CN105400596A - Method for extracting green prickleyash oleoresin through subcritical dimethyl ether fluid - Google Patents
Method for extracting green prickleyash oleoresin through subcritical dimethyl ether fluid Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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Abstract
The invention discloses a method for extracting green prickleyash oleoresin through subcritical dimethyl ether fluid. The method comprises the four steps of raw material pretreatment, extraction, exsolution separation and residue recovery. The green prickleyash oleoresin is extracted by adopting the subcritical dimethyl ether fluid, the equipment manufacture cost is low, the equipment input is less, the energy consumption is less, the whole production process is in the low-pressure vacuum closed environment, and the production safety is high; the extraction process is environment-friendly and pollution-free; the extraction temperature is relatively low and low temperature smashing is adopted, so that the character flavor substances and spicy element components of green prickleyash are relatively completely reserved, the net extraction rate of the green prickleyash oleoresin reaches 20-23%, the prickleyash spicy element content in the green prickleyash oleoresin is 120-130 mg/g, and the volatile oil content is 55-60 mL/100g.
Description
Technical field
The invention belongs to green zanthoxylum oil resin field of deep, especially relate to the method for a kind of subcritical dimethyl ether fluid extraction green zanthoxylum oil resin.
Background technology
Pericarpium zanthoxyli schinifolii can be used as food flavouring, has Titian, effect except raw meat, also have warming middle-JIAO to relieve pain in addition, the function of killing parasites to relieve itching during culinary art, can be used for wrist abdomen crymodynia, the treatment of the symptom such as vomiting is had loose bowels, abdominal pain due to worm stagnation.Extract green zanthoxylum oil resin to refer to and adopt suitable fluid or solvent its fragrance and spicy component to be extracted as far as possible from pericarpium zanthoxyli schinifolii raw material, then fluid or separated from solvent are reclaimed and obtained thick shape, resinousness product containing essential oil; The main component of green zanthoxylum oil resin has essential oil, pigment, resin some nonvolatile grease, amides and polysaccharide compounds.Green zanthoxylum oil resin not only mouthfeel is full, and has the functions such as antibacterial, anti-oxidant, therefore plays an increasingly important role in the fields such as food, medicine, chemical industry.
Current extraction green zanthoxylum oil resin mainly adopts organic solvent extractionprocess, supercritical CO
2flow process and subcritical fluids method.Organic solvent method mainly adopts ether, methyl alcohol, ethanol equal solvent under certain extraction conditions, extracts the oleo-resinous in pericarpium zanthoxyli schinifolii in specific extractor, then obtains the thick product of green zanthoxylum oil resin through process procedures such as concentrated, precipitations.The defect of organic solvent method is that extraction time is long, oil yield is low, and often containing a large amount of dissolvent residual in product, affects the overall local flavor of product.Supercritical CO
2the green zanthoxylum oil resin of flow process extraction obtains the accreditation in market, and the Product Status that the method obtains is homogeneous, no solvent residue, effect are better; But supercritical CO
2the defect of flow process is apparatus expensive, and one-time investment is large, and extracting pressure is high, has potential safety hazard, and production cost is higher, is unfavorable for industrialization scale operation.Subcritical fluid extraction technology take subcritical fluids as solvent, extracting, evaporating the processes such as precipitation, compression condensation, recovery circulation, extracting the new technology of target components from natural product by succession passing through in system with solute material.The method is used widely at numerous areas at present, such as Chinese patent CN102850350A discloses a kind of method utilizing subcritical fluid extraction evodiamine, method steps is as follows: get Medcinal Evodia Fruit pulverizing medicinal materials, add subcritical abstraction still, pass into nonpolar organic reagent, temperature 30 ~ 80 DEG C, under the state of pressure 1 ~ 10MPa, dynamic extraction 30 ~ 60min, polarity organic reagent is passed into again to extractor, temperature 80 ~ 120 DEG C, under the state