CN104231281A - Method for extracting and separating eucommia ulmoides rubber - Google Patents
Method for extracting and separating eucommia ulmoides rubber Download PDFInfo
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- CN104231281A CN104231281A CN201410500227.2A CN201410500227A CN104231281A CN 104231281 A CN104231281 A CN 104231281A CN 201410500227 A CN201410500227 A CN 201410500227A CN 104231281 A CN104231281 A CN 104231281A
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Abstract
The invention discloses a method for extracting and separating eucommia ulmoides rubber. The method comprises the following steps: performing pretreatment, performing alkali treatment, performing enzymolysis, and performing extraction and purification. The innovative points are that the step of steam explosion pretreatment is carried out after the step of pretreatment and comprises the following sub-steps: soaking a pretreated material in water with the temperature of 20-30 DEG C for 0-24 hours, and performing steam explosion on the soaked material in a steam explosion device. According to the method, the eucommia ulmoides rubber is extracted and separated by the steam explosion process, the eucommia ulmoides raw material does not need to be excessively ground, the extraction and separation time is short, the oxidation of part of the eucommia ulmoides rubber caused by long-time fermentation is effectively avoided, the natural filament eucommia ulmoides rubber can be obtained, the biological characteristics, physical performance and physical state of a rubber body are kept, and the original molecular structure and polymerization degree are kept; in addition, while the eucommia ulmoides rubber is extracted and separated by the steam explosion pretreatment, eucommia ulmoides polysaccharides are obtained by a membrane concentration and separation technology and the added value of a product is increased.
Description
Technical field:
The invention belongs to natural product Gutta extraction separation field, specifically, a kind of method utilizing steam explosion pre-treatment extraction and isolation gutta-percha from the bark of eucommia.
Background technology:
The bark of eucommia (Eucommia ulmoides Oliv.) is the distinctive famous and precious woody medicinal species of China, be called as " living fossil plant ", also be the Relict Plant in the tertiary period existing only in China, be distributed in more than 20 province (city, autonomous region) in the whole nation, mainly be positioned at that sweet, Shan, Shanxi, Henan, Hunan, Hubei Province, river, Yunnan, Guizhou Province, osmanthus, Jiangxi, Fujian etc. are economized, municipal Plain to the hills of height above sea level 1690 meters and mountain region, Natural Central is in Central Region.Since the eighties in 20th century, under the ever-increasing promotion of natural rubber demand, the exploitation of gutta-percha is as the Important Action adjusting Rubber Industry structure, the substitute gutta-percha of various places active development natural rubber, the cultivated area of the bark of eucommia is impelled sharply to expand, the cultivated area of current China bark of eucommia has developed into about 350,000 hectares, accounts for more than 99% of world's bark of eucommia total amount.Gutta-percha is present in the white filament in each organ Gutta_containing cell of the bark of eucommia, and it is (trans-polyisoprene) a kind of special natural macromolecular material.Along with success natural gutta-percha being changed into trans-polyisoprene vulcanized rubber, make it have the features such as thermoplasticity, insulativity, water tolerance, resistance to acids and bases, will have in various fields and be worth widely.But the output capacity of gutta-percha is low and complicated, the feature such as production cost is high and environmental pollution is serious of leaching process, limits its suitability for industrialized production.
