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CN110923068A - White camphor oil extraction process - Google Patents

White camphor oil extraction process Download PDF

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Publication number
CN110923068A
CN110923068A CN201911160072.1A CN201911160072A CN110923068A CN 110923068 A CN110923068 A CN 110923068A CN 201911160072 A CN201911160072 A CN 201911160072A CN 110923068 A CN110923068 A CN 110923068A
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CN
China
Prior art keywords
camphor
oil
stainless steel
white
pot
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CN201911160072.1A
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Chinese (zh)
Inventor
徐国平
李国进
饶治平
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Jiangxi Yisite Spices Ltd
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Jiangxi Yisite Spices Ltd
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Priority to CN201911160072.1A priority Critical patent/CN110923068A/en
Publication of CN110923068A publication Critical patent/CN110923068A/en
Pending legal-status Critical Current

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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

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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)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a white camphor oil extraction process, which is characterized by comprising the following steps: (1) selecting raw materials: selecting old camphor trunks or roots or camphor tree branches and leaves; (2) and (3) distillation: distilling with a stainless steel distilling pot, wherein a wooden steaming barrel is arranged in the stainless steel distilling pot, and the stainless steel distilling pot is connected with a coil condenser for distilling; (3) cooling and separating the vapor with camphor and camphor oil, and filtering to obtain crude camphor and camphor oil; (4) re-steaming and purifying: when camphor oil is used for extracting camphor, the camphor oil is put into a stainless steel distillation pot for secondary distillation, distillate at the temperature of 155 ℃ and 200 ℃ is collected to be called white oil, the white oil is cooled to separate out crystallized camphor, then the white oil is filtered, and the filtrate is repeatedly distilled for several times until no camphor is separated out, so that the white camphor oil is obtained. The invention adopts the modes of negative pressure distillation and ultrasonic assistance to improve the distillation efficiency and the yield.

