CN110803979A - Natural linalool extraction technology - Google Patents
Natural linalool extraction technology Download PDFInfo
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- CN110803979A CN110803979A CN201911150538.XA CN201911150538A CN110803979A CN 110803979 A CN110803979 A CN 110803979A CN 201911150538 A CN201911150538 A CN 201911150538A CN 110803979 A CN110803979 A CN 110803979A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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Abstract
The invention discloses a natural linalool extraction process, which comprises raw material pretreatment, solvent extraction, separation, impurity removal and reduced pressure concentration. The invention adopts the solvent method to extract the essential oil of the cinnamomum camphora leaves, thereby not only improving the yield of the cinnamomum camphora leaves, having lower temperature in the whole extraction process, low energy consumption and low cost, but also preventing the cinnamomum camphora from being oxidized and deteriorated by heating caused by overhigh temperature, improving the quality of the cinnamomum camphora products, and overcoming the problems of low product yield and poor product quality caused by adopting a steam distillation method. According to the method, the mixed solvent of ethanol and ethyl acetate is used as the extracting agent, compared with a single ethanol solvent, the extraction rate of linalool is improved by about 20%, and the coarse product can be more finely filtered through the three layers of filter screens, so that the working efficiency of people is increased.
Description
Technical Field
The invention relates to an alcohol extraction process, in particular to an alcohol extraction process of natural linalool.
Background
The camphor tree essential oil is colorless or light yellow oily transparent liquid at normal temperature, partial components can separate out solid components at normal temperature, and the camphor tree essential oil has strong special smell, strong volatility and high refractive index and optical rotation mostly; the specific gravity is between O.86 and 1.065; the product is hardly soluble in water, can be completely soluble in absolute ethyl alcohol, can be soluble in organic solvents with small polarity such as ether, chloroform, petroleum ether and the like, is sensitive to air, light and temperature, and is easy to volatilize and decompose. The camphor tree essential oil contains linalool, linalool and the like which are the most abundant, and is known as 3, 7-dimethyl-1, 6-octadiene-3-ol with a chemical formula of C10H 18O. Linalool is colorless or light yellow transparent liquid, is insoluble in water, can be dissolved in ethanol and diethyl ether, has pleasant sweet smell, soft fragrance, and is widely applied to spices, essence, perfume and perfumed soap, is important in monomer spices, and is called as spice Meiwang; meanwhile, linalool is a raw material for synthesizing vitamin E, and is applied to medicines due to the effects of antibiosis, antivirus, analgesia and the like.
At present, the natural linalool production in China still adopts a steam distillation method, because the process is laggard and the technical conditions are poor, the product yield and the product quality are low, the resource utilization is extremely insufficient, and the subsequent working efficiency is influenced because the filter screen generally adopts conventional filtration. Therefore, we improve the technology and propose a natural linalool extraction technology.
Disclosure of Invention
In order to solve the technical problems, the invention provides the following technical scheme:
the invention relates to a natural linalool extraction process, which comprises the following steps:
(1) pretreatment of raw materials: drying and crushing fresh cinnamomum camphora leaves, and crushing to 90 meshes to obtain powdery materials;
(2) solvent extraction: opening a feed inlet of the leaching device, adding a powdery material, adding a mixed solvent of ethanol and ethyl acetate according to the weight ratio of the powdery material to the solvent of 5-9:2, covering a feed inlet cover, closing a heater and a pump power supply, raising the temperature for cyclic extraction, controlling the temperature to be 70-75 ℃, performing cyclic leaching for 3-4 hours, discharging the material from a discharge outlet, and removing residues through a filtering device to obtain a crude product; the circulating extraction is carried out through eight accelerated leaching mixing areas of pump pressurization mixing, nozzle jet mixing, mixing pipe mixing, baffle cover reflection mixing, tank body flow mixing and pipeline flow mixing, so as to strengthen the leaching of active ingredients;
(3) separation: putting the crude product obtained in the step (2) into a distillation retort, distilling at the temperature of 80-82 ℃, and recovering the mixed solvent to obtain crude cinnamomum camphora essential oil;
(4) removing impurities: drying the crude cinnamomum camphora essential oil by using anhydrous sodium sulfate, and then filtering the dried cinnamomum camphora essential oil by using a conventional method to obtain an extract;
(5) and (3) concentrating under reduced pressure: and (3) decompressing and concentrating the extract obtained in the step (4) in a rotary evaporator, controlling the vacuum degree to be 0.08-0.09Mpa, and evaporating at the temperature of 70-80 ℃ to obtain the high-purity linalool.
