CN109456835A - A kind of preparation method of redwood essential oil - Google Patents
A kind of preparation method of redwood essential oil Download PDFInfo
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- CN109456835A CN109456835A CN201811452155.3A CN201811452155A CN109456835A CN 109456835 A CN109456835 A CN 109456835A CN 201811452155 A CN201811452155 A CN 201811452155A CN 109456835 A CN109456835 A CN 109456835A
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- Prior art keywords
- redwood
- temperature
- extraction
- essential oil
- molecular distillation
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Classifications
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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
-
- 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
- C11B9/025—Recovery by solvent extraction
-
- 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
- C11B9/027—Recovery of volatiles by distillation or stripping
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to plant extraction technical fields, disclose a kind of preparation method of redwood essential oil, the specific steps are as follows: the redwood sawdust that will be crushed first is added entrainer and carries out supercritical CO2Extraction, obtains extract liquor, to extract liquor separating treatment, then is concentrated in vacuo, obtain medicinal extract, and medicinal extract is finally carried out two-stage molecular distillation, obtains high-purity redwood essential oil.The present invention is by supercritical CO2Extraction and molecular distillation technique combine, and simple process safety, product no solvent residue is easy to continuous large-scale production.
Description
Technical field
The invention belongs to plant extraction technical field more particularly to a kind of preparation methods of redwood essential oil.
Background technique
Redwood refers to Pterocarpus, Dalbergia, Diospyros, precipice Macroptilium and the heartwood of Cassia tree species, altogether includes narra class, flower
Pear wood class, fragrant branch wood class, nigrotic acid branch wood class, red acid branch wood class, 8 major class timber of ebony class, striped ebony class and Door frame class.Greatly
Part redwood has its unique smell, as fragrant branch wood has strong pungent fragrance；Rosewood has fragrant；Red acid branch wood has
Deep or light different sour gas.For the furniture made of redwood because its is fine quality, hard durable, beautiful design, serious elegance, collection is real
With, it is ornamental, preserve value in one, it is all the time all deep to be liked by the majority of consumers.In mahogany furniture manufacturing process, it can generate
A large amount of sawdust, these sawdusts result in waste of resources often when rubbish is lost, if extracting redwood essential oil using these sawdusts,
It can be formulated into essence, mahogany furniture essential oil for maintaining etc. with radix aucklandiae taste, there is certain use value, the receipts of enterprise can be increased
Enter.Currently, being had not been reported using the patented technology that sawdust prepares redwood essential oil.This patent provides supercritical carbon dioxide extracting
The method for preparing redwood essential oil with molecular clock GC-MS has simple process, can continuous scale industrial production.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of mahogany furniture processing waste comprehensive utilization, with mahogany furniture plus
The waste of work --- sawdust is raw material, using supercritical CO2Extraction and molecular distillation technique prepare redwood essential oil.Using this hair
Redwood essential oil made from bright method is red, transparent, and impurity is few, good fluidity, there is strong timber fragrance, long shelf-life, quality
It is good.
Technical solution of the present invention:
A kind of preparation method of redwood essential oil, steps are as follows:
Step 1: supercritical CO2Extraction
The redwood sawdust after pulverizing and sieving is taken, is that entrainer is added in 1:1 according to mass ratio, then fills this blend into super face
Boundary CO2In extraction kettle；Control supercritical CO2Extracting pressure in extraction kettle is 25~40MPa, and extraction temperature is 40~60 DEG C, extraction
Taking circulation time is 1.5~3h；Extraction process is passed through the CO that temperature is regulated in storage tank2, flow control is 15~25L/h；
Supercritical CO2In extraction kettle after reaction, extract liquor enters in separating still 1, and control 1 pressure of separating still is 8~14MPa,
Separation temperature is 40~50 DEG C, enters back into separating still 2 by the thick extract liquor obtained after separation of separating still 1 and further separates, control
2 pressure 5MPa of separating still processed, separation temperature are 40~50 DEG C, obtain exquisite extract liquor；
Step 2: vacuum concentration
Under vacuum conditions by exquisite extract liquor, it is concentrated, obtains medicinal extract；40~70 DEG C of temperature are concentrated under reduced pressure, vacuum
Degree is 4 × 104Pa~8 × 104Pa；
Step 3: molecular distillation
Two-stage molecular distillation is carried out to medicinal extract, condensation obtains the redwood essential oil of high-purity；
First order molecular distillation is thin film evaporator, and devolatilization vacuum degree is 8 × 103Pa~6 × 104Pa, degassing temperature 60
~100 DEG C；
The vacuum degree of second level molecular distillation is 0.1Pa~10Pa, and vapo(u)rizing temperature is 130~170 DEG C；
20~40 DEG C of condensation temperature.
