CN107805546A - A kind of method that polyphenol powde and essential oil are extracted in the wood from Chinese juniper - Google Patents

A kind of method that polyphenol powde and essential oil are extracted in the wood from Chinese juniper Download PDF

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Publication number
CN107805546A
CN107805546A CN201711110724.1A CN201711110724A CN107805546A CN 107805546 A CN107805546 A CN 107805546A CN 201711110724 A CN201711110724 A CN 201711110724A CN 107805546 A CN107805546 A CN 107805546A
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Prior art keywords
wood
chinese juniper
essential oil
oil
extracted
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CN201711110724.1A
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Chinese (zh)
Inventor
霍振中
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Nanning Keicheng Mdt Infotech Ltd
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Nanning Keicheng Mdt Infotech Ltd
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Priority to CN201711110724.1A priority Critical patent/CN107805546A/en
Publication of CN107805546A publication Critical patent/CN107805546A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining

Abstract

The invention discloses a kind of method that polyphenol powde and essential oil are extracted in wood from Chinese juniper, comprise the following steps that:1. select former material material process 2. drying process:1. described raw material are bakeed into water content the 3. pulverizing process below 10%:The particle powder between 10 to 30 mesh is become, loads alembic middle part 4. low-pressure steam process:75 85 DEG C of vapor is produced in vapor generator, after 30 to 50 seconds, starts oil pump and vacuumizes and produce 40 to 60kpa negative pressure 5. distillation process:Negative pressure is finally changed into normal ambient pressure 6. filter progress 7. decolouring decoking process 8. water-oil separating process.The present invention is the raising and improvement to traditional steam distillation and vacuum distillation method, is especially suitable for the extraction of essential oil that perennial Chinese juniper wood rhizome is raw material.Avoid still suffering from a large amount of pyrolysis, hydrolysis and the generation of coking phenomenon in production process.