As a preferred technical scheme of the invention, the leaching device in the step (2) comprises an extraction tank, a mixing pipe and a pump, wherein the mixing pipe is fixed on a central axis of the extraction tank through a mixing pipe support rod, a nozzle is arranged at one end of the extraction tank in a sealing manner, a blocking cover is arranged at the other end of the extraction tank, the blocking cover is fixed on the sealing cover of the extraction tank through a blocking cover support rod, the nozzle is communicated with a discharge hole of the pump through a circulating pipe provided with a heater, a feed inlet of the pump is connected with the other port of the extraction tank through the circulating pipe, a feed inlet is arranged above the extraction tank, and a discharge hole is also arranged at the bottom of the extraction tank.
As a preferred technical scheme of the invention, the mixing pipe is an internal spiral pipe body, and one end of the mixing pipe corresponding to the nozzle is provided with a horn-shaped feed inlet.
As a preferable technical scheme of the invention, the extraction tank is also provided with a temperature measuring instrument.
As a preferred technical scheme of the invention, the filtering device in the step (2) comprises a filtering frame and three layers of filtering nets, wherein the three layers of filtering nets are sequentially and movably arranged on the filtering frame, and the diameters of the meshes of the three layers of filtering nets are sequentially reduced.
As a preferable technical scheme of the invention, the weight ratio of the ethanol to the ethyl acetate is 2-5: 3.
The invention has the beneficial effects that: according to the natural linalool extraction process, the essential oil of the linalool leaves is extracted by adopting a solvent method, so that the yield of the linalool is improved, the temperature in the whole extraction process is lower, the energy consumption is low, the cost is low, the linalool can be prevented from being oxidized and deteriorated by heating due to overhigh temperature, the quality of an linalool product is improved, and the problems of low product yield and poor product quality in a steam distillation method are solved. According to the method, the mixed solvent of ethanol and ethyl acetate is used as the extracting agent, compared with a single ethanol solvent, the extraction rate of linalool is improved by about 20%, and the coarse product can be more finely filtered through the three layers of filter screens, so that the working efficiency of people is increased.
The examples of the present invention are provided for the purpose of explanation and are not to be construed as limiting the invention.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example (b): the invention relates to a natural linalool extraction process, which comprises the following steps:
(1) pretreatment of raw materials: drying and crushing fresh cinnamomum camphora leaves, and crushing to 90 meshes to obtain powdery materials;
(2) solvent extraction: opening a feed inlet of the leaching device, adding a powdery material, adding a mixed solvent of ethanol and ethyl acetate according to the weight ratio of the powdery material to the solvent of 5-9:2, covering a feed inlet cover, closing a heater and a pump power supply, raising the temperature for cyclic extraction, controlling the temperature to be 70-75 ℃, performing cyclic leaching for 3-4 hours, discharging the material from a discharge outlet, and removing residues through a filtering device to obtain a crude product; the circulating extraction is carried out through eight accelerated leaching mixing areas of pump pressurization mixing, nozzle jet mixing, mixing pipe mixing, baffle cover reflection mixing, tank body flow mixing and pipeline flow mixing, so as to strengthen the leaching of active ingredients;
(3) separation: putting the crude product obtained in the step (2) into a distillation retort, distilling at the temperature of 80-82 ℃, and recovering the mixed solvent to obtain crude cinnamomum camphora essential oil;
(4) removing impurities: drying the crude cinnamomum camphora essential oil by using anhydrous sodium sulfate, and then filtering the dried cinnamomum camphora essential oil by using a conventional method to obtain an extract;
(5) and (3) concentrating under reduced pressure: and (3) decompressing and concentrating the extract obtained in the step (4) in a rotary evaporator, controlling the vacuum degree to be 0.08-0.09Mpa, and evaporating at the temperature of 70-80 ℃ to obtain the high-purity linalool.
Wherein, step (2) the leaching device is including drawing jar, hybrid tube and pump, the hybrid tube is fixed on the axis of drawing the jar through the hybrid tube bracing piece, the one end closing cap of drawing the jar is equipped with the nozzle, and the other end of drawing the jar is equipped with the fender lid, the fender lid is fixed on the closing cap of drawing the jar through keeping off the lid bracing piece, the nozzle is through the circulating pipe that is equipped with the heater and the discharge gate intercommunication of pump, the feed inlet of pump passes through the circulating pipe and is connected with another port of drawing the jar, the top of drawing the jar is equipped with the charge door, and the bottom of drawing the jar still is equipped with the bin outlet.
Wherein, the mixing tube is an internal spiral tube body, and one end of the mixing tube corresponding to the nozzle is provided with a trumpet-shaped feed inlet.
Wherein, the extraction tank is also provided with a temperature measuring instrument.