The investigation and application aspect of current gutta-percha, major part research concentrates on the elementary modification of gutta-percha or directly utilizes, as additive, blend components etc., the exploitation of single gutta-percha, cost is high, and difficulty is large, high-valued gutta-percha product is little, and gutta-percha low cost utilization power is pessimistic so far.At present, extracting method such as the high speed water conservancy of gutta-percha is stirred disclosed in the method for washing (Chinese patent 86100216), and the prior fermentation cycle reaches one month, and then with NaOH aqueous solution boiling process.The NaOH consumption that this method expends is too large, and productive rate is low, and the purity of gained glue is not high yet.And solvent-extraction process, as the extracting method of No. ZL00135831.6, patent, mostly be the solvent by low polarity, chloroform, lower boiling sherwood oil, benzene class is extracted, and gutta-percha is dissolved out from vegetable cell, then through adding methyl alcohol, ethanol, acetone, ethyl acetate polar solvent makes colloid separate out.Comparatively clean microbial method (Chinese patent: CN101914211A) extracts gutta-percha, and shortcoming is that the cycle is long, and cost is high, its gutta-percha structural changes in very long fermenting process is serious, deterioration by oxidation, and molecular weight diminishes, foreign matter content is many, has a strong impact on its later use.There is the following shortcoming being difficult to overcome in aforesaid method: 1. directly uses the lixiviate of bark of eucommia starting material, and organic solvent consumption is large, and environmental pollution is serious.If 2. raw material pulverizing is abundant not, colloid can not leach completely, and productive rate is affected.3., after bark of eucommia material disintegrating, the elasticity of gutta-percha, toughness, tensile strength is reduced.The ecosystem gutta-percha of high-polymerization degree can not be obtained.4. facility investment is large, and production cost remains high.Therefore, new bark of eucommia biorefinery pretreatment mode is developed and the gutta-percha separation method based on biorefinery is most important.
In view of the defect that the method for above-mentioned existing bark of eucommia extraction and isolation exists, the present inventor is based on being engaged in the practical experience and expertise that this type of product design manufacture enriches for many years, and coordinate the utilization of scientific principle, actively in addition research and innovation, to founding a kind of method utilizing steam explosion pre-treatment extraction and isolation gutta-percha, utilizing the gutta-percha of the method extraction and isolation, greatly reducing the extraction cost of gutta-percha, by improving general existing Apparatus and method for, it is made to have more practicality.Through constantly research, design, and through repeatedly studying sample and after improving, finally creating the present invention had practical value.
Summary of the invention:
The object of the present invention is to provide a kind of method utilizing steam explosion pre-treatment extraction and isolation gutta-percha, the filament gutta-percha of ecosystem can be obtained.
For solving the problems of the technologies described above, the present invention adopts following technical scheme to realize: a kind of method of extraction and isolation gutta-percha, comprise pre-treatment, alkaline purification, enzymolysis and extraction purification step, its innovative point is: after pre-treatment step, also comprise steam explosion pre-treatment step, material after pre-treatment is placed in the water of 20 ~ 30 DEG C and soaks 0 ~ 24h, then the material after immersion is put into steam blasting device and carry out steam explosion.
Further, the method for described extraction and isolation gutta-percha comprises the following steps:
(1) pre-treatment: by bark of eucommia raw material, impurity elimination process, being crushed to particle diameter is 1 ~ 15cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion pre-treatment: the material after pre-treatment is placed in the water of 20 ~ 30 DEG C and soaks 0 ~ 24h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 0.5 ~ 1.8MPa, temperature when controlling the steam explosion of steam blasting device is 140 ~ 180 DEG C, and tie up pressure 1 ~ 15min, after steam explosion, temperature of charge is room temperature;
(3) alkaline purification: adopt NaOH solution to extract twice filter residue of step (2), merge twice filtrate, salt acid for adjusting pH to 5.5 ~ 6.0, after volume membrane concentration, concentrated solution is poured in ethanolic soln, separate out eucommia bark polycose, filter, be separated eucommia bark polycose, drying, obtains finished product eucommia bark polycose;
(4) enzymolysis: the filter residue in step (3) is added distilled water, with vinegar acid for adjusting pH to 4.8 ~ 5.2, after then adding combinative enzyme hydrolysis, rinses lignin residue, obtains the thick glue of the bark of eucommia;
(5) extraction purification: mix with sherwood oil after the thick glue drying treatment of bark of eucommia step (4) obtained, condensation is extracted, heat filtering removal of impurities, and filtered liquid refrigerates, and separates out gutta-percha, reclaims sherwood oil, and vacuum-drying obtains bark of eucommia essence glue.