Description

A kind of method that polyphenol powde and essential oil are extracted in the wood from Chinese juniper
Technical field
The present invention relates to polyphenol powde and extraction of essential oil field, the side of polyphenol powde and essential oil is extracted in specially a kind of wood from Chinese juniper Method.
Background technology
Polyphenol powde typically refers in higher plant contained pure natural defence organic principle, and it is mainly terpenes, people The sense of fragrant spiciness can be had by smelling.Polyphenol powde can drive away the micro- worm, bacterium and virus for injuring the own body of plant, promote plant damage Repair traumatic part position.Chinese juniper wood polyphenol powde typically refers in particular to the aqueous solution separated during Chinese juniper another name for oil is extracted, i.e. hydrosol.
Essential oil is in the flower from plant, leaf, stem, root or fruit, passes through steam distillation, extrusion, cold-maceration or molten Agent extraction method refines the volatile flavor of extraction.It is used for people after being extracted containing substantial amounts of essential oil and polyphenol powde in Chinese juniper wood Use, contribute to the health of people, while it is that we need to study that distillation extraction essential oil and polyphenol powde are carried out to Chinese juniper wood The problem of, the convenience of distillation is improved, the yield for increasing essential oil and polyphenol powde is all the problem of needing us to study, so as to improve The utilization rate of essential oil and polyphenol powde in Chinese juniper wood.
Traditionally, it is steam distillation to extract Chinese juniper another name for oil and the most frequently used method of Chinese juniper wood polyphenol powde.Small investment, equipment Simply, the characteristics of simple operation is this method.
But the Chinese juniper wood raw material of wooden structures is directly heated, easily causes the thermally sensitive composition in Chinese juniper another name for oil to divide rapidly Solution, causes very big loss and waste.Secondly, there is also many compositions susceptible to hydrolysis in Chinese juniper another name for oil, in continuous and hot water In hot steam's contact process, these compositions will also tend to largely hydrolyze, and cause much to expend.Meanwhile heat is too high to make Obtain Chinese juniper woody part and divide coking, the essential oil extracted, dissolve and be mixed with a large amount of coking materials, color and luster is partially black, leverages product Outward appearance and quality.
Although many people are improved, such as uninterrupted continuous still method, turbine type flash distillation method etc. are created, it is raw A large amount of pyrolysis, hydrolysis and the generation of coking phenomenon are still suffered from during production, fails to tackle the problem at its root.Then in this base On plinth, there is the producer to heating container closure and then vacuumize, a series of distillation under vacuum are developed, to some flowers class draft The extraction of essential oil of plant, positive effect, it can greatly suppress decomposition and coking.But this method is highly dense with timber tubers to Chinese juniper wood etc. It is wooden for raw material prepare essential oil when, yield is greatly lowered, and energy consumption significantly raises, and equipment investment is also increased significantly.
Patent document 1:
One kind extracts the transformation distillating method of water-soluble polyphenol powde (hydrosol) and essential oil from Chinese juniper wood(CN102925291A).
The shortcomings that this method, is:
In distillation processing, do not disclose negative pressure is how to gradually become normal ambient pressure, polyphenol powde and essential oil separate out with Pressure and temperature constantly change suffered by material is closely related,.
It is to refilter impurity after water-oil separating in whole method, can causes to extract the second-rate of polyphenol powde and essential oil.
Patent document 2:
The transformation distillating method of polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper(CN107216949A).
The shortcomings that this method, is:
In pulverizing process, the Chinese juniper wood raw material mesh number after crushing is too big, the quality of considerable influence Chinese juniper wood extraction polyphenol powde and essential oil And quantity.
There is no decolouring decoking process in whole method, can cause to extract the second-rate of polyphenol powde and essential oil.
The content of the invention
It is an object of the invention to provide a kind of method that polyphenol powde and essential oil are extracted in wood from Chinese juniper, comprise the following steps that:
1. select former material material process:Become a useful person Japan cypress and yellow Chinese juniper perennial wooden Chinese juniper wood rhizome material with giant washes clean, Remove the impurity such as epidermis sandy soil;
