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CN111635828A - Rose essential oil extraction method - Google Patents

Rose essential oil extraction method Download PDF

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Publication number
CN111635828A
CN111635828A CN202010537895.8A CN202010537895A CN111635828A CN 111635828 A CN111635828 A CN 111635828A CN 202010537895 A CN202010537895 A CN 202010537895A CN 111635828 A CN111635828 A CN 111635828A
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China
Prior art keywords
oil
rose
essential oil
water
distillation
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Pending
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CN202010537895.8A
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Chinese (zh)
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王瑞雪
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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
    • C11B9/022Refining
    • 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
    • C11B9/025Recovery by solvent extraction
    • 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)

Abstract

A method for extracting rose essential oil comprises the following steps: (1) adding rose raw materials and a distilled solvent into a distillation container to form mixed liquid; (2) heating and distilling the mixed liquid, and evaporating the mixed liquid consisting of the rose essential oil and the water to form oil-gas mixed steam; (3) the oil-gas mixed steam passes through a condenser to form an oil-water mixture; (4) collecting the oil-water mixture into an oil-water separator; (5) separating the oil-water mixture by an oil-water separator to obtain essential oil and distilled water; (6) and adding the distilled water into a distillation container to be used as a distillation solvent of the subsequent rose raw material. The rose essential oil extraction method provided by the invention is simple in steps, and can increase the oil yield of rose essential oil.