Further, described step (3) is specially: by the filter residue of step (2) and the NaOH solution of 0.5 ~ 4%, according to the ratio mixing that solid-liquid ratio is 1:5 ~ 1:20, 1 ~ 3h is extracted under 60 ~ 80 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:5 ~ 1:15, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, with the salt acid for adjusting pH 5.5 ~ 6.0 of 4 ~ 8mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.2 ~ 0.3Mpa, until concentrated solution density is after 1.10 ~ 1.15g/mL, again concentrated solution is poured in the ethanolic soln of 2 ~ 3 times of volumes 95%, separate out eucommia bark polycose, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 1000 ~ 5000D, utilize the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained.
Further, described eucommia bark polycose mainly comprises rhamnosan >=1.66%, arabinan >=6.72%, mannosans >=4.11%, dextran >=6.42%, xylan >=4.75%, glucuronic acid >=1.65%.
Further, described step (4) is specially: the filter residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:10 ~ 1:40, pH to 4.8 ~ 5.2 are regulated with sodium-acetate, then the prozyme of 30 ~ 100IU/g is added, under 48 ~ 52 DEG C of conditions, after combinative enzyme hydrolysis 36 ~ 84h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 100bar ~ 800bar, obtains the thick glue of the bark of eucommia.
Further, described prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g and beta-glucanase >=11000IU/g.
Further, described step (5) is specially: after the thick glue of bark of eucommia step (4) obtained carries out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:5 ~ 1:20, under 80 ~ 85 DEG C of conditions, 1 ~ 4h is extracted in condensation, heat filtering removes impurity, by liquid at-4 ~-20 DEG C of refrigeration 0.5 ~ 3h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
Effect of the present invention:
1, the present invention utilizes steam explosion extraction and isolation gutta-percha, over grind need not be carried out to Cortex Eucommiae, the extraction and isolation time is short, effectively prevent because lengthy fermentation causes part gutta-percha oxidized, the filament gutta-percha of ecosystem can be obtained, maintain the biological nature of colloid, physicals and physical condition, keep original molecular structure and the polymerization degree.
2, the present invention utilizes eucommia bark for raw material, extracts eucommia bark polycose and gutta-percha continuously, and introduce membrane technique and carry out operations such as being separated, concentrate, can improve quality and the yield of eucommia bark polycose, filtering and impurity removing is abundant, and required time is short, and extraction and isolation temperature is low.
3, the extract residue after eucommia bark polycose is extracted in the present invention, gutta-percha is extracted through enzymic hydrolysis, greatly reduce the extraction cost of gutta-percha, processing step is few, and equipment is simple, easy to operate, have with short production cycle, pollute little, the advantages such as production cost is low, are conducive to the suitability for industrialized production of gutta-percha.
4, the present invention is while extraction and isolation gutta-percha, obtains eucommia bark polycose, improves value-added content of product, reduces the Cost Problems in Gutta extraction process, develops the high-valued extraction and separation method of gutta-percha based on biorefinery.
Accompanying drawing illustrates:
Fig. 1 is the method schematic diagram of steam explosion pre-treatment extraction and isolation gutta-percha in the embodiment of the present invention.
Embodiment:
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is elaborated.
The method of a kind of extraction and isolation gutta-percha of the present invention, comprise pre-treatment, alkaline purification, enzymolysis and extraction purification step, after pre-treatment step, also comprise steam explosion pre-treatment step, material after pre-treatment is placed in the water of 20 ~ 30 DEG C and soaks 0 ~ 24h, then the material after immersion is put into steam blasting device and carry out steam explosion.