2. drying process:1. described raw material are bakeed to water content below 10%;
3. pulverizing process:Long 6-7 centimetres, wide 2-3 centimetres, dry wood of the thickness at 0.2-0.3 centimetres is cut into mechanical chopper again Piece, fine crushing Chinese juniper wood fuzz stick, the particle powder between 10 to 30 mesh is become, loaded in the middle part of alembic;
4. low-pressure steam process:75-85 DEG C of vapor is produced in vapor generator, is entered from the lower steam import of alembic Enter, with the Chinese juniper wood raw material that fills carry out it is of short duration contact, after 30 to 50 seconds, start oil pump and vacuumize generation 40 and arrive 60kpa Negative pressure;After stable gas pressure, cooling is sprayed by normal-temperature water at the top of alembic, decompression humidification, at reduced pressure conditions with Chinese juniper The wood materials such as the rhizome of wood are sufficiently contacted so that the volatile ingredient such as essential oil in raw tissue, in less pyrolysis and water In the case of solution, by steam extraction and mix;
5. distillation process:After spending 20 to 30 minutes, the pressure of adjustment, first 0.1MPa voltage stabilizings 3-5 minutes, then allow 0.1MPa to be depressured To 0.05MPa, voltage stabilizing 5-8 minutes, and 0.05MPa is boosted into 0.1MPa, voltage stabilizing 3-5 minutes, then allow 0.1MPa to be depressurized to 0.05MPa, voltage stabilizing 20-30 minutes;Oil pump is closed, negative pressure is finally changed into normal ambient pressure, after spending 20-30 minutes again, is beaten The steam pipework above alembic is opened, connects coil condenser;
6. filter progress:The oil mixing with water condensate liquid of acquisition is subjected to filtration treatment, filtration treatment is clear by the impurity in mixed liquor Remove;
7. decolouring decoking process:Activated carbon is added to be decolourized;
8. water-oil separating process:It will filter, the oil-water mixture progress water-oil separating after decolouring decoking processing, the sweet smell of acquisition is more Essence and essential oil carry out sealing storage, complete whole technical process.
Chinese juniper wood preferably originates in China western part Sichuan and Shanxi Dian Guideng provinces.
The Chinese juniper wood preferably age of tree is more than 50 years.
Drying temperature is controlled between 30-50 DEG C.
Drying process is dried by the way of air-heater auxiliary air-dries.
Activated carbon is 50-100 grams.
The beneficial effect of invention:
The Chinese juniper wood polyphenol powde and Chinese juniper wood method of extraction of essential oil of the present invention, is to traditional steam distillation and vacuum distillation method Raising and improvement, be especially suitable for perennial Chinese juniper wood rhizome be raw material extraction of essential oil.Avoid still suffering from production process greatly Calorimetric solution, hydrolysis and the generation of coking phenomenon, without adding any poisonous and harmful solvent in production, in the extraction process of transformation, Reduce the pyrolysis and hydrolysis of Chinese juniper wood fragrance component, and effectively inhibit coking, improve the quality of product, can greatly carry High economic benefit.
Using transformation, decompression mode, the polyphenol powde and essential oil contributed in Chinese juniper wood oozes out, using oozing under atmospheric pressure normality Go out, coordinate interval decompression processing, polyphenol powde and essential oil can be allowd preferably to ooze out, at the same distillation processing procedure it It is preceding to need to steam raw material progress low temperature so that saturated with water in raw material, more conducively polyphenol powde and essential oil are dissolved in water, together When the later stage distill and cause polyphenol powde and essential oil as vapor discharges, while Low Temperature Steam can be to the steady of polyphenol powde and essential oil It is qualitative to be protected, reduce the destruction to polyphenol powde and essential oil.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with specific embodiment, to this Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not For limiting the present invention.
Embodiment 1:
The method that polyphenol powde and essential oil are extracted in this wood from Chinese juniper, is comprised the following steps that:
1. select former material material process:Become a useful person Japan cypress and yellow Chinese juniper perennial wooden Chinese juniper wood rhizome material with giant washes clean, Remove the impurity such as epidermis sandy soil.
2. drying process:1. described raw material are bakeed to water content 8%.
3. pulverizing process:Long 6 centimetres, wide 2 centimetres, fuzz stick of the thickness at 0.2 centimetre, essence are cut into mechanical chopper again Finely divided Chinese juniper wood fuzz stick, the particle powder of 10 mesh is become, loaded in the middle part of alembic.
