and clean, dry, make the water content in leaf be less than 5%, for subsequent use;

Step 2, step one is handled well Folium Eucommiae send into supper micron mill, carry out micronizing, the particle after pulverizing is floss, and particle diameter is 300-500 μm;

Step 3, Folium Eucommiae particle step 2 crushed send into ultrasonic extraction tank, and extract, concrete processing requirements is:

A, first in ultrasonic extraction tank, put into petroleum ether solution, after add the Folium Eucommiae particle crushed, the weight ratio that Folium Eucommiae particle and petroleum ether solution add is: 1:6-18;

B, unlatching ultrasonic vibration device, vibrations time 30-120 minute, temperature: 50 DEG C, makes the object in ultrasonic extraction tank form colloid mixed solution;

Step 4, the colloid mixeding liquid temperature that step 3 is formed is remained on 50 degrees Celsius, sends into 30-200 order filter sieve, filter, remove impurity, after deimpurity colloid mixed solution will be gone to send into separating tank;

The temperature of separating tank controls at 10 DEG C, time length 1-12 hour, the colloid crystallization in separating tank is precipitated completely after sending into separating tank by step 5, colloid 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.