In step 1, the mesh number of crushing is 30~50 mesh.
In step 1, entrainer is that the ethyl alcohol of methanol, dehydrated alcohol, ethyl acetate or 80% or more volume fraction is water-soluble
Liquid.
Beneficial effects of the present invention:
(1) extraction temperature is low, and yield is high, fragrance loss is few.
(2) it is refined using medicinal extract of the molecular distillation to extraction, under high vacuum state, material heated time is short, no
It easily decomposes and oxidation, essential oil quality is good.
Detailed description of the invention
Fig. 1 is the flow diagram of preparation method of the present invention.
Specific embodiment
The present invention is more specifically described in detail combined with specific embodiments below, but embodiments of the present invention are unlimited
Routine techniques progress can refer to for not specifically specified technological parameter in this.
Embodiment 1
A kind of preparation method of redwood essential oil, comprising the following steps:
Step 1: supercritical CO2Extraction
Redwood sawdust is ground into 30 mesh powders with pulverizer, the redwood powder weighing after pulverizing and sieving takes 500g,
And mixed with the dehydrated alcohol of 500g, it stirs evenly, is then loaded into supercritical CO2In extraction kettle, by extraction kettle, separating still
1, the temperature of separating still 2 is respectively set as 50 DEG C, 45 DEG C and 45 DEG C.Kettle, separating still and storage tank cooling temperature to be extracted reach respectively
To after set temperature, CO is opened2Gas cylinder valve starts CO2High-pressure pump, by CO2It is sent into extractor and knockout drum, control valve
Aperture, the pressure of extraction kettle, separating still 1 and separating still 2 is controlled respectively in 25MPa, 12MPa and 5MPa, CO2Flow control
It for 20L/h, extracts 2 hours, slowly opens the valve under separating still 1, collection obtains extract liquor 585g.
Step 2: vacuum concentration
Extract liquor is concentrated under vacuum, 50 DEG C of thickening temperature, vacuum degree is 4 × 104Pa.After concentration, soaked
Cream 91g.
Step 3: molecular distillation
Medicinal extract is subjected to two-stage molecular distillation, obtains the redwood essential oil of 22.5g, yield 45g/Kg.The molecule one
Grade degassing temperature is 80 DEG C, vacuum degree 4 × 104Pa, 140 DEG C of secondary distillation temperature, vacuum degree 5Pa.
Embodiment 2
Redwood sawdust is ground into 30 mesh powders with pulverizer, the redwood powder weighing after pulverizing and sieving takes 500g,
And mixed with the dehydrated alcohol of 500g, it stirs evenly, is then loaded into supercritical CO2In extraction kettle, by extraction kettle, separating still
1, the temperature of separating still 2 is respectively set as 60 DEG C, 55 DEG C and 45 DEG C.Kettle, separating still and storage tank cooling temperature to be extracted reach respectively
To after set temperature, CO is opened2Gas cylinder valve starts CO2High-pressure pump, by CO2It is sent into extractor and knockout drum, control valve
Aperture, the pressure of extraction kettle, separating still 1 and separating still 2 is controlled respectively in 35MPa, 14MPa and 5MPa, CO2Flow control
It for 15L/h, extracts 3 hours, slowly opens the valve under separating still 1, collection obtains extract liquor 601g.