4. low-pressure steam process:75 DEG C of vapor is produced in vapor generator, from the lower steam import of alembic Into, with the Chinese juniper wood raw material that fills carry out it is of short duration contact, after the 30 seconds, start oil pump and vacuumize and produce the negative of 40 kpa Pressure.After stable gas pressure, cooling is sprayed by normal-temperature water at the top of alembic, decompression humidification, at reduced pressure conditions with Chinese juniper wood The wood materials such as rhizome are sufficiently contacted so that the volatile ingredient such as essential oil in raw tissue, it is less pyrolysis and hydrolysis In the case of, by steam extraction and mix.
5. distillation process:After spending 20 minutes, the pressure of adjustment, first 0.1MPa voltage stabilizings 3 minutes, then allow 0.1MPa to be depressurized to 0.05MPa, voltage stabilizing 5 minutes, and 0.05MPa is boosted into 0.1MPa, voltage stabilizing 3 minutes, then allow 0.1MPa to be depressurized to 0.05MPa, voltage stabilizing 20 minutes.Oil pump is closed, negative pressure is finally changed into normal ambient pressure, after spending 20 minutes again, opens distillation Steam pipework above tank, connect coil condenser.
6. filter progress:The oil mixing with water condensate liquid of acquisition is subjected to filtration treatment, filtration treatment will be miscellaneous in mixed liquor Matter is removed.
7. decolouring decoking process:Activated carbon is added to be decolourized.
8. water-oil separating process:It will filter, the oil-water mixture progress water-oil separating after decolouring decoking processing, by acquisition Polyphenol powde and essential oil carry out sealing storage, complete whole technical process.
Chinese juniper wood preferably originates in China western part Sichuan and Shanxi Dian Guideng provinces.
The Chinese juniper wood preferably age of tree is 50 years.
Drying temperature is controlled between 30 DEG C.
Drying process is dried by the way of air-heater auxiliary air-dries.
Activated carbon is 50 grams.
Embodiment 2:
The method that polyphenol powde and essential oil are extracted in this wood from Chinese juniper, is comprised the following steps that:
1. select former material material process:Become a useful person Japan cypress and yellow Chinese juniper perennial wooden Chinese juniper wood rhizome material with giant washes clean, Remove the impurity such as epidermis sandy soil.
2. drying process:1. described raw material are bakeed to water content 9%.
3. pulverizing process:Long 7 centimetres, wide 3 centimetres, fuzz stick of the thickness at 0.3 centimetre, essence are cut into mechanical chopper again Finely divided Chinese juniper wood fuzz stick, the particle powder of 30 mesh is become, loaded in the middle part of alembic.
4. low-pressure steam process:85 DEG C of vapor is produced in vapor generator, from the lower steam import of alembic Into, with the Chinese juniper wood raw material that fills carry out it is of short duration contact, after 50 seconds, start oil pump and vacuumize the negative pressure for producing 60kpa. After stable gas pressure, cooling is sprayed by the normal-temperature water at the top of alembic, decompression is humidified, at reduced pressure conditions the rhizome wooden with Chinese juniper Sufficiently contacted Deng wood material so that the volatile ingredient such as essential oil in raw tissue, in the situation of less pyrolysis and hydrolysis Under, by steam extraction and mix.
5. distillation process:After spending 30 minutes, the pressure of adjustment, first 0.1MPa voltage stabilizings 5 minutes, then allow 0.1MPa to be depressurized to 0.05MPa, voltage stabilizing 8 minutes, and 0.05MPa is boosted into 0.1MPa, voltage stabilizing 5 minutes, then allow 0.1MPa to be depressurized to 0.05MPa, voltage stabilizing 30 minutes.Oil pump is closed, negative pressure is finally changed into normal ambient pressure, after spending 30 minutes again, opens distillation Steam pipework above tank, connect coil condenser.
6. filter progress:The oil mixing with water condensate liquid of acquisition is subjected to filtration treatment, filtration treatment will be miscellaneous in mixed liquor Matter is removed.
7. decolouring decoking process:Activated carbon is added to be decolourized.
8. water-oil separating process:It will filter, the oil-water mixture progress water-oil separating after decolouring decoking processing, by acquisition Polyphenol powde and essential oil carry out sealing storage, complete whole technical process.
Chinese juniper wood preferably originates in China western part Sichuan and Shanxi Dian Guideng provinces.
The Chinese juniper wood preferably age of tree is 60 years.
Drying temperature is controlled at 50 DEG C.
Drying process is dried by the way of air-heater auxiliary air-dries.
Activated carbon is 100 grams.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.

