CN104231282A - Method for extracting and separating eucommia seed oil and eucommia gum from eucommia samaras - Google Patents
Method for extracting and separating eucommia seed oil and eucommia gum from eucommia samaras Download PDFInfo
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Abstract
The invention discloses a method for extracting and separating eucommia seed oil and eucommia gum from eucommia samaras. The method comprises the following steps: processing the eucommia samaras to separate shells from kernels; performing steam explosion, enzymolysis, extracting and purifying on the shells to obtain the eucommia gum; crushing, extracting and separating the kernels to obtain the eucommia seed oil. In the method, the eucommia samaras are taken as raw materials for extracting the eucommia gum and the eucommia seed oil, and a membrane technology is introduced for implementing separation, so that the product quality and the yield can be improved, impurities can be fully removed through filtering, the needed time is short, and the extraction and separation temperature is low. The steam explosion is performed on the shells of the eucommia samaras for extracting and separating the eucommia gum, the eucommia seed oil is extracted by a supercritical CO2 technology, and residues obtained after extraction of the eucommia seed oil are used as raw materials of a bio-organic fertilizer, so that comprehensive development and utilization of the eucommia samaras are effectively realized, the cost during the development process of the eucommia gum is reduced and a high-value utilization way of the eucommia samaras is developed.
Description
Technical field:
The invention belongs to natural product Gutta extraction separation field, specifically, a kind of method of extraction and isolation eucommia ulmoides seed oil and gutta-percha from 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, various places are using the Important Action of the substitute gutta-percha of exploitation natural rubber as adjustment Rubber Industry structure, cultivating eucommia area 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, wherein, Folium Eucommiae is containing glue 2 ~ 4wt%, Cortex Eucommiae gel content 8 ~ 10wt%, seed of bark of eucommia is containing glue 10 ~ 15wt%, 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, acid-fast alkali-proof, will have in various fields and be worth widely.Extraction and isolation gutta-percha from Cortex Eucommiae gel content and samara, it will be the main raw material source of gutta-percha industry, 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, seriously limits its suitability for industrialized production.
Containing important component such as eucommia ulmoides seed oil, gutta-percha and pectin in Eucommia, eucommia ulmoides seed oil oleaginousness is about 10wt%, wherein unsaturated fatty acid content is 91.18%, employing capillary gas chromatography, mass spectrometry combination method are analyzed the lipid acid (with methyl ester form) in the bark of eucommia, identify 10 kinds of lipid acid, lipid acid consists of linolenic acid 67.38%, linolic acid 9.97%, oleic acid 15.81%, stearic acid 2.15%.Palmitinic acid 4.68%.Unique antihyperglycemic antisenescence effect had in human body due to it and cause the extensive attention of people.In Eucommia, gel content is higher in addition, but extraction cost is higher.Therefore, the higher value application of Eucommia resource is the great difficult problem of bark of eucommia area research and industry member thereof always, especially as the investigation and application aspect of macromolecular material gutta-percha, major part research at present 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 visible 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.The microbial method (Chinese patent: CN101914211A) that application is comparatively cleaned 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 of the method existence that above-mentioned existing Gutta extraction is separated, found the method for the high-valued extraction and isolation of a kind of new bark of eucommia, a kind of gutta-percha utilized in steam explosion pre-treatment extraction and isolation Eucommia shell, use seed of bark of eucommia extraction and isolation eucommia ulmoides seed oil simultaneously, the dregs of fat after extraction and isolation are as the raw material preparing biological organic fertilizer, the method extraction and isolation is utilized to go out gutta-percha, greatly reduce the extraction and isolation cost of gutta-percha, by improving existing Apparatus and method for, it is made to have more practicality.
Summary of the invention:
The object of the invention is to for deficiency of the prior art, provide a kind of method of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia, improve the quality of products and yield, the time is short.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia, for being processed by Eucommia, being separated kind of shell and planting benevolence; Plant shell and obtain gutta-percha through steam explosion, enzymolysis and extraction purification step; Plant benevolence and obtain eucommia ulmoides seed oil through pulverizing, extraction, separating step.
