CN106750371B - The extracting method of high-purity gutta-percha - Google Patents

The extracting method of high-purity gutta-percha Download PDF

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CN106750371B
CN106750371B CN201611155255.0A CN201611155255A CN106750371B CN 106750371 B CN106750371 B CN 106750371B CN 201611155255 A CN201611155255 A CN 201611155255A CN 106750371 B CN106750371 B CN 106750371B
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percha
gutta
solution
purity
extracting method
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CN106750371A (en
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樊永明
张继川
陈雁聪
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Beijing Forestry University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2307/00Characterised by the use of natural rubber

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention discloses a kind of extracting methods of high-purity gutta-percha, belong to chemical extraction field.The extracting method of the high-purity gutta-percha, raw material are folium cortex eucommiae, eucommia bark and/or Eucommia pericarp, include the following steps: step 1: raw material is mixed with inorganic salt solution;Step 2: organic solvent being added in the above solution, forms water phase-organic phase two-phase system;Step 3: heating stirring is carried out to above-mentioned two-phase system;Step 4: separation organic phase, and organic phase is distilled, obtain the concentrated solution dissolved with gutta-percha;Step 5: freezing processing will be carried out dissolved with the concentrated solution of gutta-percha or mixed with ketone and/or alcoholic solution, gutta-percha is precipitated to get gutta-percha.The characteristics of present invention, which has, does not generate contaminated wastewater, and Folium glue wire structural integrity, the extraction efficiency of extraction be high, purity is high, at low cost, energy conservation and environmental protection.

Description

The extracting method of high-purity gutta-percha
Technical field
The present invention relates to chemical extraction fields, particularly relate to a kind of from folium cortex eucommiae, eucommia bark and/or Eucommia pericarp The middle method for extracting gutta-percha.
Background technique
Cortex Eucommiae is the distinctive single section plant in China, belongs to national two class Rare plants, be distributed mainly on sweet, Shan, Shanxi, The Plain to the hills and mountainous region of height above sea level 1690m of the province such as Henan, Hunan, Hubei Province, river, Yunnan, Guizhou Province, osmanthus, Jiangxi, Fujian, autonomous region, Natural Central exist Central Region.Oneself has more than 500 ten thousand mu to China Cortex Eucommiae woods, accounts for 99% or more world's Cortex Eucommiae cultivated area, has unique money Source advantage.And the eucommia bark seed harvested forms a kind of new resource far more than breeding and afforestation needs.Seed of bark of eucommia is ground at present Study carefully with development and application still in its infancy.
Contain gutta-percha in Folium Eucommiae, skin and seed, mature seed of bark of eucommia gel content highest is 10%~17%.Du Secondary xanthan molecule structure be trans-polyisoprene, have unique " rubber (glue) one (plastics) dual character ", can develop thermoplasticity, Thermoelasticity and caoutchouc elasticity three zones material, application prospect are very wide.Therefore, seed of bark of eucommia has great Development volue. Currently, the extraction of gutta-percha is mainly using folium cortex eucommiae as raw material, lhm2Cortex Eucommiae woods leaf gum yield is about 150kg, and lhm2Seed of bark of eucommia Gum yield can break through 750kg, therefore seed of bark of eucommia is the primary raw material that Cortex Eucommiae mentions glue from now on.Folium glue wire is distributed in seed of bark of eucommia shell dimension In tube bank, only the permeability that gutta-percha peptization goes out just is can be improved in destruction vascular bundle.Previous Extraction Method of Eucommia Rubber, it is mostly sharp Make collodion silk exposure with alkali hydrolysis method, generally destroys vascular bundle lignin with 10%NaOH solution boiling 3h.But alkali is to dimension pipe hydrolysis Slowly, and after hydrolyzing a large amount of industrial wastes are generated, causes severe environmental pollution.