Embodiment 1:
A method for extraction and isolation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after impurity elimination process, according to the specification of quality of Chinese Pharmacopoeia, through being up to the standards, suitably pulverized by the eucommia bark machinery of drying, granularity is 1cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion: the material handled well in step (1) is put into steam blasting device and carries out steam explosion, the pressure of steam explosion is 0.5MPa, temperature when controlling the steam explosion of steam blasting device is 140 DEG C, and dimension pressure 15min, after steam explosion, temperature of charge is room temperature;
(3) by the filter residue in step (2) and 0.5% NaOH solution, according to the ratio mixing that solid-liquid ratio is 1:5, 3h is extracted under 60 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:15, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, with the salt acid for adjusting pH 5.5 of 4mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.2Mpa, until concentrated solution density is after 1.10g/mL, again concentrated solution is poured in the ethanolic soln of 2 times of volumes 95%, after eucommia bark polycose is separated out, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 1000D, polysaccharide utilizes the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained,
(4) enzymolysis: the filter residue in step (3) is added distilled water according to the ratio of solid-liquid ratio 1:10, regulate pH to 4.8 with sodium-acetate, then add the prozyme of 30IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g composition, under 48 DEG C of conditions, after hydrolysis 84h, utilize high-pressure cleaning device to rinse lignin residue, hydraulic pressure 100bar, obtains the thick glue of the bark of eucommia;
(5) extraction purification: after the thick glue of the bark of eucommia in step (4) is carried out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:5, under 80 DEG C of conditions, 4h is extracted in condensation, heat filtering removes impurity, by liquid at-4 DEG C of refrigeration 3h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
Embodiment 2:
A method for extraction and isolation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after impurity elimination process, according to the specification of quality of Chinese Pharmacopoeia, through being up to the standards, suitably pulverized by the eucommia bark machinery of drying, granularity is 10cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion: the material handled well in step (1) is put into steam blasting device and carries out steam explosion, the pressure of steam explosion is 1.2MPa, temperature when controlling the steam explosion of steam blasting device is 160 DEG C, and dimension pressure 8min, after steam explosion, temperature of charge is room temperature;
(3) by the filter residue in step (2) and 2% NaOH solution, according to the ratio mixing that solid-liquid ratio is 1:10, 2h is extracted under 70 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:5, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, with the salt acid for adjusting pH 6 of 6mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.2Mpa, until concentrated solution density is after 1.12g/mL, again concentrated solution is poured in the ethanolic soln of 2.5 times of volumes 95%, after eucommia bark polycose is separated out, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 3000D, polysaccharide utilizes the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained,
(4) enzymolysis: the filter residue in step (3) is added distilled water according to the ratio of solid-liquid ratio 1:25, regulate pH to 5.0 with sodium-acetate, then add the prozyme of 60IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g composition, under 49 DEG C of conditions, after combinative enzyme hydrolysis 48h, utilize high-pressure cleaning device to rinse lignin residue, hydraulic pressure 500bar, obtains the thick glue of the bark of eucommia;
(5) extraction purification: after the thick glue of the bark of eucommia in step (4) is carried out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:10, under 83 DEG C of conditions, 2.5h is extracted in condensation, heat filtering removes impurity, by liquid at-10 DEG C of refrigeration 2h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
Embodiment 3:
A method for extraction and isolation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after impurity elimination process, according to the specification of quality of Chinese Pharmacopoeia, through being up to the standards, suitably pulverized by the eucommia bark machinery of drying, granularity is 5cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion: the material handled well in step (1) is put into steam blasting device and carries out steam explosion, the pressure of steam explosion is 1.8MPa, temperature when controlling the steam explosion of steam blasting device is 180 DEG C, and dimension pressure 1min, after steam explosion, temperature of charge is room temperature;