of pressure 0.3 ~ 3MPa, dynamic extraction 30 ~ 80min, extraction liquid is lowered the temperature, cross gac and diatomite resin column, cross the crystallization of post liquid concentrating under reduced pressure, crystallisate uses acetone soln recrystallization again, obtain evodiamine, in extraction process of the present invention extract and extraction liquid segregation ratio more difficult, final percentage extraction can be affected.Chinese patent CN102876456A discloses one and utilizes subcritical fluids from Chinese prickly ash, extract volatile oil and alkaloidal method, method steps is as follows: get Chinese prickly ash raw material pulverizing, add in subcritical abstraction still, pass into nonpolar organic reagent, under temperature 30 ~ 80 DEG C, pressure 1 ~ 10MPa state, dynamic extraction 30 ~ 60min, extraction liquid reclaim under reduced pressure reagent, add activated decoloration again, filter and obtain volatile oil; In material slag after above-mentioned extraction, pass into polarity organic reagent, under temperature 100 ~ 120 DEG C, pressure 0.2 ~ 5MPa state, dynamic extraction 30 ~ 60min, extraction liquid reclaim under reduced pressure reagent, concentrated solution regulates pH8 ~ 10, then extracts 2 ~ 3 times with chloroformic solution, collect chloroform layer condensing crystal, crystallisate is dry obtains alkaloid; This invention adopts nonpolar organic reagent and polarity organic reagent to extract volatile oil and alkaloid respectively, considerably increases extraction cost and extraction time, and then adds extraction cost.
Summary of the invention
In view of this, the object of the invention is for the deficiencies in the prior art, provide a kind of subcritical dimethyl ether fluid to extract the method for green zanthoxylum oil resin, technique is simple, and percentage extraction is high.
For achieving the above object, the present invention by the following technical solutions:
A method for subcritical dimethyl ether fluid extraction green zanthoxylum oil resin, comprises the following steps:
(1) raw materials pretreatment: pericarpium zanthoxyli schinifolii is crushed to 20 ~ 30 orders at 20 ~ 30 DEG C, obtains pericarpium zanthoxyli schinifolii powder, then loads in pocket by pericarpium zanthoxyli schinifolii powder;
(2) extract: the pocket that pericarpium zanthoxyli schinifolii powder is housed in step (1) is put into extractor, the pressure controlling extractor is-0.08MPa ~-0.1MPa, utilize pressure difference that the dme in solvent tank is injected extractor, temperature be 50 ~ 55 DEG C, under extracting pressure is the condition of 0.8MPa ~ 1.0MPa, after extraction 50 ~ 60min, extraction liquid enters separating tank from extractor;
(3) precipitation is separated: controlling temperature in separating tank is 55 ~ 60 DEG C, start compressor, after pressure tank to be separated is down to 0.1MPa ~ 0.2MPa, start vacuum pump, when Pressure Drop is to-0.08MPa ~-0.1MPa, after precipitation is separated 2 ~ 5min, obtain gaseous dimethyl and green zanthoxylum oil resin, gaseous dimethyl becomes liquid by compressor, condenser condenses, and enter solvent tank through purification, green zanthoxylum oil resin takes out from separating tank;
(4) reclaim defective material: by the pericarpium zanthoxyli schinifolii defective material in extractor temperature be 40 ~ 50 DEG C, under pressure is the condition of-0.08MPa ~-0.1MPa, decompression precipitation 2 ~ 5min, obtains pericarpium zanthoxyli schinifolii defective material.
Preferably, moisture content≤13% of pericarpium zanthoxyli schinifolii in described step (1), intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g.
Preferably, the pocket in described step (1) is 250 ~ 350 object mesh bag.
Preferably, in described step (2), the solid-liquid ratio of pericarpium zanthoxyli schinifolii and dme is 1kg:3L ~ 4L, and the amount of dme exceeds 5 ~ 10cm place above submergence pocket wherein.
Preferably, repeating step (2) extraction 1 ~ 3 time.
The invention has the beneficial effects as follows:
(1) in raw materials pretreatment process, the method of pulverize at low temperature is adopted to carry out pulverization process to pericarpium zanthoxyli schinifolii, the temperature of pulverize at low temperature is 20 ~ 30 DEG C, the flavour ingredient mainly volatile oil of Chinese prickly ash, spicy component is amide substance mainly, pulverize at low temperature can not be destroyed by the activeconstituents retained better to greatest extent in pericarpium zanthoxyli schinifolii preprocessing process in green zanthoxylum oil resin, increases the percentage extraction of green zanthoxylum oil resin.