A kind of method that upper silk gutta-percha is extracted from folium cortex eucommiae and skin that Patent No. CN101157827B is provided, first will Folium cortex eucommiae or Bark of Eucommia Ulmoides are processed into small pieces, with NaOH solution dissolve cuticula, then use cellulose hydrolyzation cell wall, then plus Enter petroleum ether solvent, reflux extraction is filtered while hot, and gutta-percha can be obtained in -20-0 DEG C of freezing 30-60min after cooling.Patent A kind of number method that high-purity gutta-percha is extracted from Eucommia provided for CN102977380, need to be first using Mechanical Method point From Cortex Eucommiae pericarp and kernel, complex enzyme formulation is added into Eucommia skin and carries out enzymolysis processing, is molten with petroleum ether after dry Agent extracts the gutta-percha in Eucommia with soxhlet extraction method, and uses ultrasonic wave assisted extraction.
In the prior art, most all to improve dissolution efficiency by crushing raw material.But Folium glue wire is high poly- Object is destroyed to a certain extent under mechanical external force effect, reduces glue elasticity, toughness, tensile strength, limit the application of glue Range.After being handled using the methods of other methods such as enzymatic isolation method, alkali hydrolysis method raw material, then mentioned using organic solvent It takes, there are long flow path, low efficiency, at high cost, waste liquid is more, gutta-percha loses the drawbacks such as larger, recovery rate is low.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of extraction sides of low in cost, environmentally friendly, high-purity gutta-percha Method.
In order to solve the above technical problems, present invention offer technical solution is as follows:
A kind of extracting method of high-purity gutta-percha is provided, raw material is folium cortex eucommiae, eucommia bark and/or Eucommia fruit Skin includes the following steps:
Step 1: raw material is mixed with 20%~80% inorganic salt solution;
Step 2: organic solvent being added in the above solution, forms water phase-organic phase two-phase system;
Step 3: heating stirring is carried out to above-mentioned two-phase system;
Step 4: separation organic phase, and organic phase is distilled, obtain the concentrated solution dissolved with gutta-percha;
Step 5: freezing processing will be carried out dissolved with the concentrated solution of gutta-percha or mixed with ketone and/or alcoholic solution, by gutta-percha Precipitating is to get gutta-percha.
Wherein, in the step 1, inorganic salts are one of calcium chloride, zinc chloride, iron chloride or a variety of.Cellulose is Have glucose group at macromolecular polysaccharide, not soluble in water and common organic solvents are the important composition ingredients of plant cell wall, fine Dimension element can with the metallic ion coordination in calcium chloride, zinc chloride, iron chloride and react, make cellulose dissolution and then divided From.
Wherein, when a variety of compoundings of the inorganic salts, calcium chloride, zinc chloride, iron chloride mixed proportion be 0.5~1:1~ 5:1~6.
Wherein, in the step 1, the weight ratio of raw material and inorganic salt solution is 1:2~15.
Wherein, in the step 2, organic solvent is petroleum ether, toluene, benzene, chloroform, gasoline or kerosene, water phase organic phase Volume ratio be 0.3~2:1.Gutta-percha is natural polymer resources, and the molecular structure of gutta-percha is trans-polyisoprene, molten It is not soluble in water such as hydrocarbon, ether and its derivative in non-polar organic solvent.
Wherein, in the step 3,50~120 DEG C are heated to, speed of agitator is 10~3000rpm, stirs 60~300 points Clock;It is normal pressure or vacuum distillation in the step 4.
Wherein, in the step 5, cryogenic temperature is -15~10 DEG C, 0.5~8h of cooling time.By reducing temperature, make Solubility decline of the gelatin substance in organic phase, is precipitated in the form of precipitating.
Wherein, in the step 5, ketone solution is the ketone compounds comprising carbon atom number 3~5, and alcoholic solution is to include carbon The brothers tertiary alcohol that atomicity is 1~5.
Wherein, in the step 5, ketone solution be aqueous 0-80% ketone compounds solution, ketone compounds be acetone, One of butanone, pentanone, above-mentioned ketone compound isomers are a variety of, and alcoholic solution is that the alcohol compound of aqueous 0-80% is molten Liquid, alcohol compound are methanol, ethyl alcohol, one of propyl alcohol, butanol, amylalcohol, above-mentioned alcohol compound isomers or a variety of.