(3) by the filter residue in step (2) and 4% NaOH solution, according to the ratio mixing that solid-liquid ratio is 1:20, 1h is extracted under 80 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:10, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, with the salt acid for adjusting pH 6.0 of 8mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.3Mpa, until concentrated solution density is after 1.15g/mL, again concentrated solution is poured in the ethanolic soln of 3 times of volumes 95%, after eucommia bark polycose is separated out, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 5000D, polysaccharide utilizes the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained,
(4) enzymolysis: the filter residue in step (3) is added distilled water according to the ratio of solid-liquid ratio 1:40, regulate pH to 5.2 with sodium-acetate, then add the prozyme of 100IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g composition, under 50 DEG C of conditions, after combinative enzyme hydrolysis 36h, utilize high-pressure cleaning device to rinse lignin residue, hydraulic pressure 800bar, obtains the thick glue of the bark of eucommia;
(5) extraction purification: after the thick glue of the bark of eucommia in step (4) is carried out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:20, under 85 DEG C of conditions, 1h is extracted in condensation, heat filtering removes impurity, by liquid at-20 DEG C of refrigeration 0.5h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
Embodiment 4:
A method for extraction and isolation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after impurity elimination process, according to the specification of quality of Chinese Pharmacopoeia, through being up to the standards, suitably pulverized by the eucommia bark machinery of drying, granularity is 12cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion: the material after pre-treatment is put into steam blasting device and carries out steam explosion, the pressure of steam explosion is 1.0MPa, temperature when controlling the steam explosion of steam blasting device is 150 DEG C, and dimension pressure 3min, after steam explosion, temperature of charge is room temperature;
(3) by the filter residue of step (2) and the NaOH solution of 1%, according to the ratio mixing that solid-liquid ratio is 1:15, 2.5h is extracted under 65 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:8, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, pH5.7 is regulated with the hydrochloric acid of 5mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.22Mpa, until concentrated solution density is after 1.11g/mL, again concentrated solution is poured in the ethanolic soln of 2.2 times of volumes 95%, separate out eucommia bark polycose, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 2000D, polysaccharide utilizes the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained,
(4) enzymolysis: the filter residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:20, pH to 4.9 is regulated with sodium-acetate, then add the prozyme of 50IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g and beta-glucanase >=11000IU/g, under 51 DEG C of conditions, after combinative enzyme hydrolysis 60h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 500bar, obtains the thick glue of the bark of eucommia;
(5) after the thick glue of the bark of eucommia that step (4) obtains being carried out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:8, under 82 DEG C of conditions, 3h is extracted in condensation, heat filtering removes impurity, by liquid at-8 DEG C of refrigeration 2.5h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
Embodiment 5:
A method for extraction and isolation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after impurity elimination process, according to the specification of quality of Chinese Pharmacopoeia, through being up to the standards, suitably pulverized by the eucommia bark machinery of drying, granularity is 15cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion: the material after pre-treatment is placed in the water of 26 DEG C and soaks 16h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 1MPa, temperature when controlling the steam explosion of steam blasting device is 170 DEG C, and dimension pressure 12min, after steam explosion, temperature of charge is room temperature;
(3) by the filter residue of step (2) and the NaOH solution of 3.2%, according to the ratio mixing that solid-liquid ratio is 1:14, 1.5h is extracted under 72 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:12, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, with the salt acid for adjusting pH 5.8 of 7mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.28Mpa, until concentrated solution density is after 1.14g/mL, again concentrated solution is poured in the ethanolic soln of 2.8 times of volumes 95%, separate out eucommia bark polycose, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 1400D, polysaccharide utilizes the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained,