(2) the present invention is when extracting green zanthoxylum oil resin, load after pericarpium zanthoxyli schinifolii is pulverized in pocket, then pocket is put into extractor to extract, the pericarpium zanthoxyli schinifolii defective material after extraction can be made better to be separated with extraction liquid, and easy cleaning pericarpium zanthoxyli schinifolii defective material, reduce the loss amount of green zanthoxylum oil resin in extraction process.
(3) extraction agent used in the present invention is dme, to compare other organic solvents, stable chemical nature, the low toxicity of dme, all there is comparatively high resolution to polarity and apolar substance, when dme exists with subcritical state, molecule diffusion and mass transfer velocity can be further strengthened, to green zanthoxylum oil resin, there is very strong solvability, the percentage extraction of green zanthoxylum oil resin can be improved, use the green zanthoxylum oil resin after subcritical dimethyl ether extraction not need through special processing, namely can be used as food flavouring and use.
(4) in the process of precipitation separation, first start compressor, after pressure tank to be separated is down to 0.1MPa ~ 0.2MPa, restart vacuum pump, when Pressure Drop is to-0.08MPa ~-0.1MPa, carry out decompression precipitation and be separated, employing vacuum pump and compressor link the mode reduced pressure, can precipitation velocity of separation be accelerated, make the more thorough of solvent and green zanthoxylum oil resin isolation.
(5) after having extracted, by the extraction in extractor the pericarpium zanthoxyli schinifolii defective material of green zanthoxylum oil resin to reduce pressure under certain temperature and pressure precipitation, dme remaining in pericarpium zanthoxyli schinifolii defective material is thoroughly separated totally, the residual quantity of the dme after testing in pericarpium zanthoxyli schinifolii defective material is less than 50ppm, can directly use as feed.
The present invention adopts subcritical dimethyl ether fluid to extract green zanthoxylum oil resin, and equipment making cost is low, and equipment investment is little, and consume energy little, production cost is only supercritical CO generally
2/ 4th of a flow process, production whole process is low-voltage vacuum closed environment, and production security is high; Extraction process is environment friendly and pollution-free, because the temperature of extraction is lower, and adopts pulverize at low temperature, more completely retains character flavor compound and the fiber crops element composition of pericarpium zanthoxyli schinifolii.Green zanthoxylum oil resin after extraction can directly apply to food service industry, and the pericarpium zanthoxyli schinifolii defective material after extraction is through carrying out precipitation treatment again, can directly use as feed.The present invention is through experiment repeatedly, determine the processing parameter of the best of subcritical dimethyl ether fluid extraction green zanthoxylum oil resin, and in order to improve percentage extraction further, prepare the highly purified green zanthoxylum oil resin of high-quality, the present invention carries out management and control to the raw material quality of pericarpium zanthoxyli schinifolii, wherein moisture content≤13% of pericarpium zanthoxyli schinifolii; Intrinsic contaminants content≤2.5%; Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content>=10.5mL/100g; The clean percentage extraction of the processing parameter extraction green zanthoxylum oil resin adopting the present invention to determine reaches 20% ~ 23%, and in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 120 ~ 130mg/g, and the content of volatile oil is 55 ~ 60mL/100g, and adopts supercritical CO in comparative example
2the clean percentage extraction of fluid extraction green zanthoxylum oil resin is 15% ~ 18%, in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 120 ~ 130mg/g, the content of volatile oil is 45 ~ 50mL/100g, therefore adopts preparation method of the present invention, and the percentage extraction of green zanthoxylum oil resin is than adopting supercritical CO
2the percentage extraction of fluid extraction improves 3 ~ 5 percentage points, and in green zanthoxylum oil resin, the content of volatile oil improves 5 ~ 10 percentage points.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
(1) raw materials pretreatment: select 20kg pericarpium zanthoxyli schinifolii, wherein moisture content≤10% of pericarpium zanthoxyli schinifolii, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, by pericarpium zanthoxyli schinifolii at 20 ~ 30 DEG C of flour to 20 orders, obtain pericarpium zanthoxyli schinifolii powder, pericarpium zanthoxyli schinifolii powder being distributed into 8 250 object total volumies is in the netted pocket of 3L, unsuitable overfill during packing pericarpium zanthoxyli schinifolii powder, be filled to 2/3rds places of pocket, fasten with white Nylon cord tying;