Description

Rose essential oil extraction method
Technical Field
The invention relates to a distillation extraction method with classification number B01D3/00, in particular to a distillation extraction method of rose essential oil.
The rose essential oil is the essential oil extracted from fresh roses, has the international market price equivalent to gold, is known as 'liquid gold', and is the most common famous and precious floral raw material. The rose essential oil is the crown of fresh flower oil, has elegant, soft, fine and sweet fragrance like the fragrance of a honey and fragrant rose, has strong fragrance, and is the most important and most common famous and precious flower fragrance raw material in the fragrance blending. The rose essential oil is a high-quality spice, can be mixed with various flower fragrance essences, has the effects of maintaining beauty and keeping young and protecting skin, and belongs to fine products and treasure products in cosmetics. The production of edible essence by using rose essential oil for blending fragrance is becoming one of the important technological means in the fine chemical industry.
The existing extraction method of rose essential oil mainly adopts a steam distillation method, and is widely used due to simple operation and low cost. The steam distillation method adopts the working principle and the operation steps that picked raw materials and water are added into a distillation kettle according to a certain proportion to form mixed liquid, and then the mixed liquid is heated. According to the law of dalton partial pressure, the total pressure in the mixture is equal to the sum of the vapor pressures of the components, and the components can be distilled out when the total pressure is lower than the respective boiling points, so that the mixed liquid of the rose essential oil and the water can be evaporated into the vapor of the mixture. Then an oil-water mixture is prepared by condensation, and essential oil and water of the oil-water mixture are separated by an oil-water separator, so that the rose essential oil can be obtained.
The rose essential oil content is low, how to adopt a reasonable process flow and obtain higher oil yield is always a problem to be solved urgently in industrial production. In order to increase the oil yield, the method of redistilling the distillate water separated by the oil-water separator is called redistillation of the distillate water. The re-distillation can recover the essential oil contained in the water and improve the oil yield, but the re-distillation needs to increase the distillation process, so the process is complicated.
Disclosure of Invention
The invention provides a method for increasing the oil yield of rose essential oil and saving the process.
The technical scheme for realizing the technical effects provided by the invention provides a rose essential oil extraction method, which comprises the following steps: (1) adding rose raw materials and a distilled solvent into a distillation container to form mixed liquid; (2) heating and distilling the mixed liquid, and evaporating the mixed liquid consisting of the rose essential oil and the water to form oil-gas mixed steam; (3) the oil-gas mixed steam passes through a condenser to form an oil-water mixture; (4) collecting the oil-water mixture into an oil-water separator; (5) separating the oil-water mixture by an oil-water separator to obtain essential oil and distilled water; (6) the distilled water is not re-distilled and is added into a distillation container to be used as a subsequent distillation solvent of the rose raw material.
Further, in the step (1), the distilled solvent comprises distilled water generated in the previous rose essential oil extraction process.
Further, the distilled solvent in the step (1) comprises 3-5% of NaCl by mass fraction.
Further, the ratio of the materials to the liquid in the step (1) is 1: 3-5.
As another aspect of the present invention, there is provided a method for extracting rose essential oil, comprising the steps of: (1) adding rose raw materials and a distilled solvent into a distillation container to form mixed liquid; (2) opening a switch valve of the negative pressure collecting part, heating and distilling the mixed liquid, and evaporating the mixed liquid consisting of the rose essential oil and the water to form oil-gas mixed steam; (3) the oil-gas mixed steam passes through a condenser to form an oil-water mixture; (4) the negative pressure collecting part divides and collects the steam passing through the condenser through a dividing pipeline; (5) the oil-water mixture flows into the oil-water separator through the connecting pipeline; (6) closing the switch valve of the negative pressure collecting part after the rose essence begins to be extracted for half an hour; (7) stopping heating of the distillation vessel after the distillation time is reached; performing oil-water separation by an oil-water separator to obtain rose essential oil and distilled water in the oil-water separator; (8) further refining the solution in the collection container to obtain shunted rose essential oil; (9) mixing the rose essential oil obtained by the oil-water separator with the shunt rose essential oil to obtain a finished product; (10) the distilled water is not re-distilled and is added into a distillation container to be used as a subsequent distillation solvent of the rose raw material.
Further, in the step (8), the purification is further performed by distillation under reduced pressure.
Further, in the step (1), the distilled solvent comprises distilled water generated in the previous rose essential oil extraction process.
Further, the distillation time in the step (7) is 2.5-3.5 h.
Drawings
FIG. 1 is a flow chart of the prior art process for extracting rose essential oil by steam distillation.
FIG. 2 is a flow chart of extracting rose essential oil according to the embodiment of the present invention.
Fig. 3 is a schematic view showing the composition of a rose essence extraction system of the rose essential oil extraction method according to the preferred embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
FIG. 1 is a flow chart of a rose essential oil extraction method in the prior art, wherein roses are condensed into an oil-water mixture after steam distillation, the oil-water mixture is subjected to oil-water separation to form rose essential oil and distilled water, and the distilled water is subjected to redistillation to extract the rose essential oil.
FIG. 2 is a flow chart of the method for extracting rose essential oil according to the embodiment of the present invention, which comprises the following steps: (1) adding rose raw materials and a distilled solvent into a distillation container to form mixed liquid; wherein the distilled solvent comprises distilled water produced in the previous rose essential oil extraction process; in order to improve the oil yield, the distillation solvent in the distillation container can be set to comprise 3-5% of NaCl by mass; the ratio of the materials to the liquid can be set to be 1: 3-5; (2) heating and distilling the mixed liquid, and evaporating the mixed liquid consisting of the rose essential oil and the water to form oil-gas mixed steam; (3) the oil-gas mixed steam passes through a condenser to form an oil-water mixture; (4) collecting the oil-water mixture into an oil-water separator; (5) separating the oil-water mixture by an oil-water separator to obtain essential oil and distilled water; (6) the distilled water is not re-distilled and is added into a distillation container to be used as a subsequent distillation solvent of the rose raw material.
By the method, the distilled water is used as a subsequent distillation solvent without being re-distilled, so that the rose essential oil in the distilled water can be further distilled, the re-distillation procedure is reduced, and water resources used in the extraction process of the rose essential oil are saved.
Fig. 3 shows a rose essential oil extraction system of a preferred embodiment of the present invention, comprising: a distillation container 1 for putting rose raw material therein for distillation; the condenser 2 is communicated with a steam outlet of the distillation container and is used for condensing the oil-gas mixed steam; the oil-water separator 4 is connected with the outlet of the condenser 2 through a connecting pipeline 3 and is used for receiving an oil-water mixture; the negative pressure collecting part is arranged between the condenser 2 and the oil-water separator 4 and is connected with the connecting pipeline 3 through a shunt pipeline 5; preferably, the diversion pipeline 5 and the connecting pipeline 3 are arranged to form an upward included angle of about 45 degrees, so that the condensed oil-water mixture flows into the oil-water separator through the connecting pipeline 3 due to the action of gravity and cannot enter the diversion pipeline 5, and uncondensed gas in the connecting pipeline 3 is pumped to the diversion pipeline 5 by negative pressure; the negative pressure collecting part comprises a switch valve 6, a negative pressure pump 7 and a collecting container 8; the switch valve 6 can open or close the shunt pipeline 5 occasionally, is opened in the first half hour when the rose essential oil begins to be extracted, and is closed after the rose essence begins to be extracted for half hour; the negative pressure pump 7 can provide negative pressure for extracting the gas from the connecting pipeline 3; the collection container 8 is provided with an organic solvent, the input pipe orifice of which is positioned below the liquid level of the organic solvent, and the organic solvent is ethanol or petroleum ether.
The rose essential oil extraction method of the preferred embodiment of the invention comprises the following steps: (1) adding rose raw materials and a distilled solvent into a distillation container 1 to form mixed liquid; wherein the distilled solvent comprises distilled water produced in the previous rose essential oil extraction process; in order to improve the oil yield, the distillation solvent in the distillation container 1 can be set to comprise 3-5% of NaCl by mass; the ratio of the materials to the liquid can be set to be 1: 3-5; (2) opening a switch valve 6 of the negative pressure collecting part, heating and distilling the mixed liquid, and evaporating the mixed liquid consisting of the rose essential oil and the water to form oil-gas mixed steam; (3) the oil-gas mixed steam passes through the condenser 2 to form an oil-water mixture; (4) the negative pressure collecting part divides and collects the steam passing through the condenser 2 through a dividing pipeline 5; (5) the oil-water mixture flows into an oil-water separator 4 through a connecting pipeline 3; (6) closing the switch valve 6 of the negative pressure collecting part after the rose essential oil begins to be extracted for half an hour; (7) after the distillation time has been reached, the heating of the distillation vessel 1 is stopped; performing oil-water separation by an oil-water separator 4 to obtain rose essential oil and distilled water in the oil-water separator 4; (8) further refining the solution in the collection container 8 to obtain split-flow rose essential oil; (9) mixing the rose essential oil obtained by the separation of the oil-water separator 4 with the shunt rose essential oil to obtain a finished product; (10) the distilled water was not re-distilled, but was added to the distillation vessel 1 as a solvent for the subsequent distillation of the rose raw material.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. The particular features, structures, materials, or characteristics described in this disclosure may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.