2, the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 1, is characterized in that: described method specifically comprises the following steps:
(1) pre-treatment: take Eucommia as raw material, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator, is separated kind of shell and plants benevolence;
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: kind shell step (1) obtained carries out Steam explosion treatment after soaking;
B, enzymolysis: after the filter residue in step a adds prozyme, carry out enzymic hydrolysis, rinses, obtain the thick glue of the bark of eucommia;
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, mix with sherwood oil, then condensation is extracted, and filters, and separates out gutta-percha, dry bark of eucommia essence glue;
B, eucommia ulmoides seed oil are separated
A, extraction: seed of bark of eucommia utilizes the CO of supercritical state after pulverizing
2extraction, is separated seed of bark of eucommia plant milk extract;
B, filtration: the extract obtained by extraction and isolation in step a, after concentrate drying, makes moisture lower than 10%, more namely removal of impurities filtration obtains eucommia ulmoides seed oil.
Further, described gutta-percha is separated a step kind shell Steam explosion treatment and is specially: be placed on by the kind shell that step (1) obtains in the water of 20 ~ 30 DEG C and soak 0 ~ 12h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 0.5 ~ 1.5MPa, temperature when controlling the steam explosion of steam blasting device is 140 ~ 180 DEG C, dimension pressure 1 ~ 10min, after steam explosion, temperature of charge is room temperature.
Further, the b step enzymolysis that described gutta-percha is separated is specially: add distilled water according to the ratio of solid-liquid ratio 1:10 ~ 1:40, with vinegar acid for adjusting pH to 4.8 ~ 5.2, then the prozyme of 30 ~ 100IU/g is added, under 48 ~ 52 DEG C of conditions, after combinative enzyme hydrolysis 36 ~ 72h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 100bar ~ 800bar, obtains the thick glue of the bark of eucommia.
Further, in the b step that described gutta-percha is separated, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g.
Further, the step c extraction purification that described gutta-percha is separated is specially: according to ratio and the sherwood oil mixing of solid-liquid ratio 1:5 ~ 1:20, under 80 ~ 85 DEG C of conditions, 2 ~ 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.
Further, a step extraction that described eucommia ulmoides seed oil is separated is specially: after seed of bark of eucommia drying and crushing to 10 ~ 20 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 45 ~ 55 DEG C in temperature, pressure is 1.2 ~ 2.0Mpa, CO
2flow velocity is: under the condition of 0.10 ~ 0.15L/min, extracts 2 ~ 5 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 48 ~ 60 DEG C for being separated by seed of bark of eucommia plant milk extract with pressure 2.0Mpa ~ 3.0Mpa, and CO
2gas enters extraction kettle after compression and recycles.
Further, the b step that described eucommia ulmoides seed oil is separated is filtered and is specially: the extract obtained by extraction and isolation in eucommia ulmoides seed oil separating step a, utilize volume membrane concentration, volume film is 300D by molecular weight, top hole pressure 0.2 ~ 0.3Mpa, makes moisture lower than 10%, and the method removal of impurities that recycling periosteum filters is filtered, wherein periosteum molecular weight cut-off 20000 ~ 30000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
Further, after the residue drying process that the b step that described eucommia ulmoides seed oil is separated obtains, use as the raw material preparing biological organic fertilizer.
Beneficial effect of the present invention:
1, the present invention utilizes Eucommia for raw material, extracts gutta-percha and eucommia ulmoides seed oil, and introduce membrane technique and carry out separation circuit, can improve the quality of products and yield, filtering and impurity removing is abundant, and required time is short, and extraction and isolation temperature is low.
2, 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.
3, the present invention utilizes steam explosion extraction and isolation gutta-percha, excessively need not pulverize Eucommia shell, the extraction and isolation time is short, effectively prevent because fermentation time is long, and cause part gutta-percha oxidized due to lengthy fermentation, 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.
4, a kind of steam explosion Eucommia of the present invention shell extraction and isolation gutta-percha, recycling supercritical CO
2extract eucommia ulmoides seed oil, extract the seed of bark of eucommia dregs of fat as the raw material of biological organic fertilizer, effectively realize the comprehensive development and utilization of bark of eucommia biomass resource, reduce the cost in gutta-percha performance history, expanded the approach of bark of eucommia higher value application.
5, main products Eucommia of the present invention oil alpha-linolenic acid, linoleic acid content are higher, and be a kind of nutritious functional health edible oil, safety non-toxic, is applicable to the industries such as food, medicine and healthcare products.