(2) extract: pocket is put into extractor from bottom to top, utilize vacuum pump that extractor internal pressure is evacuated to-0.08MPa, slowly open solvent tank liquid-outlet valve and extractor liquid feed valve, utilize pressure difference that 60L extraction agent dme is injected extractor, the amount of dme exceeds 5cm place above submergence pocket wherein; Open hot water circulating pump, extractor hot water circulation valve, and to control temperature in extractor be 55 DEG C, extracting pressure is 1.0MPa, after extraction 50min, opens extractor bleeder valve, separating tank feed valve, makes extraction liquid inject separating tank completely; And then re-extract 2 times;
(3) precipitation is separated: open separating tank hot water circulation valve, controlling temperature in separating tank is 55 DEG C, start compressor, carry out intensification decompression precipitation to extraction mixed solution to be separated, after pressure tank to be separated is down to 0.1MPa, start vacuum pump, link with compressor and accelerate precipitation and be separated, when Pressure Drop is to-0.08MPa, after precipitation is separated 5min, in separating tank, liquid state stable homogeneous is without obvious bubble, obtains gaseous dimethyl and green zanthoxylum oil resin, gaseous dimethyl becomes liquid by compressor, condenser condenses, enters solvent tank through purification; Slowly open separating tank vacuum valve, after tensimeter index return normal pressure, open separating tank bleeder valve, xanthoxylum oleoresin is taken out from separating tank by green grass or young crops;
(4) defective material is reclaimed: by vacuum pump, decompression carrying out precipitation treatment is carried out to pericarpium zanthoxyli schinifolii defective material stripped in extractor, the temperature controlled in extractor is 40 DEG C, pressure is-0.08MPa, decompression precipitation 5min, obtain pericarpium zanthoxyli schinifolii defective material, then vacuum pump is closed, open extractor vacuum valve, take out pericarpium zanthoxyli schinifolii defective material gross weight 15.2kg, can recycle as feed weighting material.
Collect green zanthoxylum oil rosin products crude oil 4.46kg altogether, hair percentage extraction is 22.3%, and the green zanthoxylum oil resin after molecular distillation is refined is 4.11kg, and clean percentage extraction is 20.5%, in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 122.1mg/g after testing, and the content of volatile oil is 56.2mL/100g.
Embodiment 2
(1) raw materials pretreatment: select 30kg pericarpium zanthoxyli schinifolii, wherein moisture content≤10% of pericarpium zanthoxyli schinifolii, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, by pericarpium zanthoxyli schinifolii at 20 ~ 30 DEG C of flour to 25 orders, obtain pericarpium zanthoxyli schinifolii powder, pericarpium zanthoxyli schinifolii powder being distributed into 12 300 object total volumies is in the netted pocket of 3L, unsuitable overfill during packing pericarpium zanthoxyli schinifolii powder, be filled to 2/3rds places of pocket, fasten with white Nylon cord tying;
(2) extract: pocket is put into extractor from bottom to top, utilize vacuum pump that extractor internal pressure is evacuated to-0.09MPa, slowly open solvent tank liquid-outlet valve and extractor liquid feed valve, utilize pressure difference that 105L extraction agent dme is injected extractor, the amount of dme exceeds 8cm place above submergence pocket wherein; Open hot water circulating pump, extractor hot water circulation valve, and to control temperature in extractor be 54 DEG C, extracting pressure is 0.9MPa, after extraction 55min, opens extractor bleeder valve, separating tank feed valve, makes extraction mixed solution inject separating tank completely; And then re-extract 1 time;
(3) precipitation is separated: open separating tank hot water circulation valve, controlling temperature in separating tank is 58 DEG C, start compressor, carry out intensification decompression precipitation to extraction mixed solution to be separated, after pressure tank to be separated is down to 0.15MPa, start vacuum pump, link with compressor and accelerate precipitation and be separated, when Pressure Drop is to-0.09MPa, after precipitation is separated 4min, in separating tank, liquid state stable homogeneous is without obvious bubble, obtains gaseous dimethyl and green zanthoxylum oil resin, gaseous dimethyl becomes liquid by compressor, condenser condenses, enters solvent tank through purification; Slowly open separating tank vacuum valve, after tensimeter index return normal pressure, open separating tank bleeder valve, xanthoxylum oleoresin takes out from separating tank by green grass or young crops;
(4) defective material is reclaimed: by vacuum pump, decompression carrying out precipitation treatment is carried out to pericarpium zanthoxyli schinifolii defective material stripped in extractor, the temperature controlled in extractor is 45 DEG C, pressure is-0.09MPa, decompression precipitation 4min, obtain pericarpium zanthoxyli schinifolii defective material, then vacuum pump is closed, open extractor vacuum valve, take out pericarpium zanthoxyli schinifolii defective material gross weight 22.8kg, can recycle as feed weighting material.