Step 2: vacuum concentration
Extract liquor is concentrated under vacuum, 60 DEG C of thickening temperature, vacuum degree is 5 × 104Pa.After concentration, soaked
Cream 102g.
Step 3: molecular distillation
Medicinal extract is subjected to two-stage molecular distillation, obtains the redwood essential oil of 26g, yield 52g/Kg.The molecule level-one
Degassing temperature is 90 DEG C, vacuum degree 4.5 × 104Pa, 160 DEG C of secondary distillation temperature, vacuum degree 2Pa.
Embodiment 3
Redwood sawdust is ground into 20 mesh powders with pulverizer, the redwood powder weighing after pulverizing and sieving takes 500g,
And mixed with 500g volume fraction for 95% ethyl alcohol, it stirs evenly, is then loaded into supercritical CO2In extraction kettle, it will extract
The temperature of kettle, separating still 1, separating still 2 is taken to be respectively set as 55 DEG C, 50 DEG C and 45 DEG C.Kettle, separating still and storage tank to be extracted are cooling
After temperature respectively reaches set temperature, CO is opened2Gas cylinder valve starts CO2High-pressure pump, by CO2It is sent into extractor and knockout drum
In, the aperture of control valve controls respectively the pressure of extraction kettle, separating still 1 and separating still 2 in 20MPa, 10MPa and 5MPa,
CO2Flow control is 25L/h, is extracted 2.5 hours, and the valve under separating still 1 is slowly opened, and collection obtains extract liquor 565g.
Step 2: vacuum concentration
Extract liquor is concentrated under vacuum, 65 DEG C of thickening temperature, vacuum degree is 4.5 × 104Pa.After concentration, obtain
Medicinal extract 82g.
Step 3: molecular distillation
Medicinal extract is subjected to two-stage molecular distillation, obtains the redwood essential oil of 17.5g, yield 35g/Kg.The molecule one
Grade degassing temperature is 750 DEG C, vacuum degree 4 × 104Pa, 1450 DEG C of secondary distillation temperature, vacuum degree 2Pa.
Claims (3)
1. a kind of preparation method of redwood essential oil, which is characterized in that steps are as follows:
Step 1: supercritical CO2Extraction
The redwood sawdust after pulverizing and sieving is taken, is that entrainer is added in 1:1 according to mass ratio, then fills this blend into supercritical CO2
In extraction kettle；Control supercritical CO2Extracting pressure in extraction kettle is 25~40MPa, and extraction temperature is 40~60 DEG C, and extraction follows
The ring time is 1.5~3h；Extraction process is passed through the CO that temperature is regulated in storage tank2, flow control is 15~25L/h；It is super to face
Boundary CO2In extraction kettle after reaction, extract liquor enters in separating still 1, and control 1 pressure of separating still is 8~14MPa, separation
Temperature is 40~50 DEG C, enters back into separating still 2 by the thick extract liquor obtained after separation of separating still 1 and further separates, control point
From 2 pressure 5MPa of kettle, separation temperature is 40~50 DEG C, obtains exquisite extract liquor；
Step 2: vacuum concentration
Under vacuum conditions by exquisite extract liquor, it is concentrated, obtains medicinal extract；40~70 DEG C of temperature are concentrated under reduced pressure, vacuum degree 4
×104Pa~8 × 104Pa；
Step 3: molecular distillation
Two-stage molecular distillation is carried out to medicinal extract, condensation obtains the redwood essential oil of high-purity；
First order molecular distillation is thin film evaporator, and devolatilization vacuum degree is 8 × 103Pa~6 × 104Pa, degassing temperature be 60~
100℃；
The vacuum degree of second level molecular distillation is 0.1Pa~10Pa, and vapo(u)rizing temperature is 130~170 DEG C；
20~40 DEG C of condensation temperature.