Description

White camphor oil extraction process
Technical Field
The invention belongs to the technical field of spice and essence, and relates to a white camphor oil extraction process.
Background
The camphor wood oil is mainly used for medicine and preparing essence for soap, and can also be used for preparing varnish, shoe polish and the like. Camphor oil is mainly composed of various terpenoids. Generally, multi-tower continuous vacuum distillation is combined with freezing, sublimation and other processes to prepare refined camphor, various essential oils (such as eucalyptol, linalool, pine oil, safrole) and byproducts (such as white camphor oil, red camphor oil and blue camphor oil). The white camphor oil is a volatile oil obtained by distilling and fractionating camphor tree of Lauraceae or other plants of the same genus, and is the first fraction essential oil obtained by vacuum distilling camphor oil. The boiling range is 160-185 ℃ under normal pressure, and the boiling range is 115-125 ℃ under 19995 Pa. The product has special odor of camphor, pungent and cool taste, is colorless or yellowish clear oily liquid, has the density (25 ℃) of 0.870-0.880, the refractive index (25 ℃) of 1.4663 and the optical rotation (25 ℃) of + 16-19 degrees. The main components of the medicine are pinene and camphene 20-30%, eucalyptol 30%, dipentene 30-40%, linalool 2-5%, and camphor content less than 2.5%. White oil can replace turpentine oil as paint thinner, deodorant, pesticide and mineral dressing flotation agent. Can be used for extracting eucalyptol, and is used in pharmaceutical industry. Pinene and dipentene may be used in synthesizing camphor, borneol, terpene resin, etc. In addition, the white camphor oil has the efficacy of relieving itching and pain, and is suitable for symptoms such as neuralgia and skin pruritus.
Disclosure of Invention
The invention aims to provide a white camphor oil extraction process, which improves the distillation efficiency and the yield by adopting a negative pressure distillation and ultrasonic auxiliary mode.
In order to achieve the purpose, the invention adopts the following technical scheme: a white camphor oil extraction process is characterized by comprising the following steps:
(1) selecting raw materials: selecting old camphor trunks or roots or camphor tree branches and leaves;
(2) and (3) distillation: distilling with a stainless steel distilling pan, wherein a wooden steaming barrel is arranged in the stainless steel distilling pan, and the wooden steaming barrel is in the same diameter with the stainless steel distilling pan and sleeved on the stainless steel distilling pan; when in processing, the branches and leaves of camphor trees or camphor wood slices are put into a wooden steaming barrel, the water in a stainless steel distilling pot is separated from the raw materials by 10 cm, the stainless steel distilling pot is closed immediately after the materials are put into the barrel and is connected with a coil condenser, the water level in the pot is kept during distilling to prevent the materials from being dried or burnt, and the water after oil-water separation is used as return water and is returned to the stainless steel distilling pot for use;
(3) cooling and separating steam with camphor and camphor oil, entering a coil condenser through an air duct, condensing the camphor and the oil to float on the water surface, separating the water to be transparent when separating, and separating the oil again if the water is not transparent, so as to improve the oil yield, filtering the camphor and the camphor oil floating on the water surface by using gauze to obtain crude camphor, wherein the remaining camphor oil contains most of camphor, so that the camphor oil is called as camphor oil;
(4) re-steaming and purifying: when camphor oil is used for extracting camphor, the camphor oil is put into a stainless steel distillation pot for secondary distillation, distillate at the temperature of 155 ℃ and 200 ℃ is collected to be called white oil, the white oil is cooled to separate out crystallized camphor, then the white oil is filtered, the filtrate is repeatedly distilled for several times until no camphor is separated out, and the rest is the white camphor oil.
Preferably, the stainless steel distillation pot during re-steaming and purifying adopts a negative pressure distillation pot, the negative pressure distillation pot is connected with an air inlet of a negative pressure fan, and an air outlet of the negative pressure fan is connected with a coil condenser.
More preferably, the pressure of the negative pressure distillation pot is-0.05 to-0.01 MPa
Preferably, old camphor trees with the length of more than 20 years are felled, the trunk and the root of the camphor trees are split into camphor wood slices, and then the camphor wood slices contain 2 to 4 percent of camphor and camphor oil.
Preferably, the camphor tree branches and leaves are picked in autumn, and then the camphor tree branches and leaves are cut into sections and pressed into camphor tree branch and leaf cakes through a press.
Further preferably, the wooden steaming barrel and the negative pressure distillation pot are provided with ultrasonic wave generating devices, and the ultrasonic power is maintained at 50KHz during distillation.
The invention has the advantages that: the distillation efficiency is improved by adopting a negative pressure distillation mode, the distillation temperature of the white camphor wood oil is reduced, the efficiency is improved by combining the ultrasonic effect, and the yield is improved.
Detailed Description
The present invention will be explained in further detail below with reference to examples for the purpose of facilitating understanding.
Example 1
(1) Selecting raw materials: picking branches and leaves of camphor trees in autumn, wherein the branches and leaves of camphor trees contain 1% -3% of camphor and camphor oil. The larger the age of the tree is, the more camphor is contained in the big pieces with bitter taste, the more camphor oil is contained in the big pieces with spicy taste, and then the branches and leaves of the camphor trees are cut into sections and pressed into camphor tree branch and leaf cakes through a press.
(2) And (3) distillation: distilling with a stainless steel distilling pan, wherein a wooden steaming barrel is arranged in the stainless steel distilling pan, and the wooden steaming barrel is in the same diameter with the stainless steel distilling pan and sleeved on the stainless steel distilling pan; when in processing, the camphor tree branch leaf cakes are put into a wooden steaming barrel, the water in a stainless steel distillation pot is separated from the raw materials by 10 cm, the stainless steel distillation pot is closed immediately after the materials are put into the barrel and is connected with a coil condenser, the water level in the pot is kept during distillation to prevent the stainless steel distillation pot from being dried or scorched, and the water after oil-water separation is used as return water and is returned to the stainless steel distillation pot for use.
(3) Cooling and separating steam with camphor and camphor oil, entering a coil condenser through an air duct, condensing the camphor and the oil to float on the water surface, separating the water to be transparent when separating, and separating the camphor and the camphor oil floating on the water surface again if the water is not transparent to improve the oil yield.
(4) Re-steaming and purifying: when camphor oil is used for extracting camphor, the camphor oil is put into a negative pressure distillation pot, the negative pressure distillation pot is connected with an air inlet of a negative pressure fan, an air outlet of the negative pressure fan is connected with a coil condenser for secondary distillation, distillate at the temperature of 155 plus of 200 ℃ is collected to be called white oil, the white oil is cooled to separate out crystallized camphor, then the white oil is filtered, the filtrate is repeatedly distilled for several times until no camphor is separated out, and the rest is the white camphor oil.