Collect green zanthoxylum oil rosin products crude oil 6.9kg altogether, hair percentage extraction is 23.0%, and the green zanthoxylum oil resin after molecular distillation is refined is 6.66kg, and clean percentage extraction is 22.2%, in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 125.1mg/g after testing, and the content of volatile oil is 57.8mL/100g.
Embodiment 3
(1) raw materials pretreatment: select 35kg pericarpium zanthoxyli schinifolii, wherein moisture content≤10% of pericarpium zanthoxyli schinifolii, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, by pericarpium zanthoxyli schinifolii at 20 ~ 30 DEG C of flour to 30 orders, obtain pericarpium zanthoxyli schinifolii powder, pericarpium zanthoxyli schinifolii powder being distributed into 14 270 object total volumies is in the netted pocket of 3L, unsuitable overfill during packing pericarpium zanthoxyli schinifolii powder, be filled to 2/3rds places of pocket, fasten with white Nylon cord tying;
(2) extract: pocket is put into extractor from bottom to top, utilize vacuum pump that extractor internal pressure is evacuated to-0.1MPa, slowly open solvent tank liquid-outlet valve and extractor liquid feed valve, utilize pressure difference that 112L extraction agent dme is injected extractor, the amount of dme exceeds 6cm place above submergence pocket wherein; Open hot water circulating pump, extractor hot water circulation valve, and to control temperature in extractor be 55 DEG C, extracting pressure is 0.8MPa, after extraction 60min, opens extractor bleeder valve, separating tank feed valve, makes extraction mixed solution inject separating tank completely; And then re-extract 3 times;
(3) precipitation is separated: open separating tank hot water circulation valve, controlling temperature in separating tank is 60 DEG C, start compressor, carry out intensification decompression precipitation to extraction mixed solution to be separated, after pressure tank to be separated is down to 0.2MPa, start vacuum pump, link with compressor and accelerate precipitation and be separated, when Pressure Drop is to-0.1MPa, after precipitation is separated 2min, in separating tank, liquid state stable homogeneous is without obvious bubble, obtains gaseous dimethyl and green zanthoxylum oil resin, gaseous dimethyl becomes liquid by compressor, condenser condenses, enters solvent tank through purification; Slowly open separating tank vacuum valve, after tensimeter index return normal pressure, open separating tank bleeder valve, xanthoxylum oleoresin takes out from separating tank by green grass or young crops;
(4) defective material is reclaimed: by vacuum pump, decompression carrying out precipitation treatment is carried out to pericarpium zanthoxyli schinifolii defective material stripped in extractor, the temperature controlled in extractor is 50 DEG C, pressure is-0.1MPa, decompression precipitation 2min, obtain pericarpium zanthoxyli schinifolii defective material, then vacuum pump is closed, open extractor vacuum valve, take out pericarpium zanthoxyli schinifolii defective material gross weight 26.4kg, can recycle as feed weighting material.
Collect green zanthoxylum oil rosin products crude oil 8.26kg altogether, hair percentage extraction is 23.6%, and the green zanthoxylum oil resin after molecular distillation is refined is 8.05kg, and clean percentage extraction is 23%, in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 130mg/g after testing, and the content of volatile oil is 60mL/100g.
