CN106433951A - Extraction method of camphorated oil - Google Patents
Extraction method of camphorated oil Download PDFInfo
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- CN106433951A CN106433951A CN201610858399.6A CN201610858399A CN106433951A CN 106433951 A CN106433951 A CN 106433951A CN 201610858399 A CN201610858399 A CN 201610858399A CN 106433951 A CN106433951 A CN 106433951A
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- oil
- distillation
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Classifications
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
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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)
- Microbiology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an extraction method of camphorated oil. The method comprises the steps of crushing camphor branches and leaves to 50-80 meshes, leaching with aether petrolei, leaching for 2-4 times in cycles, after concentrating and recycling the aether petrolei, adding the concentrated liquid and material residue into a distilling device for distillation, cooling the distilled products and conducting the oil-water separation, collecting the oil layer and conducting the membrane filtration to obtain the camphorated oil product, at the same time conducting distillation again to the water layer acquired from the oil-water separation. The camphorated oil extracted by the method has the advantage of high extraction rate, low residues and higher quality.
Description
Technical field
The present invention relates to plant extract field, more particularly to a kind of extracting method of Oleum Camphora.
Background technology
Oleum Camphora is refined by Lignum cinnamomi camphorae fat, is a kind of colourless or faint yellow oily liquids to rufous, is dissolved in ethanol and ether,
There is strong Camphora abnormal smells from the patient, be ash-rich material, high volatility, the special delicate fragrance of Oleum Camphora, outside decapacitation Vermins-proof and mosquito-driving, also have more
The functions such as wound, deodorization are closed, purposes is quite varied.Oleum Camphora is picked with Cotton Gossypii, Camphora Cotton Gossypii ball is made, is placed in piano, or
In wood furniture, wardrobe, combing platform, can Anti-moth-eating, anti-Blatta seu periplaneta.Oleum Camphora is smeared along door and window, wall side, can be in anti-Blatta seu periplaneta enters.
Meanwhile, Oleum Camphora is fractionated into can extract Camphora, white camphor oil, red camphor oil and blue camphor oil, according to difference evaporate section main constituent difference and
There are different purposes.Extraction to Oleum Camphora is mainly extracted using vapor distillation at present, but there is the low and quality of extraction ratio
Low shortcoming.
Content of the invention
The present invention is for problem present in existing Oleum Camphora extractive technique, there is provided a kind of extracting method of Oleum Camphora,
The method can improve the extraction ratio of Oleum Camphora and quality.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of extracting method of Oleum Camphora, comprises the following steps that：
1) raw material is chosen：Choose more than 30 years Lignum cinnamomi camphorae branch and leaf of the age of tree to clean, the Lignum cinnamomi camphorae branch and leaf for cleaning up are crushed uniform
To 50-80 mesh；
2) extract：With petroleum ether leach step 1) gained raw material, volume ratio is 4: 1, and circulation extraction 2-4 time extracts 2 every time
Hour；
3) distill：By step 2) extract concentrating under reduced pressure recovery petroleum ether, concentrated solution is obtained, by concentrated solution, after extraction
Raw material and water put into distillating still distilled, be passed through steam direct heating into distillating still；Vacuum in distillating still for-
0.06--0.08MPa, vapo(u)rizing temperature is 120-150 DEG C；When distillation temperature in the kettle reaches 100-110 DEG C, open and distillating still
The condenser being connected, connects cooling water, by adjusting cooling water flow, the water temperature control of condenser cooling water outlet is existed
35-40℃；When distillation temperature in the kettle rises to 120-150 DEG C, start to calculate distillation time and by adjusting cooling water flow
The water temperature of condenser cooling water outlet is controlled at 28-33 DEG C, persistently 1.8-2.2 hour is distilled, then again by regulation
Cooling water flow controls the water temperature of condenser cooling water outlet at 24-28 DEG C or so, continues distillation 2.0-2.5 hour；
4) oil-water separation：The oil water mixture that condenser cooling is obtained is imported in oily-water seperating equipment, treats that profit is abundant
After layering, oil reservoir is collected；
5) membrane filtration：By step 4) oil reservoir collected carries out membrane filtration, obtains Camphora oil product.
As the preferred version of the present invention, step 5) membrane material used by membrane filtration be inorganic or organic membrane, molecular cut off
300-2000Da；During membrane filtration, control pressure is 0.1-0.6MPa, and control temperature is 25-40 DEG C.
As the preferred version of the present invention, step 4) lower aqueous layer isolated in oil water separation process is through distillating still upper end
Multiple fractional distillation column return distillating still repeat distillation.