Accompanying drawing illustrates:
Fig. 1 is the schema of the method for extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia of the present invention.
Embodiment:
Below in conjunction with specific embodiment, technical scheme of the present invention is elaborated.
Embodiment 1
(1) pre-treatment: by Eucommia, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator; Plant benevolence and carry out suitable mechanical disintegration, be placed in dry shady and cool place, in order to extraction and isolation eucommia key fruit seed oil.
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: the kind shell that step (1) obtains is placed in the water of 30 DEG C and soaks 1h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 0.5MPa, temperature when controlling the steam explosion of steam blasting device is 180 DEG C, dimension pressure 1min, after steam explosion, temperature of charge is room temperature;
B, enzymolysis: the filter residue in step a adds distilled water according to the ratio of solid-liquid ratio 1:10, with vinegar acid for adjusting pH to 4.8, then add the prozyme of 30IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g, under 48 DEG C of conditions, after combinative enzyme hydrolysis 72h, utilize high-pressure cleaning device to rinse lignin residue, hydraulic pressure 100bar, obtains the thick glue of the bark of eucommia.
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, according to ratio and the sherwood oil 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;
B, eucommia ulmoides seed oil are separated
A, extraction: after seed of bark of eucommia drying and crushing to 10 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 45 DEG C in temperature, pressure is 1.2Mpa, CO
2flow velocity is: under the condition of 0.10L/min, extracts 5 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 48 DEG C for being separated by seed of bark of eucommia plant milk extract with pressure 2.0Mpa, and CO
2gas enters extraction kettle after compression and recycles;
B, the extract that extraction and isolation in step a is obtained, utilize concentrated volume film, volume film is 300D by molecular weight, top hole pressure 0.2Mpa, makes moisture lower than 10%, and the method removal of impurities that recycling periosteum filters is filtered, wherein periosteum molecular weight cut-off 20000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
C, post-processing stages: after the residue drying process in step b, use as the raw material preparing biological organic fertilizer.
Embodiment 2
(1) pre-treatment: by Eucommia, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator; Plant benevolence and carry out suitable mechanical disintegration, be placed in dry shady and cool place, in order to extraction and isolation eucommia key fruit seed oil.
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: the kind shell that step (1) obtains is placed in the water of 28 DEG C and soaks 4h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 0.8MPa, temperature when controlling the steam explosion of steam blasting device is 170 DEG C, dimension pressure 3min, after steam explosion, temperature of charge is room temperature;
B, enzymolysis: the filter residue in step a adds distilled water according to the ratio of solid-liquid ratio 1:25, with vinegar acid for adjusting pH to 4.9, then add the prozyme of 40IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g, under 49 DEG C of conditions, after combinative enzyme hydrolysis 60h, utilize high-pressure cleaning device to rinse lignin residue, hydraulic pressure 200bar, obtains the thick glue of the bark of eucommia.
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, according to ratio and the sherwood oil mixing of solid-liquid ratio 1:10, under 81 DEG C of conditions, 3h is extracted in condensation, heat filtering removes impurity, by liquid at-15 DEG C of refrigeration 2h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying;
B, eucommia ulmoides seed oil are separated
A, extraction: after seed of bark of eucommia drying and crushing to 12 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 47 DEG C in temperature, pressure is 1.4Mpa, CO
2flow velocity is: under the condition of 0.11L/min, extracts 2.5 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 50 C for being separated by seed of bark of eucommia plant milk extract with pressure 2.2Mpa, and CO
2gas enters extraction kettle after compression and recycles;
B, the extract that extraction and isolation in step a is obtained, utilize volume membrane concentration, volume film is 300D by molecular weight, top hole pressure 0.25Mpa, make moisture lower than 10%, the method removal of impurities that recycling periosteum filters is filtered, and wherein periosteum molecular weight cut-off 25000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
C, post-processing stages: after the residue drying process in step b, use as the raw material preparing biological organic fertilizer.
Embodiment 3
(1) pre-treatment: by Eucommia, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator; Plant benevolence and carry out suitable mechanical disintegration, be placed in dry shady and cool place, in order to extraction and isolation eucommia key fruit seed oil.