Embodiment 4
(1) raw materials pretreatment: select 40kg pericarpium zanthoxyli schinifolii, wherein moisture content≤10% of pericarpium zanthoxyli schinifolii, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, by pericarpium zanthoxyli schinifolii at 20 ~ 30 DEG C of flour to 25 orders, obtain pericarpium zanthoxyli schinifolii powder, pericarpium zanthoxyli schinifolii powder being distributed into 16 325 object total volumies is in the netted pocket of 3L, unsuitable overfill during packing pericarpium zanthoxyli schinifolii powder, be filled to 2/3rds places of pocket, fasten with white Nylon cord tying;
(2) extract: pocket is put into extractor from bottom to top, utilize vacuum pump that extractor internal pressure is evacuated to-0.08MPa, slowly open solvent tank liquid-outlet valve and extractor liquid feed valve, utilize pressure difference that 120L extraction agent dme is injected extractor, the amount of dme exceeds 5cm place above submergence pocket wherein; Open hot water circulating pump, extractor hot water circulation valve, and to control temperature in extractor be 52 DEG C, extracting pressure is 1.0MPa, after extraction 50min, opens extractor bleeder valve, separating tank feed valve, makes extraction mixed solution inject separating tank completely; And then re-extract 1 time;
(3) precipitation is separated: open separating tank hot water circulation valve, controlling temperature in separating tank is 55 DEG C, start compressor, carry out intensification decompression precipitation to extraction mixed solution to be separated, after pressure tank to be separated is down to 0.1MPa, start vacuum pump, link with compressor and accelerate precipitation and be separated, when Pressure Drop is to-0.08MPa, after precipitation is separated 3min, in separating tank, liquid state stable homogeneous is without obvious bubble, obtains gaseous dimethyl and green zanthoxylum oil resin, gaseous dimethyl becomes liquid by compressor, condenser condenses, enters solvent tank through purification; Slowly open separating tank vacuum valve, after tensimeter index return normal pressure, open separating tank bleeder valve, xanthoxylum oleoresin takes out from separating tank by green grass or young crops;
(4) defective material is reclaimed: by vacuum pump, decompression carrying out precipitation treatment is carried out to pericarpium zanthoxyli schinifolii defective material stripped in extractor, the temperature controlled in extractor is 48 DEG C, pressure is-0.08MPa, decompression precipitation 3min, obtain pericarpium zanthoxyli schinifolii defective material, then vacuum pump is closed, open extractor vacuum valve, take out pericarpium zanthoxyli schinifolii defective material gross weight 30.8kg, can recycle as feed weighting material.
Collect green zanthoxylum oil rosin products crude oil 8.76kg altogether, hair percentage extraction is 21.9%, and the green zanthoxylum oil resin after molecular distillation is refined is 8.0kg, and clean percentage extraction is 20%, in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 120.5mg/g after testing, and the content of volatile oil is 55mL/100g.