As the preferred version of the present invention, step 2) water and concentrated solution in distillating still, the volume ratio of raw material after extraction
For 3-7: 1.
As the preferred version of the present invention, step 2) the petroleum ether boiling range specification be 60-90 DEG C.
Beneficial effects of the present invention：1st, raw material adopts Mechanical Crushing, improves the dissolution rate of Lignum cinnamomi camphorae fat；2nd, compared to existing
Have in vapor distillation and raw material is directly distilled, before it is distilled, raw material is extracted, impurity is reduced, improve
The quality of Oleum Camphora, alleviates the burden of subsequent treatment, while organic solvent can be reused, also reduces and produce into
This；3rd, the strict control condition parameter of still-process, using progressively heating up, can avoid temperature shock cause component occur replace or
Additive reaction, reduces the quality of Oleum Camphora；4th, oil reservoir adopts membrane filtration, reduces impurity, improves quality；
Specific embodiment
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
All other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
Embodiment 1
A kind of extracting method of Oleum Camphora, comprises the following steps that：
1) raw material is chosen：Choose more than 30 years Lignum cinnamomi camphorae branch and leaf of the age of tree to clean, the Lignum cinnamomi camphorae branch and leaf for cleaning up are crushed uniform
To 80 mesh；2) extract：Petroleum ether leach step 1 with boiling range is 80 DEG C) gained raw material, volume ratio is 4: 1, circulation extraction 2 times,
Extract 2 hours every time；3) distill：By step 2) extract concentrating under reduced pressure recovery petroleum ether, concentrated solution is obtained, by concentrated solution, warp
Raw material and water after extraction puts into distillating still with volume ratio 1: 4 and is distilled, and is passed through steam direct heating into distillating still；Distillation
Vacuum in kettle is -0.06MPa, and vapo(u)rizing temperature is 140 DEG C；When distillation temperature in the kettle reaches 100 DEG C, open and distillating still
The condenser being connected, connects cooling water, by adjusting cooling water flow, the water temperature control of condenser cooling water outlet is existed
35℃；When distillation temperature in the kettle rises to 140 DEG C, start to calculate distillation time and by adjusting cooling water flow by condenser
The water temperature of cooling water outlet controls at 28-33 DEG C, persistently distills 2 hours, then will be cold again by regulation cooling water flow
The water temperature of condenser cooling water outlet controls at 24-28 DEG C or so, continues distillation 2.2 hours；4) oil-water separation：Condenser is cold
But the oil water mixture for obtaining is imported in oily-water seperating equipment, after profit is fully layered, and collects oil reservoir, and lower aqueous layer is through distillation
The multiple fractional distillation column of kettle upper end returns distillating still and repeats distillation.5) membrane filtration：By step 4) oil reservoir collected carries out membrane filtration, film used
Material is inorganic or organic membrane, molecular cut off 300Da；During membrane filtration, control pressure is 0.1-0.6MPa, and control temperature is 25-
40 DEG C, obtain Camphora oil product.
Embodiment 2
A kind of extracting method of Oleum Camphora, comprises the following steps that：
1) raw material is chosen：Choose more than 30 years Lignum cinnamomi camphorae branch and leaf of the age of tree to clean, the Lignum cinnamomi camphorae branch and leaf for cleaning up are crushed uniform
To 50 mesh；2) extract：It is 60 DEG C of petroleum ether leach steps 1) gained raw material with boiling range, volume ratio is 4: 1, circulation extraction 4 times, per
Secondary extraction 2 hours；3) distill：By step 2) extract concentrating under reduced pressure recovery petroleum ether, concentrated solution is obtained, by concentrated solution, through extraction
Raw material and water after taking puts into distillating still with volume ratio 1: 7 and is distilled, and is passed through steam direct heating into distillating still；Distillating still
Interior vacuum is -0.08MPa, and vapo(u)rizing temperature is 150 DEG C；When distillation temperature in the kettle reaches 100 DEG C, open and distillating still phase
The condenser of connection, connects cooling water, is controlled the water temperature of condenser cooling water outlet 40 by adjusting cooling water flow
℃；When distill temperature in the kettle rise to 150 DEG C when, start calculate distillation time and by regulation cooling water flow condenser is cold
But the water temperature of water outlet controls at 28-33 DEG C, persistently distills 1.8 hours, then will be cold again by regulation cooling water flow
The water temperature of condenser cooling water outlet controls at 24-28 DEG C or so, continues distillation 2.5 hours；4) oil-water separation：Condenser is cold
But the oil water mixture for obtaining is imported in oily-water seperating equipment, after profit is fully layered, and collects oil reservoir, and lower aqueous layer is through distillation
The multiple fractional distillation column of kettle upper end returns distillating still and repeats distillation；5) membrane filtration：By step 4) oil reservoir collected carries out membrane filtration, film used
Material is inorganic or organic membrane, molecular cut off 2000Da；During membrane filtration, control pressure is 0.1-0.6MPa, and control temperature is
25-40 DEG C, obtain Camphora oil product.