Example 2
(1) Selecting raw materials: the old camphor trees which are over 20 years old are felled, the trunk and the root parts of the camphor trees are split into camphor wood slices, and then the camphor wood slices contain 2 to 4 percent of camphor and camphor oil.
(2) And (3) distillation: distilling with a stainless steel distilling pan, wherein a wooden steaming barrel is arranged in the stainless steel distilling pan, and the wooden steaming barrel is in the same diameter with the stainless steel distilling pan and sleeved on the stainless steel distilling pan; when in processing, camphor tree leaves or camphor wood slices are put into a wooden steaming barrel, water in a stainless steel distillation pot is separated from raw materials by 10 cm, the stainless steel distillation pot is closed immediately after the materials are put into the barrel, the stainless steel distillation pot is connected with a coil condenser, the water level in the pot is kept during distillation to prevent the stainless steel distillation pot from being burnt out or burnt, and water after oil-water separation is used as return water and is returned to the stainless steel distillation pot for use.
(3) Cooling and separating steam with camphor and camphor oil, entering a coil condenser through an air duct, condensing the camphor and the oil to float on the water surface, separating the water to be transparent when separating, and separating the camphor and the camphor oil floating on the water surface again if the water is not transparent to improve the oil yield.
(4) Re-steaming and purifying: when camphor oil is used for extracting camphor, the camphor oil is put into a negative pressure distillation pot, the negative pressure distillation pot is connected with an air inlet of a negative pressure fan, an air outlet of the negative pressure fan is connected with a coil condenser for secondary distillation, the pressure of the negative pressure distillation pot is maintained at-0.05 MPa, distillate at 155 ℃ and 200 ℃ is collected and called white oil, crystallized camphor is separated out after the white oil is cooled, then the filtrate is filtered and distilled repeatedly for several times until no camphor is separated out, and the rest is the white camphor oil.
Example 3
(1) Selecting raw materials: picking branches and leaves of camphor trees in autumn, wherein the branches and leaves of camphor trees contain 1% -3% of camphor and camphor oil. The larger the age of the tree is, the more camphor is contained in the big pieces with bitter taste, the more camphor oil is contained in the big pieces with spicy taste, and then the branches and leaves of the camphor trees are cut into sections and pressed into camphor tree branch and leaf cakes through a press.
(2) And (3) distillation: distilling with a stainless steel distilling pan, wherein a wooden steaming barrel is arranged in the stainless steel distilling pan, and the wooden steaming barrel is in the same diameter with the stainless steel distilling pan and sleeved on the stainless steel distilling pan; when in processing, camphor tree leaves or camphor wood slices are put into a wooden steaming barrel, water in a stainless steel distillation pot is separated from raw materials by 10 cm, the stainless steel distillation pot is closed immediately after the materials are put into the barrel, the stainless steel distillation pot is connected with a coil condenser, the water level in the pot is kept during distillation to prevent the stainless steel distillation pot from being burnt out or burnt, and water after oil-water separation is used as return water and is returned to the stainless steel distillation pot for use.
(3) Cooling and separating steam with camphor and camphor oil, entering a coil condenser through an air duct, condensing the camphor and the oil to float on the water surface, separating the water to be transparent when separating, and separating the camphor and the camphor oil floating on the water surface again if the water is not transparent to improve the oil yield.
(4) Re-steaming and purifying: when camphor oil is used for extracting camphor, the camphor oil is put into a negative pressure distillation pot, the negative pressure distillation pot is connected with an air inlet of a negative pressure fan, an air outlet of the negative pressure fan is connected with a coil condenser for secondary distillation, the pressure of the negative pressure distillation pot is maintained at-0.01 MPa, distillate at 155 ℃ and 200 ℃ is collected and called white oil, crystallized camphor is separated out after the white oil is cooled, then the filtrate is filtered and distilled repeatedly for several times until no camphor is separated out, and the rest is the white camphor oil.
Example 4
(1) Selecting raw materials: picking branches and leaves of camphor trees in autumn, wherein the branches and leaves of camphor trees contain 1% -3% of camphor and camphor oil. The larger the age of the tree is, the more camphor is contained in the big pieces with bitter taste, the more camphor oil is contained in the big pieces with spicy taste, and then the branches and leaves of the camphor trees are cut into sections and pressed into camphor tree branch and leaf cakes through a press.
(2) And (3) distillation: distilling by using a stainless steel distilling pot, wherein a wooden steaming barrel is arranged in the stainless steel distilling pot, the opening diameters of the wooden steaming barrel and the stainless steel distilling pot are consistent, the wooden steaming barrel is sleeved on the stainless steel distilling pot, and an ultrasonic generating device is arranged in the wooden steaming barrel; when in processing, camphor tree leaves or camphor wood slices are put into a wooden steaming barrel, water in a stainless steel distillation pot is separated from raw materials by 10 cm, the stainless steel distillation pot is immediately sealed after the materials are fed, an ultrasonic wave generating device is started, the ultrasonic power is 50KHz, the stainless steel distillation pot is connected with a coil pipe condenser, the water level in the pot is kept during distillation to prevent the distillation from being dried or burnt, and the water after oil-water separation is used as return water to be returned into the stainless steel distillation pot for use.
(3) Cooling and separating steam with camphor and camphor oil, entering a coil condenser through an air duct, condensing the camphor and the oil to float on the water surface, separating the water to be transparent when separating, and separating the camphor and the camphor oil floating on the water surface again if the water is not transparent to improve the oil yield.
(4) Re-steaming and purifying: when camphor oil is used for extracting camphor, the camphor oil is put into a negative pressure distillation pot, an ultrasonic wave generating device is installed in the negative pressure distillation pot, the negative pressure distillation pot is connected with an air inlet of a negative pressure fan, an air outlet of the negative pressure fan is connected with a coil condenser for secondary distillation, the pressure of the negative pressure distillation pot is maintained at-0.01 MPa, distillate of 145-plus-180 ℃ is collected and called white oil, crystallized camphor is separated out after the white oil is cooled, then the filtrate is filtered and distilled for several times repeatedly until no camphor is separated out, and the rest is the white camphor oil.