Embodiment 5
(1) raw materials pretreatment: select 50kg pericarpium zanthoxyli schinifolii, wherein moisture content≤10% of pericarpium zanthoxyli schinifolii, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, by pericarpium zanthoxyli schinifolii at 20 ~ 30 DEG C of flour to 20 orders, obtain pericarpium zanthoxyli schinifolii powder, pericarpium zanthoxyli schinifolii powder being distributed into 20 350 object total volumies is in the netted pocket of 3L, unsuitable overfill during packing pericarpium zanthoxyli schinifolii powder, be filled to 2/3rds places of pocket, fasten with white Nylon cord tying;
(2) extract: pocket is put into extractor from bottom to top, utilize vacuum pump that extractor internal pressure is evacuated to-0.1MPa, slowly open solvent tank liquid-outlet valve and extractor liquid feed valve, utilize pressure difference that 200L extraction agent dme is injected extractor, the amount of dme exceeds 10cm place above submergence pocket wherein; Open hot water circulating pump, extractor hot water circulation valve, and to control temperature in extractor be 50 DEG C, extracting pressure is 0.8MPa, after extraction 60min, opens extractor bleeder valve, separating tank feed valve, makes extraction mixed solution inject separating tank completely; And then re-extract 2 times;
(3) precipitation is separated: open separating tank hot water circulation valve, controlling temperature in separating tank is 55 DEG C, start compressor, carry out intensification decompression precipitation to extraction mixed solution to be separated, after pressure tank to be separated is down to 0.15MPa, start vacuum pump, link with compressor and accelerate precipitation and be separated, when Pressure Drop is to-0.1MPa, after precipitation is separated 3min, in separating tank, liquid state stable homogeneous is without obvious bubble, obtains gaseous dimethyl and green zanthoxylum oil resin, gaseous dimethyl becomes liquid by compressor, condenser condenses, enters solvent tank through purification; Slowly open separating tank vacuum valve, after tensimeter index return normal pressure, open separating tank bleeder valve, xanthoxylum oleoresin takes out from separating tank by green grass or young crops;
(4) defective material is reclaimed: by vacuum pump, decompression carrying out precipitation treatment is carried out to pericarpium zanthoxyli schinifolii defective material stripped in extractor, the temperature controlled in extractor is 50 DEG C, pressure is-0.1MPa, decompression precipitation 2min, obtain pericarpium zanthoxyli schinifolii defective material, then vacuum pump is closed, open extractor vacuum valve, take out pericarpium zanthoxyli schinifolii defective material gross weight 38.4kg, can recycle as feed weighting material.
Collect green zanthoxylum oil rosin products crude oil 11.2kg altogether, hair percentage extraction is 22.4%, and the green zanthoxylum oil resin after molecular distillation is refined is 10.8kg, and clean percentage extraction is 21.6%, in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 126.2mg/g after testing, and the content of volatile oil is 59.2mL/100g.
Comparative example 1
Adopt supercritical CO
2fluid extraction green zanthoxylum oil resin, comprises the following steps:
(1) raw materials pretreatment: take 50kg pericarpium zanthoxyli schinifolii, wherein pericarpium zanthoxyli schinifolii moisture content≤10%, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, at 20 ~ 30 DEG C of flour to 40 orders, obtain pericarpium zanthoxyli schinifolii powder;
(2) extract: loaded by pericarpium zanthoxyli schinifolii powder in supercritical extraction reactor, the temperature controlling extraction kettle is 45 DEG C, CO
2flow is 100L/h, and extracting pressure is 27.5MPa, after extraction 6h, prepares xanthoxylum oleoresin mixed solution;
(3) oily water separation: pour in water-and-oil separator by the green zanthoxylum oil resin mixture liquor of preparation in step (2), carry out oily water separation at 60 DEG C, after being discharged by moisture, obtains green zanthoxylum oil resin.
Xanthoxylum oleoresin after molecular distillation is refined for 8.0kg, clean percentage extraction is 16%, and in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 120.5mg/g after testing, and the content of volatile oil is 45.1mL/100g.
Comparative example 2
Adopt supercritical CO
2fluid extraction green zanthoxylum oil resin, comprises the following steps:
(1) raw materials pretreatment: take 50kg pericarpium zanthoxyli schinifolii, wherein pericarpium zanthoxyli schinifolii moisture content≤10%, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, at 20 ~ 30 DEG C of flour to 50 orders, obtain pericarpium zanthoxyli schinifolii powder;
(2) extract: loaded by pericarpium zanthoxyli schinifolii powder in supercritical extraction reactor, the temperature controlling extraction kettle is 40 DEG C, CO
2flow is 110L/h, and extracting pressure is 28MPa, after extraction 5h, prepares xanthoxylum oleoresin mixed solution;
(3) oily water separation: pour in water-and-oil separator by the green zanthoxylum oil resin mixture liquor of preparation in step (2), carry out oily water separation at 60 DEG C, after being discharged by moisture, obtains green zanthoxylum oil resin.
Xanthoxylum oleoresin after molecular distillation is refined for 9.0kg, clean percentage extraction is 18%, and in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 128.6mg/g after testing, and the content of volatile oil is 50mL/100g.