Claims (5)
1. a kind of extracting method of Oleum Camphora, it is characterised in that comprise the following steps：
1) raw material is chosen：Choose more than 30 years Lignum cinnamomi camphorae branch and leaf of the age of tree to clean, the Lignum cinnamomi camphorae branch and leaf for cleaning up are crushed uniformly to 50-
80 mesh；
2) extract：With petroleum ether leach step 1) gained raw material, volume ratio is 4: 1, circulation extraction 2-4 time, and extraction 2 is little every time
When；
3) distill：By step 2) extract concentrating under reduced pressure recovery petroleum ether, concentrated solution is obtained, by concentrated solution, the original after extraction
Material and water put into distillating still and are distilled, and are passed through steam direct heating into distillating still；Vacuum in distillating still is -0.06--
0.08MPa, vapo(u)rizing temperature is 120-150 DEG C；When distillation temperature in the kettle reaches 100-110 DEG C, open and be connected with distillating still
Condenser, connect cooling water, controlled the water temperature of condenser cooling water outlet in 35-40 by adjusting cooling water flow
℃；When distillation temperature in the kettle rises to 120-150 DEG C, start to calculate distillation time and by adjusting cooling water flow by condensation
The water temperature of device cooling water outlet controls at 28-33 DEG C, persistently distills 1.8-2.2 hour, then again by regulation cooling water
Flow controls the water temperature of condenser cooling water outlet at 24-28 DEG C or so, continues distillation 2.0-2.5 hour；
4) oil-water separation：The oil water mixture that condenser cooling is obtained is imported in oily-water seperating equipment, treats that profit is fully layered
Afterwards, oil reservoir is collected；
5) membrane filtration：By step 4) oil reservoir collected carries out membrane filtration, obtains Camphora oil product.
2. the extracting method of Oleum Camphora according to claim 1, it is characterised in that step 5) membrane material used by membrane filtration is
Inorganic or organic membrane, molecular cut off 300-2000Da；During membrane filtration, control pressure is 0.1-0.6MPa, and control temperature is 25-
40℃.
3. the extracting method of Oleum Camphora according to claim 1, it is characterised in that step 4) separate in oil water separation process
Multiple fractional distillation column of the lower aqueous layer for going out through distillating still upper end returns distillating still and repeats distillation.
4. the extracting method of Oleum Camphora according to claim 1, it is characterised in that step 2) water and concentration in distillating still
Liquid, the volume ratio of raw material after extraction are 3-7: 1.
5. the extracting method of Oleum Camphora according to claim 1, it is characterised in that step 2) the petroleum ether boiling range specification
For 60-90 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610858399.6A CN106433951A (en) | 2016-09-22 | 2016-09-22 | Extraction method of camphorated oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610858399.6A CN106433951A (en) | 2016-09-22 | 2016-09-22 | Extraction method of camphorated oil |
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| Publication Number | Publication Date |
|---|---|
| CN106433951A true CN106433951A (en) | 2017-02-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610858399.6A Pending CN106433951A (en) | 2016-09-22 | 2016-09-22 | Extraction method of camphorated oil |
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| Country | Link |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903998A (en) * | 2018-01-03 | 2018-04-13 | 黄振忠 | A kind of technique for processing extraction camphorated oil using yellow cinnamon leaf |
| CN109971546A (en) * | 2019-04-10 | 2019-07-05 | 范加家 | A kind of high-voltage pulse extracting method of borneol essential oil |
| CN116497619A (en) * | 2023-05-17 | 2023-07-28 | 岳阳林纸股份有限公司 | Natural color chemimechanical pulping process for camphorwood sodium hydroxide |
-
2016
- 2016-09-22 CN CN201610858399.6A patent/CN106433951A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903998A (en) * | 2018-01-03 | 2018-04-13 | 黄振忠 | A kind of technique for processing extraction camphorated oil using yellow cinnamon leaf |
| CN109971546A (en) * | 2019-04-10 | 2019-07-05 | 范加家 | A kind of high-voltage pulse extracting method of borneol essential oil |
| CN116497619A (en) * | 2023-05-17 | 2023-07-28 | 岳阳林纸股份有限公司 | Natural color chemimechanical pulping process for camphorwood sodium hydroxide |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170222 |