(4) enzymolysis: the filter residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:35, pH to 5.1 is regulated with sodium-acetate, then add the prozyme of 70IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g and beta-glucanase >=11000IU/g, under 52 DEG C of conditions, after combinative enzyme hydrolysis 72h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 500bar, obtains the thick glue of the bark of eucommia;
(5) after the thick glue of the bark of eucommia that step (4) obtains being carried out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:16, under 84 DEG C of conditions, 2h is extracted in condensation, heat filtering removes impurity, by liquid at-14 DEG C of refrigeration 1.5h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
Embodiment 6:
A method for extraction and isolation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after impurity elimination process, according to the specification of quality of Chinese Pharmacopoeia, through being up to the standards, suitably pulverized by the eucommia bark machinery of drying, granularity is 4cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion: the material after pre-treatment is placed in the water of 27 DEG C and soaks 20h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 1.5MPa, temperature when controlling the steam explosion of steam blasting device is 172 DEG C, and dimension pressure 14min, after steam explosion, temperature of charge is room temperature;
(3) by the filter residue of step (2) and the NaOH solution of 3.6%, according to the ratio mixing that solid-liquid ratio is 1:18, 1.2h is extracted under 78 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:15, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, with the salt acid for adjusting pH 5.9 of 7.5mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.26Mpa, until concentrated solution density is after 1.13g/mL, again concentrated solution is poured in the ethanolic soln of 2.7 times of volumes 95%, separate out eucommia bark polycose, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 4500D, polysaccharide utilizes the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained,
(4) enzymolysis: the filter residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:25, pH to 5.1 is regulated with sodium-acetate, then add the prozyme of 80IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g and beta-glucanase >=11000IU/g, under 51 DEG C of conditions, after combinative enzyme hydrolysis 80h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 500bar, obtains the thick glue of the bark of eucommia;
(5) after the thick glue of the bark of eucommia that step (4) obtains being carried out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:15, under 81 DEG C of conditions, 2h is extracted in condensation, heat filtering removes impurity, by liquid at-15 DEG C of refrigeration 1.5h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, when the method and technology contents that can utilize above-mentioned announcement are made a little change or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (7)
1. the method for an extraction and isolation gutta-percha, comprise pre-treatment, alkaline purification, enzymolysis and extraction purification step, it is characterized in that: after pre-treatment step, also comprise steam explosion pre-treatment step, material after pre-treatment is placed in the water of 20 ~ 30 DEG C and soaks 0 ~ 24h, then the material after immersion is put into steam blasting device and carry out steam explosion.
2. the method for a kind of extraction and isolation gutta-percha according to claim 1, is characterized in that: the method for described extraction and isolation gutta-percha comprises the following steps:
(1) pre-treatment: by bark of eucommia raw material, impurity elimination process, being crushed to particle diameter is 1 ~ 15cm, is placed in dry shady and cool place for subsequent use;
(2) steam explosion pre-treatment: the material after pre-treatment is placed in the water of 20 ~ 30 DEG C and soaks 0 ~ 24h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 0.5 ~ 1.8MPa, temperature when controlling the steam explosion of steam blasting device is 140 ~ 180 DEG C, dimension pressure 1 ~ 15min, after steam explosion, temperature of charge is room temperature;
(3) alkaline purification: adopt NaOH solution to extract twice filter residue of step (2), merge twice filtrate, salt acid for adjusting pH to 5.5 ~ 6.0, after volume membrane concentration, concentrated solution is poured in ethanolic soln, separate out eucommia bark polycose, filter, be separated eucommia bark polycose, drying, obtains finished product eucommia bark polycose;
(4) enzymolysis: the filter residue in step (3) is added distilled water, with vinegar acid for adjusting pH to 4.8 ~ 5.2, then adds combinative enzyme hydrolysis, rinses lignin residue, obtains the thick glue of the bark of eucommia;
(5) extraction purification: mix with sherwood oil after the thick glue drying treatment of bark of eucommia step (4) obtained, condensation is extracted, heat filtering removal of impurities, and filtered liquid refrigerates, and separates out gutta-percha, reclaims sherwood oil, and vacuum-drying obtains bark of eucommia essence glue.