Claims (6)

1. A white camphor oil extraction process is characterized by comprising the following steps:
(1) selecting raw materials: selecting old camphor trunks or roots or camphor tree branches and leaves;
(2) and (3) distillation: distilling with a stainless steel distilling pan, wherein a wooden steaming barrel is arranged in the stainless steel distilling pan, and the wooden steaming barrel is in the same diameter with the stainless steel distilling pan and sleeved on the stainless steel distilling pan; when in processing, the branches and leaves of camphor trees or camphor wood slices are put into a wooden steaming barrel, the water in a stainless steel distilling pot is separated from the raw materials by 10 cm, the stainless steel distilling pot is closed immediately after the materials are put into the barrel and is connected with a coil condenser, the water level in the pot is kept during distilling to prevent the materials from being dried or burnt, and the water after oil-water separation is used as return water and is returned to the stainless steel distilling pot for use;
(3) cooling and separating steam with camphor and camphor oil, entering a coil condenser through an air duct, condensing the camphor and the oil to float on the water surface, separating the water to be transparent when separating, and separating the oil again if the water is not transparent, so as to improve the oil yield, filtering the camphor and the camphor oil floating on the water surface by using gauze to obtain crude camphor, wherein the remaining camphor oil contains most of camphor, so that the camphor oil is called as camphor oil;
(4) re-steaming and purifying: when camphor oil is used for extracting camphor, the camphor oil is put into a stainless steel distillation pot for secondary distillation, distillate at the temperature of 155 ℃ and 200 ℃ is collected to be called white oil, the white oil is cooled to separate out crystallized camphor, then the white oil is filtered, the filtrate is repeatedly distilled for several times until no camphor is separated out, and the rest is the white camphor oil.
2. The white camphor oil extraction process of claim 1, which is characterized by comprising the following steps: the stainless steel distillation pot during re-steaming and purification adopts a negative pressure distillation pot, the negative pressure distillation pot is connected with an air inlet of a negative pressure fan, and an air outlet of the negative pressure fan is connected with a coil condenser.
3. The white camphor oil extraction process of claim 2, which is characterized by comprising the following steps: the pressure of the negative pressure distillation pot is-0.05 to-0.01 MPa.
4. The white camphor oil extraction process of claim 1, which is characterized by comprising the following steps: the old camphor trees which are over 20 years old are felled, the trunk and the root parts of the camphor trees are split into camphor wood slices, and then the camphor wood slices contain 2 to 4 percent of camphor and camphor oil.
5. The white camphor oil extraction process of claim 1, which is characterized by comprising the following steps: picking branches and leaves of camphor trees in autumn, cutting the branches and leaves of the camphor trees into sections, and pressing the sections into camphor tree branch and leaf cakes through a press.
6. The white camphor oil extraction process of claim 1, which is characterized by comprising the following steps: the wooden steaming barrel and the negative pressure distillation pot are provided with ultrasonic wave generating devices, and the ultrasonic power is maintained at 50KHz during distillation.
CN201911160072.1A 2019-11-23 2019-11-23 White camphor oil extraction process Pending CN110923068A (en)

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Application Number Priority Date Filing Date Title
CN201911160072.1A CN110923068A (en) 2019-11-23 2019-11-23 White camphor oil extraction process

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114307240A (en) * 2021-12-31 2022-04-12 云南森美达生物科技股份有限公司 Extraction and preparation method of natural camphor
CN116497619A (en) * 2023-05-17 2023-07-28 岳阳林纸股份有限公司 A kind of natural color chemical mechanical pulping process of camphor wood sodium hydroxide

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114307240A (en) * 2021-12-31 2022-04-12 云南森美达生物科技股份有限公司 Extraction and preparation method of natural camphor
CN116497619A (en) * 2023-05-17 2023-07-28 岳阳林纸股份有限公司 A kind of natural color chemical mechanical pulping process of camphor wood sodium hydroxide

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