Wherein, in the step 5, the volume ratio of ketone and/or alcoholic solution and the concentrated solution dissolved with gutta-percha is 1~15:1.
The invention has the following advantages:
In the present invention, the inorganic salt solution being added in raw material can decompose the cellulose in cell wall, improve cell Permeability accelerates the dissolution of intracellular gelatin substance, cooperates organic solvent, while obtaining high yield gutta-percha, obtains day Right, structural integrity, high tenacity filament gutta-percha.Compared with the methods of enzyme process, basic hydrolysis, mechanical crushing, reagent is used At low cost, low to extract equipment requirement, equipment operating cost is cheap, and separates the organic solvent and inorganic salt solvent after gutta-percha It is recyclable to be recycled, it is reused for the extraction of gutta-percha, avoids the pollution to environment.The present invention, which has, does not generate waste water The characteristics of pollution, the not pulverized destruction of the Folium glue wire of extraction, extraction efficiency are high, with high purity, energy conservation and environmental protection.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with specific implementation Example is described in detail.
The present invention is provided at high cost in the prior art, waste liquid is more, gutta-percha loses problem larger, that recovery rate is low A kind of extracting method of the gutta-percha of high-purity low in cost, environmentally friendly, collodion silk structural integrity.
Following instance further illustrates the feature and details of this method, but listed process and data are not meant to this hair The limitation of bright range.
Embodiment 1:
The extracting method of high-purity gutta-percha, comprising the following steps:
(1) ZnCl that Eucommia pericarp 30g and mass fraction are 70% is taken2Solution 300g mixing;
(2) be added boiling range be 60-90 DEG C of petroleum ether 350ml 85 DEG C stirring and leaching 1 hour;
(3) upper layer petroleum ether liquid is taken out, then adds petroleum ether 200ml in raffinate, it is small to continue reflux extraction stirring 2 When;
(4) it takes out upper layer petroleum ether phase and mixes the petroleum ether of evaporation recycling while hot with the resulting petroleum ether solution of step 2 530ml;
(5) the gutta-percha concentrated solution after recycling petroleum ether is added to while hot in the ethyl alcohol of 150ml aqueous 25%, is shut out Secondary glue sediment;
(6) gutta-percha is taken out, spontaneously dries to obtain blocky gutta-percha product;
(7) petroleum ether that evaporation process obtains, which is sent back in extractor, reuses;Ethanol solution carries out essence after using 5 times It evaporates, the petroleum ether being mixed into ethyl alcohol is separated, gained petroleum ether is used for extractor Gutta extraction process, and ethyl alcohol is reused for shutting out Secondary glue precipitation process;
(8) recovery rate is the 18.8% of Eucommia pericarp weight to gutta-percha after measured after drying, purity 94.37%.
Embodiment 2:
(1) FeCl that the dry bark 30g of Cortex Eucommiae and mass fraction are 50% is taken3Aqueous solution 400g mixing;
(2) be added toluene 200ml 65 DEG C stirring and leaching 1 hour;
(3) upper toluene solution is taken out, then adds toluene 100ml in raffinate, continues reflux extraction stirring 2 hours;
(4) it takes out upper toluene solution to mix with toluene solution before, evaporation recycling toluene 280ml;
(5) the toluene concentrated solution after recycling dissolved with gutta-percha is placed in -10 DEG C and stands 1h, gutta-percha is precipitated;
(6) gutta-percha is taken out, spontaneously dries to obtain blocky gutta-percha;
(7) toluene after separating gutta-percha is sent back in extractor, is directly reused;
(8) recovery rate is the 11.3% of dry bark volume to gutta-percha after measured after drying, purity 93.68%.