3. the method for a kind of extraction and isolation gutta-percha according to claim 2, it is characterized in that: described step (3) is specially: by the filter residue of step (2) and the NaOH solution of 0.5 ~ 4%, according to the ratio mixing that solid-liquid ratio is 1:5 ~ 1:20, 1 ~ 3h is extracted under 60 ~ 80 DEG C of conditions, after filtration, pump is to receiver, during second extraction, mix according to the solid-liquid ratio of 1:5 ~ 1:15, Extracting temperature is identical with first time with the time, separating filtrate, filter residue stores for future use, after merging twice filtrate, with the salt acid for adjusting pH 5.5 ~ 6.0 of 4 ~ 8mol/L, utilize the volume membrane concentration being 300D by molecular weight, top hole pressure 0.2 ~ 0.3Mpa, until concentrated solution density is after 1.10 ~ 1.15g/mL, again concentrated solution is poured in the ethanolic soln of 2 ~ 3 times of volumes 95%, separate out eucommia bark polycose, the method separating polyose that application periosteum filters, wherein periosteum molecular weight cut-off 1000 ~ 5000D, polysaccharide utilizes the method for vacuum lyophilization dry, namely finished product eucommia bark polycose is obtained.
4. the method for a kind of extraction and isolation gutta-percha according to claim 2 and 3, it is characterized in that: described eucommia bark polycose mainly comprises rhamnosan >=1.66%, arabinan >=6.72%, mannosans >=4.11%, dextran >=6.42%, xylan >=4.75%, glucuronic acid >=1.65%.
5. the method for a kind of extraction and isolation gutta-percha according to claim 2, it is characterized in that: described step (4) is specially: the filter residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:10 ~ 1:40, pH to 4.8 ~ 5.2 are regulated with sodium-acetate, then the prozyme of 30 ~ 100IU/g is added, under 48 ~ 52 DEG C of conditions, after combinative enzyme hydrolysis 36 ~ 84h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 100bar ~ 800bar, obtains the thick glue of the bark of eucommia.
6. the method for a kind of extraction and isolation gutta-percha according to claim 4, is characterized in that: described prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g and beta-glucanase >=11000IU/g.
7. the method for a kind of extraction and isolation gutta-percha according to claim 2, it is characterized in that: described step (5) is specially: after the thick glue of bark of eucommia step (4) obtained carries out drying treatment, according to ratio and sherwood oil (boiling range: 60 ~ 90 DEG C) mixing of solid-liquid ratio 1:5 ~ 1:20, under 80 ~ 85 DEG C of conditions, 1 ~ 4h is extracted in condensation, heat filtering removes impurity, by liquid at-4 ~-20 DEG C of refrigeration 0.5 ~ 3h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479143A (en) * | 2014-11-26 | 2015-04-01 | 国家林业局泡桐研究开发中心 | Method for separating and extracting eucommia ulmoides rubber through supersonic steam explosion |
| CN105111465A (en) * | 2015-09-23 | 2015-12-02 | 成都艾比科生物科技有限公司 | Method for extracting filament gutta-percha from eucommia ulmoides by adopting solvent method |
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| CN106107341A (en) * | 2016-06-24 | 2016-11-16 | 广西灵山县宇峰保健食品有限公司 | A kind of Herba mesonae chinensis beverage and preparation method thereof |
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| CN113801341A (en) * | 2020-06-15 | 2021-12-17 | 广州中国科学院先进技术研究所 | Method for extracting, concentrating and recovering organic solvent from gutta-percha |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351700A (en) * | 2011-08-15 | 2012-02-15 | 中国科学院过程工程研究所 | Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves |
| CN102977380A (en) * | 2012-12-21 | 2013-03-20 | 吉首大学 | Method for extracting high-purity gutta-percha from cortex eucommiae key fruit |
-
2014
- 2014-09-26 CN CN201410500227.2A patent/CN104231281B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351700A (en) * | 2011-08-15 | 2012-02-15 | 中国科学院过程工程研究所 | Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves |
| CN102977380A (en) * | 2012-12-21 | 2013-03-20 | 吉首大学 | Method for extracting high-purity gutta-percha from cortex eucommiae key fruit |
Non-Patent Citations (1)
| Title |
|---|
| 何国菊: "杜仲籽中油和杜仲胶的提取工艺研究", 《贵阳学院学报(自然科学版) (季刊)》 * |
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