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: the kind shell that step (1) obtains is placed in the water of 25 DEG C and soaks 6h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 0.9MPa, temperature when controlling the steam explosion of steam blasting device is 150 DEG C, dimension pressure 5min, after steam explosion, temperature of charge is room temperature;
B, enzymolysis: the filter residue in step a adds distilled water according to the ratio of solid-liquid ratio 1:30, with vinegar acid for adjusting pH to 5.0, then add the prozyme of 55IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g, under 50 DEG C of conditions, after combinative enzyme hydrolysis 48h, utilize high-pressure cleaning device to rinse lignin residue, hydraulic pressure 400bar, obtains the thick glue of the bark of eucommia.
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, according to ratio and the sherwood oil mixing of solid-liquid ratio 1:15, under 82 DEG C of conditions, 2.5h is extracted in condensation, heat filtering removes impurity, by liquid at-17 DEG C of refrigeration 2h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying;
B, eucommia ulmoides seed oil are separated
A, extraction: after seed of bark of eucommia drying and crushing to 14 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 49 DEG C in temperature, pressure is 1.5Mpa, CO
2flow velocity is: under the condition of 0.13L/min, extracts 3.5 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 52 DEG C for being separated by seed of bark of eucommia plant milk extract with pressure 2.5Mpa, and CO
2gas enters extraction kettle after compression and recycles;
B, the extract obtained by extraction and isolation in step a, utilize volume membrane concentration, and volume film is 300D by molecular weight, top hole pressure 0.3Mpa, makes moisture lower than 10%, and the method removal of impurities that recycling periosteum filters is filtered, wherein periosteum molecular weight cut-off 30000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
C, post-processing stages: after the residue drying process in step b, use as the raw material preparing biological organic fertilizer.
Embodiment 4
(1) pre-treatment: by Eucommia, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator; Plant benevolence and carry out suitable mechanical disintegration, be placed in dry shady and cool place, in order to extraction and isolation eucommia key fruit seed oil.
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: the kind shell that step (1) obtains is placed in the water of 23 and soaks 8h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 1.1MPa, temperature when controlling the steam explosion of steam blasting device is 170 DEG C, dimension pressure 6min, after steam explosion, temperature of charge is room temperature;
B, enzymolysis: the filter residue in step a adds distilled water according to the ratio of solid-liquid ratio 1:30, with vinegar acid for adjusting pH to 5.0, then add the prozyme of 70IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g, under 51 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.
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, according to ratio and the sherwood oil mixing of solid-liquid ratio 1:20, under 83 DEG C of conditions, 2h is extracted in condensation, heat filtering removes impurity, by liquid at-12 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;
B, eucommia ulmoides seed oil are separated
A, extraction: after seed of bark of eucommia drying and crushing to 16 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 50 DEG C in temperature, pressure is 1.6Mpa, CO
2flow velocity is: under the condition of 0.13L/min, extracts 2.5 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 54 DEG C for being separated by seed of bark of eucommia plant milk extract with pressure 2.8Mpa, and CO
2gas enters extraction kettle after compression and recycles;
B, the extract obtained by extraction and isolation in step a, utilize volume membrane concentration, and volume film is 300D by molecular weight, top hole pressure 0.2Mpa, makes moisture lower than 10%, and the method removal of impurities that recycling periosteum filters is filtered, wherein periosteum molecular weight cut-off 25000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
C, post-processing stages: after the residue drying process in step b, use as the raw material preparing biological organic fertilizer.
Embodiment 5
(1) pre-treatment: by Eucommia, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator; Plant benevolence and carry out suitable mechanical disintegration, be placed in dry shady and cool place, in order to extraction and isolation eucommia key fruit seed oil.
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: the kind shell that step (1) obtains is placed in the water of 25 DEG C and soaks 10h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 1.3MPa, temperature when controlling the steam explosion of steam blasting device is 145 DEG C, dimension pressure 8min, after steam explosion, temperature of charge is room temperature;
B, enzymolysis: the filter residue in step a adds distilled water according to the ratio of solid-liquid ratio 1:35, with vinegar acid for adjusting pH to 5.1, then add the prozyme of 90IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g, under 51 DEG C of conditions, after combinative enzyme hydrolysis 60h, utilize high-pressure cleaning device to rinse lignin residue, hydraulic pressure 600bar, obtains the thick glue of the bark of eucommia.