Embodiment 3:
(1) FeCl that the sub- 30g of Folium Eucommiae and mass fraction are 50% is taken3Solution 150g and 20%CaCl2Solution 150g is mixed It closes;
(2) be added benzene 200ml 95 DEG C stirring and leaching 1 hour;
(3) upper layer benzole soln is taken out, then benzene 100ml is added in raffinate, continues reflux extraction stirring 2 hours;
(4) upper layer benzole soln is taken to mix the benzene 280ml of evaporation recycling while hot with the benzole soln obtained before;
(5) the benzene concentrated solution after recycling dissolved with gutta-percha is slowly added into while hot in aqueous 30% propyl alcohol 200ml, is shut out Secondary glue precipitating;
(6) gutta-percha is taken out, blocky gutta-percha is spontaneously dried to obtain:
(7) benzene that evaporation removal process obtains, which is sent back in extractor, reuses;Propanol solution carries out essence after using 5 times It evaporates, the benzene being mixed into propyl alcohol is separated, gained benzene enters extractor, and propyl alcohol is reused for precipitation process;
(8) recovery rate is the 2.3% of cured leaf weight to gutta-percha after measured after drying, purity 95.2%.
Embodiment 4:
(1) FeCl that Eucommia dry fruit skin 30g and mass fraction are 50% is taken3Solution 100g, 20% CaCl2Solution 100g, 70% ZnCl2100g mixing;
(2) be added chloroform 200ml 100 DEG C stirring and leaching 1 hour;
(3) upper layer chloroformic solution is taken out, then chloroform 100ml is added in raffinate, continues reflux extraction stirring 2 hours;
(4) upper layer gutta-percha chloroformic solution is taken to mix the chloroform of evaporation recycling while hot with the gutta-percha chloroformic solution got before 280ml;
(5) gutta-percha chloroform concentrated solution after the recovery is slowly added into while hot in aqueous 30% acetone soln 200ml, Gutta-percha precipitating;
(6) gutta-percha is taken out, blocky gutta-percha is spontaneously dried to obtain:
(7) chloroform that evaporation removal process obtains, which is sent back in extractor, reuses;Acetone soln carries out essence after using 5 times It evaporates, the chloroform being mixed into acetone is separated, gained chloroform enters extractor, and acetone is reused for precipitation process;
(8) recovery rate is the 17.13% of samara pericarp weight to gutta-percha after measured after drying, purity 98.32%.
Embodiment 5:
(1) FeCl that Folium Eucommiae 30g and mass fraction are 50% is taken3Solution 200g, 70% ZnCl2Solution 100g;
(2) be added toluene 200ml 115 DEG C stirring and leaching 1 hour;
(3) upper toluene is taken out, then toluene 100ml is added in raffinate, continues reflux extraction stirring 2 hours;
(4) upper toluene solution is taken to mix the toluene solution 280ml of evaporation recycling while hot with the toluene taken out before;
(5) the toluene concentrated solution after the recovery dissolved with gutta-percha is slowly added into aqueous 20% acetone 100ml while hot In aqueous 20% ethanol solution 100ml mixed solution (total 200ml), gutta-percha Precipitation;
(6) gutta-percha is taken out, blocky gutta-percha is spontaneously dried to obtain:
(7) toluene that evaporation removal process obtains is sent back in extractor;Acetone/ethanol solution carries out rectifying after using 5 times, The toluene being mixed into acetone/ethanol is separated, gained toluene enters extractor, and acetone/ethanol is reused for precipitation process;
(8) recovery rate is the 2.5% of Folium Eucommiae weight to gutta-percha after measured after drying, purity 95.67%.
Inorganic salt solution used in above-described embodiment can be further processed, and remove non-solute, all be recycled and for shutting out The extraction process of secondary glue avoids the loss of inorganic salts and the pollution to environment.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of extracting method of high-purity gutta-percha, raw material be one of folium cortex eucommiae, eucommia bark, Eucommia pericarp or A variety of combinations, which comprises the steps of:
Step 1: raw material is mixed with 20%~80% inorganic salt solution;
Step 2: organic solvent being added in the above solution, forms water phase-organic phase two-phase system;
Step 3: heating stirring is carried out to above-mentioned two-phase system;
Step 4: separation organic phase, and organic phase is distilled, obtain the concentrated solution dissolved with gutta-percha;
Step 5: freezing processing being carried out dissolved with the concentrated solution of gutta-percha or being mixed with ketone and/or alcoholic solution, gutta-percha is precipitated, Up to gutta-percha.