Wherein, step (2) filter equipment includes filtering frame and three-layer filter screen, and the three-layer filter screen is in proper order the activity setting on filtering frame, and the mesh diameter of three-layer filter screen reduces in proper order.
Wherein the weight ratio of the ethanol to the ethyl acetate is 2-5: 3.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A natural linalool extraction process comprises the following steps:
(1) pretreatment of raw materials: drying and crushing fresh cinnamomum camphora leaves, and crushing to 90 meshes to obtain powdery materials;
(2) solvent extraction: opening a feed inlet of the leaching device, adding a powdery material, adding a mixed solvent of ethanol and ethyl acetate according to the weight ratio of the powdery material to the solvent of 5-9:2, covering a feed inlet cover, closing a heater and a pump power supply, raising the temperature for cyclic extraction, controlling the temperature to be 70-75 ℃, performing cyclic leaching for 3-4 hours, discharging the material from a discharge outlet, and removing residues through a filtering device to obtain a crude product; the circulating extraction is carried out through eight accelerated leaching mixing areas of pump pressurization mixing, nozzle jet mixing, mixing pipe mixing, baffle cover reflection mixing, tank body flow mixing and pipeline flow mixing, so as to strengthen the leaching of active ingredients;
(3) separation: putting the crude product obtained in the step (2) into a distillation retort, distilling at the temperature of 80-82 ℃, and recovering the mixed solvent to obtain crude cinnamomum camphora essential oil;
(4) removing impurities: drying the crude cinnamomum camphora essential oil by using anhydrous sodium sulfate, and then filtering the dried cinnamomum camphora essential oil by using a conventional method to obtain an extract;
(5) and (3) concentrating under reduced pressure: and (3) decompressing and concentrating the extract obtained in the step (4) in a rotary evaporator, controlling the vacuum degree to be 0.08-0.09Mpa, and evaporating at the temperature of 70-80 ℃ to obtain the high-purity linalool.
2. The natural linalool extraction process according to claim 1, characterized in that, step (2) the leaching device is including extracting jar, hybrid tube and pump, the hybrid tube is fixed on the axis of extracting the jar through the hybrid tube bracing piece, the one end closing cap of extracting the jar is equipped with the nozzle, and the other end of extracting the jar is equipped with keeps off the lid, keep off the lid and fix on the closing cap of extracting the jar through keeping off the lid bracing piece, the nozzle is through the circulating pipe that is equipped with the heater and the discharge gate intercommunication of pump, the feed inlet of pump passes through the circulating pipe and is connected with another port of extracting the jar, the top of extracting the jar is equipped with the charge door, and the bottom of extracting the jar still is equipped with the bin outlet.
3. The extraction process of natural linalool according to claim 1, wherein the mixing tube is an internal spiral tube, and a flared feeding port is provided at one end of the mixing tube corresponding to the nozzle.
4. The extraction process of natural linalool according to claim 1, characterized in that said extraction tank is further equipped with a temperature measuring instrument.
5. The natural linalool extraction process according to claim 1, wherein the filtration device of step (2) comprises a filtration frame and three layers of filtration screens, the three layers of filtration screens are sequentially movably disposed on the filtration frame, and the mesh diameters of the three layers of filtration screens are sequentially reduced.
6. The natural linalool extraction process according to claim 1, wherein the weight ratio of ethanol to ethyl acetate is 2-5: 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911150538.XA CN110803979A (en) | 2019-11-21 | 2019-11-21 | Natural linalool extraction technology |
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| CN201911150538.XA CN110803979A (en) | 2019-11-21 | 2019-11-21 | Natural linalool extraction technology |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484392A (en) * | 2020-05-06 | 2020-08-04 | 厦门阿胜生态科技有限公司 | Preparation method of solid linalool |
| CN113185381A (en) * | 2021-04-20 | 2021-07-30 | 金溪华香香料有限公司 | Method for separating and extracting linalool by taking camphor tree leaves as raw materials through high-speed countercurrent chromatography |
| CN113185401A (en) * | 2021-04-20 | 2021-07-30 | 金溪华香香料有限公司 | Synthesis process of linalyl acetate |
-
2019
- 2019-11-21 CN CN201911150538.XA patent/CN110803979A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484392A (en) * | 2020-05-06 | 2020-08-04 | 厦门阿胜生态科技有限公司 | Preparation method of solid linalool |
| CN113185381A (en) * | 2021-04-20 | 2021-07-30 | 金溪华香香料有限公司 | Method for separating and extracting linalool by taking camphor tree leaves as raw materials through high-speed countercurrent chromatography |
| CN113185401A (en) * | 2021-04-20 | 2021-07-30 | 金溪华香香料有限公司 | Synthesis process of linalyl acetate |
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Application publication date: 20200218 |