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, according to ratio and the sherwood oil mixing of solid-liquid ratio 1:17, under 84 DEG C of conditions, 2h is extracted in condensation, heat filtering removes impurity, by liquid at-18 DEG C of refrigeration 3h, after gutta-percha is separated out, reclaim sherwood oil, namely obtain bark of eucommia essence glue through vacuum-drying;
B, eucommia ulmoides seed oil are separated
A, extraction: after seed of bark of eucommia drying and crushing to 20 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 53 DEG C in temperature, pressure is 1.8Mpa, CO
2flow velocity is: under the condition of 0.14L/min, extracts 4 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 58 DEG C for being separated by seed of bark of eucommia plant milk extract with pressure 2.8Mpa, and CO
2gas enters extraction kettle after compression and recycles;
B, the extract that extraction and isolation in step a is obtained, utilize volume membrane concentration, volume film is 300D by molecular weight, top hole pressure 0.25Mpa, make moisture lower than 10%, the method removal of impurities that recycling periosteum filters is filtered, and wherein periosteum molecular weight cut-off 25000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
C, post-processing stages: after the residue drying process in step b, use as the raw material preparing biological organic fertilizer.
Embodiment 6
(1) pre-treatment: by Eucommia, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator; Plant benevolence and carry out suitable mechanical disintegration, be placed in dry shady and cool place, in order to extraction and isolation eucommia key fruit seed oil.
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: the kind shell that step (1) obtains is placed in the water of 30 DEG C and soaks 12h, 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 140 DEG C, dimension pressure 10min, after steam explosion, temperature of charge is room temperature;
B, enzymolysis: the filter residue in step a adds distilled water according to the ratio of solid-liquid ratio 1:40, with vinegar acid for adjusting pH to 5.2, then add the prozyme of 100IU/g, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g, under 52 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.
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, according to ratio and the sherwood oil mixing of solid-liquid ratio 1:20, under 85 DEG C of conditions, 2h 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;
B, eucommia ulmoides seed oil are separated
A, extraction: after seed of bark of eucommia drying and crushing to 20 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 55 DEG C in temperature, pressure is 2.0Mpa, CO
2flow velocity is: under the condition of 0.15L/min, extracts 2 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 60 C for being separated by seed of bark of eucommia plant milk extract with pressure 3.0Mpa, and CO
2gas enters extraction kettle after compression and recycles;
B, the extract obtained by extraction and isolation in step a, utilize volume membrane concentration, and volume film is 300D by molecular weight, top hole pressure 0.3Mpa, makes moisture lower than 10%, and the method removal of impurities that recycling periosteum filters is filtered, wherein periosteum molecular weight cut-off 20000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
C, post-processing stages: after the residue drying process in step b, use as the raw material preparing biological organic fertilizer.
It should be noted that, above in each embodiment, the method of a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia of the present invention is not limited in this, other Conventional procedures that some steps or working method can be learnt by those skilled in the art or method are replaced to realize the present invention, the number of times such as carrying out supercritical extraction eucommia ulmoides seed oil is not limited to once, also can be one or many.
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 (9)
1. the method for extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia, is characterized in that: processed by Eucommia, is separated kind of shell and plants benevolence; Plant shell and obtain gutta-percha through steam explosion, enzymolysis and extraction purification step; Plant benevolence and obtain eucommia ulmoides seed oil through pulverizing, extraction, separating step.
2. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 1, is characterized in that: described method specifically comprises the following steps:
(1) pre-treatment: take Eucommia as raw material, after impurity elimination process, removes kind of a shell by the Eucommia of drying decorticator, is separated kind of shell and plants benevolence;
(2) being separated of eucommia ulmoides seed oil and gutta-percha:
A, gutta-percha are separated
A, kind shell Steam explosion treatment: kind shell step (1) obtained carries out Steam explosion treatment after soaking;
B, enzymolysis: after the filter residue in step a adds prozyme, carry out enzymic hydrolysis, rinses, obtain the thick glue of the bark of eucommia;
C, extraction purification: after thick for the bark of eucommia in step c glue is carried out drying treatment, mix with sherwood oil, then condensation is extracted, and filters, and separates out gutta-percha, dry bark of eucommia essence glue;
B, eucommia ulmoides seed oil are separated
A, extraction: seed of bark of eucommia utilizes the CO of supercritical state after pulverizing
2extraction, is separated seed of bark of eucommia plant milk extract;
B, filtration: the extract obtained by extraction and isolation in step a, after concentrate drying, makes moisture lower than 10%, more namely removal of impurities filtration obtains eucommia ulmoides seed oil.
3. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 2, it is characterized in that: described gutta-percha is separated a step kind shell Steam explosion treatment and is specially: be placed on by the kind shell that step (1) obtains in the water of 20 ~ 30 DEG C and soak 0 ~ 12h, then the material after immersion is put into steam blasting device and carry out steam explosion, the pressure of steam explosion is 0.5 ~ 1.5MPa, temperature when controlling the steam explosion of steam blasting device is 140 ~ 180 DEG C, dimension pressure 1 ~ 10min, after steam explosion, temperature of charge is room temperature.
4. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 2, it is characterized in that: the b step enzymolysis that described gutta-percha is separated is specially: add distilled water according to the ratio of solid-liquid ratio 1:10 ~ 1:40, with vinegar acid for adjusting pH to 4.8 ~ 5.2, then the prozyme of 30 ~ 100IU/g is added, under 48 ~ 52 DEG C of conditions, after combinative enzyme hydrolysis 36 ~ 72h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 100bar ~ 800bar, obtains the thick glue of the bark of eucommia.
5. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 2 or 4, it is characterized in that: in the b step that described gutta-percha is separated, prozyme mainly comprises polygalacturonase 18000IU/g, zytase 3500IU/g, cellulase 5500IU/g, beta-glucanase >=11000IU/g.
6. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 2, it is characterized in that: the step c extraction purification that described gutta-percha is separated is specially: according to ratio and the sherwood oil mixing of solid-liquid ratio 1:5 ~ 1:20, under 80 ~ 85 DEG C of conditions, 2 ~ 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.
7. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 2, it is characterized in that: a step extraction that described eucommia ulmoides seed oil is separated is specially: after seed of bark of eucommia drying and crushing to 10 ~ 20 orders, put into extraction kettle, by the CO of supercritical state
2inject extraction kettle, be 45 ~ 55 DEG C in temperature, pressure is 1.2 ~ 2.0Mpa, CO
2flow velocity is: under the condition of 0.10 ~ 0.15L/min, extracts 2 ~ 5 hours, is dissolved with the CO of seed of bark of eucommia extract
2fluid enters separating still, by regulating temperature 48 ~ 60 DEG C for being separated by seed of bark of eucommia plant milk extract with pressure 2.0Mpa ~ 3.0Mpa, and CO
2gas enters extraction kettle after compression and recycles.
8. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 2, it is characterized in that: the b step that described eucommia ulmoides seed oil is separated is filtered and is specially: the extract obtained by extraction and isolation in eucommia ulmoides seed oil separating step a, utilize volume membrane concentration, volume film is 300D by molecular weight, top hole pressure 0.2 ~ 0.3Mpa, make moisture lower than 10%, the method removal of impurities that recycling periosteum filters is filtered, wherein periosteum molecular weight cut-off 20000 ~ 30000D, namely obtains eucommia ulmoides seed oil by after contaminant filter.
9. the method for a kind of extraction and isolation eucommia ulmoides seed oil and gutta-percha from Eucommia according to claim 1, is characterized in that: after the residue drying process that the b step that described eucommia ulmoides seed oil is separated obtains, and uses as the raw material preparing biological organic fertilizer.
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| CN105950287A (en) * | 2016-07-01 | 2016-09-21 | 国家林业局泡桐研究开发中心 | Extracting and refining technology of eucommia seed oil |
| CN106118855A (en) * | 2016-06-27 | 2016-11-16 | 郭迎庆 | A kind of method utilizing flaxseed to prepare edible oil |
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| CN106118855A (en) * | 2016-06-27 | 2016-11-16 | 郭迎庆 | A kind of method utilizing flaxseed to prepare edible oil |
| CN105950287A (en) * | 2016-07-01 | 2016-09-21 | 国家林业局泡桐研究开发中心 | Extracting and refining technology of eucommia seed oil |
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