2. the preparation method of redwood essential oil according to claim 1, which is characterized in that in step 1, the mesh number of crushing is
30~50 mesh.
3. the preparation method of redwood essential oil according to claim 1 or 2, which is characterized in that in step 1, the entrainment
Agent is the ethanol water of methanol, dehydrated alcohol, ethyl acetate or 80% or more volume fraction.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811452155.3A CN109456835A (en) | 2018-11-30 | 2018-11-30 | A kind of preparation method of redwood essential oil |
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| CN201811452155.3A CN109456835A (en) | 2018-11-30 | 2018-11-30 | A kind of preparation method of redwood essential oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368795A (en) * | 2019-07-26 | 2019-10-25 | 杨鑫 | A kind of natural lignin's formaldehyde purifying agent and preparation method thereof |
| CN113442251A (en) * | 2021-07-08 | 2021-09-28 | 浙江省林业科学研究院 | Bamboo and/or wood coloring method |
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| CN101259247A (en) * | 2008-04-22 | 2008-09-10 | 美晨集团股份有限公司 | Method for continuously extracting various active ingredient in turmeric |
| CN102618072A (en) * | 2012-01-12 | 2012-08-01 | 华南理工大学 | Method for refining capsanthin by enzyme catalysis, esterification and molecular distillation |
| CN104818118A (en) * | 2015-04-21 | 2015-08-05 | 绍兴文理学院 | Production process and equipment for extracting rosewood essential oil from rosewood chips |
| CN105368579A (en) * | 2015-12-09 | 2016-03-02 | 江西天美生物科技有限公司 | Production method used for producing cunninghamia lanceolata biological essential oil from cunninghamia lanceolata saw dust |
| CN106987316A (en) * | 2017-04-17 | 2017-07-28 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of the red sandalwood essential oil with bacteriostatic activity |
| CN107397699A (en) * | 2017-09-28 | 2017-11-28 | 深圳市天香赋生物科技有限公司 | A kind of extracting method of Lignum Aquilariae Resinatum extract |
| CN107410469A (en) * | 2017-09-25 | 2017-12-01 | 广西壮族自治区农业科学院农产品加工研究所 | The extracting method of a kind of mango core essential oil and its in the fresh-keeping application of dragon fruit |
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- 2018-11-30 CN CN201811452155.3A patent/CN109456835A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101259247A (en) * | 2008-04-22 | 2008-09-10 | 美晨集团股份有限公司 | Method for continuously extracting various active ingredient in turmeric |
| CN102618072A (en) * | 2012-01-12 | 2012-08-01 | 华南理工大学 | Method for refining capsanthin by enzyme catalysis, esterification and molecular distillation |
| CN104818118A (en) * | 2015-04-21 | 2015-08-05 | 绍兴文理学院 | Production process and equipment for extracting rosewood essential oil from rosewood chips |
| CN105368579A (en) * | 2015-12-09 | 2016-03-02 | 江西天美生物科技有限公司 | Production method used for producing cunninghamia lanceolata biological essential oil from cunninghamia lanceolata saw dust |
| CN106987316A (en) * | 2017-04-17 | 2017-07-28 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of the red sandalwood essential oil with bacteriostatic activity |
| CN107410469A (en) * | 2017-09-25 | 2017-12-01 | 广西壮族自治区农业科学院农产品加工研究所 | The extracting method of a kind of mango core essential oil and its in the fresh-keeping application of dragon fruit |
| CN107397699A (en) * | 2017-09-28 | 2017-11-28 | 深圳市天香赋生物科技有限公司 | A kind of extracting method of Lignum Aquilariae Resinatum extract |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368795A (en) * | 2019-07-26 | 2019-10-25 | 杨鑫 | A kind of natural lignin's formaldehyde purifying agent and preparation method thereof |
| CN113442251A (en) * | 2021-07-08 | 2021-09-28 | 浙江省林业科学研究院 | Bamboo and/or wood coloring method |
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Application publication date: 20190312 |
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