Claims (6)

1. the method for polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper, it is characterised in that:This method comprises the following steps that:
1. select former material material process:Become a useful person the perennial wooden Chinese juniper wood rhizome material of Japan cypress and yellow Chinese juniper, with giant washes clean, Remove the impurity such as epidermis sandy soil;
2. drying process:1. described raw material are bakeed to water content below 10%;
3. pulverizing process:Long 6-7 centimetres, wide 2-3 centimetres, dry wood of the thickness at 0.2-0.3 centimetres is cut into mechanical chopper again Piece, fine crushing Chinese juniper wood fuzz stick, the particle powder between 10 to 30 mesh is become, loaded in the middle part of alembic;
4. low-pressure steam process:75-85 DEG C of vapor is produced in vapor generator, is entered from the lower steam import of alembic Enter, with the Chinese juniper wood raw material that fills carry out it is of short duration contact, after 30 to 50 seconds, start oil pump and vacuumize generation 40 and arrive 60kpa Negative pressure;After stable gas pressure, cooling is sprayed by normal-temperature water at the top of alembic, decompression humidification, at reduced pressure conditions with Chinese juniper The wood materials such as the rhizome of wood are sufficiently contacted so that the volatile ingredient such as essential oil in raw tissue, in less pyrolysis and water In the case of solution, by steam extraction and mix;
5. distillation process:After spending 20 to 30 minutes, the pressure of adjustment, first 0.1MPa voltage stabilizings 3-5 minutes, then allow 0.1MPa to be depressured To 0.05MPa, voltage stabilizing 5-8 minutes, and 0.05MPa is boosted into 0.1MPa, voltage stabilizing 3-5 minutes, then allow 0.1MPa to be depressurized to 0.05MPa, voltage stabilizing 20-30 minutes;Oil pump is closed, negative pressure is finally changed into normal ambient pressure, after spending 20-30 minutes again, is beaten The steam pipework above alembic is opened, connects coil condenser;
6. filter progress:The oil mixing with water condensate liquid of acquisition is subjected to filtration treatment, filtration treatment is clear by the impurity in mixed liquor Remove;
7. decolouring decoking process:Activated carbon is added to be decolourized;
8. water-oil separating process:It will filter, the oil-water mixture progress water-oil separating after decolouring decoking processing, the sweet smell of acquisition is more Essence and essential oil carry out sealing storage, complete whole technical process.
2. the method for polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper according to claim 1, it is characterised in that:Described Chinese juniper wood preferably originates in China western part Sichuan and Shanxi Dian Guideng provinces.
3. the method for polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper according to claim 1, it is characterised in that:Described The Chinese juniper wood preferably age of tree is more than 50 years.
4. the method for polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper according to claim 1, it is characterised in that:Described Drying temperature is controlled between 30-50 DEG C.
5. the method for polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper according to claim 1, it is characterised in that:Described Drying process is dried by the way of air-heater auxiliary air-dries.
6. the method for polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper according to claim 1, it is characterised in that:Described Activated carbon is 50-100 grams.
CN201711110724.1A 2017-11-13 2017-11-13 A kind of method that polyphenol powde and essential oil are extracted in the wood from Chinese juniper Withdrawn CN107805546A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109321363A (en) * 2018-09-30 2019-02-12 四川桧元素生物科技有限公司 A kind of method that low-temperature negative-pressure extracts Chinese juniper another name for oil and polyphenol powde
CN110540906A (en) * 2019-09-24 2019-12-06 亓桐月 method for preparing fendorin extracting solution
CN110742912A (en) * 2019-11-05 2020-02-04 深圳市芬多精纳米生物科技有限公司 Method for preparing nano fendorin
CN113845978A (en) * 2021-11-03 2021-12-28 上海木汗实业有限公司 Volatile liquid of hinoki extract and processing method thereof
CN115251448A (en) * 2022-08-22 2022-11-01 江西中烟工业有限责任公司 Efficient tobacco essential oil extraction equipment and method thereof

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CN102925291A (en) * 2012-11-22 2013-02-13 广西森呼吸科技工程有限公司 Variable pressure distillation method for extracting pythoncidere and essential oil from Chamaecyparis plants
CN105273843A (en) * 2015-11-27 2016-01-27 四川昱天成科技有限公司 Extraction method of wood essential oil
CN107216949A (en) * 2017-07-29 2017-09-29 安徽扬子生物科技有限公司 The transformation distillating method of polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper

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Publication number Priority date Publication date Assignee Title
CN102807921A (en) * 2012-09-14 2012-12-05 广西森呼吸科技工程有限公司 Method for preparing cypress essential oil by combining water vapor distillation with supercritical CO2 extraction
CN102925291A (en) * 2012-11-22 2013-02-13 广西森呼吸科技工程有限公司 Variable pressure distillation method for extracting pythoncidere and essential oil from Chamaecyparis plants
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CN107216949A (en) * 2017-07-29 2017-09-29 安徽扬子生物科技有限公司 The transformation distillating method of polyphenol powde and essential oil is extracted in a kind of wood from Chinese juniper

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109321363A (en) * 2018-09-30 2019-02-12 四川桧元素生物科技有限公司 A kind of method that low-temperature negative-pressure extracts Chinese juniper another name for oil and polyphenol powde
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CN110540906A (en) * 2019-09-24 2019-12-06 亓桐月 method for preparing fendorin extracting solution
CN110742912A (en) * 2019-11-05 2020-02-04 深圳市芬多精纳米生物科技有限公司 Method for preparing nano fendorin
CN113845978A (en) * 2021-11-03 2021-12-28 上海木汗实业有限公司 Volatile liquid of hinoki extract and processing method thereof
CN115251448A (en) * 2022-08-22 2022-11-01 江西中烟工业有限责任公司 Efficient tobacco essential oil extraction equipment and method thereof

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Application publication date: 20180316