Comparative example 3
Adopt supercritical CO
2fluid extraction green zanthoxylum oil resin, comprises the following steps:
(1) raw materials pretreatment: take 50kg pericarpium zanthoxyli schinifolii, wherein pericarpium zanthoxyli schinifolii moisture content≤10%, intrinsic contaminants content≤2.5%, Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g, at 20 ~ 30 DEG C of flour to 60 orders, obtain pericarpium zanthoxyli schinifolii powder;
(2) extract: loaded by pericarpium zanthoxyli schinifolii powder in supercritical extraction reactor, the temperature controlling extraction kettle is 50 DEG C, CO
2flow is 120L/h, and extracting pressure is 27MPa, after extraction 4h, prepares xanthoxylum oleoresin mixed solution;
(3) oily water separation: pour in water-and-oil separator by the green zanthoxylum oil resin mixture liquor of preparation in step (2), carry out oily water separation at 60 DEG C, after being discharged by moisture, obtains green zanthoxylum oil resin.
Xanthoxylum oleoresin after molecular distillation is refined for 7.5kg, clean percentage extraction is 15%, and in green zanthoxylum oil resin, the content of numb-taste component of zanthoxylum is 121.5mg/g after testing, and the content of volatile oil is 46mL/100g.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, other amendments that those of ordinary skill in the art make technical scheme of the present invention or equivalently to replace, only otherwise depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of right of the present invention.
Claims (5)
1. a method for subcritical dimethyl ether fluid extraction green zanthoxylum oil resin, is characterized in that, comprise the following steps:
(1) raw materials pretreatment: pericarpium zanthoxyli schinifolii is crushed to 20 ~ 30 orders at 20 ~ 30 DEG C, obtains pericarpium zanthoxyli schinifolii powder, then loads in pocket by pericarpium zanthoxyli schinifolii powder;
(2) extract: the pocket that pericarpium zanthoxyli schinifolii powder is housed in step (1) is put into extractor, the pressure controlling extractor is-0.08MPa ~-0.1MPa, utilize pressure difference that the dme in solvent tank is injected extractor, temperature be 50 ~ 55 DEG C, under extracting pressure is the condition of 0.8MPa ~ 1.0MPa, after extraction 50 ~ 60min, extraction liquid enters separating tank from extractor;
(3) precipitation is separated: controlling temperature in separating tank is 55 ~ 60 DEG C, start compressor, after pressure tank to be separated is down to 0.1MPa ~ 0.2MPa, start vacuum pump, when Pressure Drop is to-0.08MPa ~-0.1MPa, after precipitation is separated 2 ~ 5min, obtain gaseous dimethyl and green zanthoxylum oil resin, gaseous dimethyl becomes liquid by compressor, condenser condenses, and enter solvent tank through purification, green zanthoxylum oil resin takes out from separating tank;
(4) reclaim defective material: by the pericarpium zanthoxyli schinifolii defective material in extractor temperature be 40 ~ 50 DEG C, under pressure is the condition of-0.08MPa ~-0.1MPa, decompression precipitation 2 ~ 5min, obtains pericarpium zanthoxyli schinifolii defective material.
2. subcritical dimethyl ether fluid extracts the method for green zanthoxylum oil resin according to claim 1, it is characterized in that, moisture content≤13% of pericarpium zanthoxyli schinifolii in described step (1); Intrinsic contaminants content≤2.5%; Semen Pericarpium Zanthoxyli content≤7%, eye closing green pepper content≤35%, tramp material content≤0.5%, volatile oil content >=10.5mL/100g.
3. subcritical dimethyl ether fluid extracts the method for green zanthoxylum oil resin according to claim 1, and it is characterized in that, the pocket in described step (1) is 250 ~ 350 object mesh bag.
4. subcritical dimethyl ether fluid extracts the method for green zanthoxylum oil resin according to claim 1, it is characterized in that, in described step (2), the solid-liquid ratio of pericarpium zanthoxyli schinifolii and dme is 1kg:3L ~ 4L.
5. subcritical dimethyl ether fluid extracts the method for green zanthoxylum oil resin according to claim 1, it is characterized in that, repeating step (2) extraction 1 ~ 3 time.
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