2. the extracting method of high-purity gutta-percha according to claim 1, which is characterized in that in the step 1, inorganic salts For one of calcium chloride, zinc chloride, iron chloride or a variety of.
3. the extracting method of high-purity gutta-percha according to claim 2, which is characterized in that a variety of compoundings of inorganic salts When, calcium chloride, zinc chloride, iron chloride mixed proportion be 0.5~1:1~5:1~6.
4. the extracting method of high-purity gutta-percha according to claim 1 to 3, which is characterized in that the raw material and nothing The weight ratio of machine saline solution is 1:2~15.
5. the extracting method of high-purity gutta-percha according to claim 1, which is characterized in that in the step 2, You Jirong Agent is petroleum ether, toluene, benzene, chloroform, gasoline or kerosene, and the volume ratio of water phase and organic phase is 0.3~2:1.
6. the extracting method of high-purity gutta-percha according to claim 1, which is characterized in that in the step 3, be heated to 50~120 DEG C, speed of agitator is 10~3000rpm, is stirred 60~300 minutes;In the step 4, the distillation is that normal pressure steams It evaporates or is evaporated under reduced pressure.
7. the extracting method of high-purity gutta-percha according to claim 1, which is characterized in that in the step 5, freezing temperature Degree is -15~10 DEG C, 0.5~8h of cooling time.
8. the extracting method of high-purity gutta-percha according to claim 1, which is characterized in that in the step 5, ketone solution For the ketone compounds comprising carbon atom number 3~5, alcoholic solution is the brothers tertiary alcohol for being 1~5 comprising carbon atom number.
9. the extracting method of high-purity gutta-percha according to claim 1, which is characterized in that in the step 5, ketone solution For the ketone compounds solution of aqueous 0-80%, ketone compounds are acetone, in butanone, pentanone, above-mentioned ketone compound isomers It is one or more, alcoholic solution be aqueous 0-80% alcohol compound solution, alcohol compound be methanol, ethyl alcohol, propyl alcohol, fourth One of alcohol, amylalcohol, above-mentioned alcohol compound isomers are a variety of.
10. according to the extracting method of any high-purity gutta-percha of claim 8-9, which is characterized in that the step 5 In, the volume ratio of ketone and/or alcoholic solution and the concentrated solution dissolved with gutta-percha is 1~15:1.
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* Cited by examiner, † Cited by third party
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CN111748104A (en) * 2020-06-30 2020-10-09 北京林业大学 Two-phase high-efficiency extraction method of gutta-percha
CN111808298A (en) * 2020-07-13 2020-10-23 中国科学院广州能源研究所 Method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis
CN112724420B (en) * 2021-02-01 2022-08-30 福州大学 Method for efficiently extracting high-purity gutta-percha based on ionic liquid and organic solvent biphase
CN113354833A (en) * 2021-07-29 2021-09-07 吉首大学 Method for extracting gutta-percha at ultralow temperature

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* Cited by examiner, † Cited by third party
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CN101157827B (en) * 2007-09-27 2014-03-05 贵州大学 Method for extracting filament gutta-percha from eucommia leaf and skin
CN102977380B (en) * 2012-12-21 2014-04-16 吉首大学 Method for extracting high-purity gutta-percha from cortex eucommiae key fruit
CN103087331B (en) * 2013-01-25 2015-02-11 灵宝金地杜仲产业有限公司 Process for extracting gutta-percha by natural fermentation method
CN104448345A (en) * 2014-11-28 2015-03-25 河南恒瑞源实业有限公司 Method for extracting eucommia ulmoides gum from eucommia ulmoides

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