Claims (8)

1. A method for extracting rose essential oil comprises the following steps: (1) adding rose raw materials and a distilled solvent into a distillation container to form mixed liquid; (2) heating and distilling the mixed liquid, and evaporating the mixed liquid consisting of the rose essential oil and the water to form oil-gas mixed steam; (3) the oil-gas mixed steam passes through a condenser to form an oil-water mixture; (4) collecting the oil-water mixture into an oil-water separator; (5) separating the oil-water mixture by an oil-water separator to obtain essential oil and distilled water; the method is characterized by further comprising the step (6): adding distilled water into a distillation container to be used as a distillation solvent of the subsequent rose raw material.
2. The method for extracting rose essential oil according to claim 1, characterized in that: in the step (6), the distilled water is not re-distilled.
3. The method for extracting rose essential oil according to claim 1, characterized in that: the distillation solvent in the step (1) comprises NaCl with the mass fraction of 3% -5%.
4. The method for extracting rose essential oil according to claim 1, characterized in that: the distillation solvent in the step (1) comprises NaCl with the mass fraction of 4%.
5. The rose essence extraction method according to claim 1, characterized in that: the material-liquid ratio in the step (1) is 1: 3-5.
6. The rose essence extraction method according to claim 1, characterized in that: the material-liquid ratio in the step (1) is 1: 4.
7. The rose essence extraction method according to claim 1, characterized in that: the distillation time in the step (2) is 2.5-3.5 h.
8. The rose essence extraction method according to claim 1, characterized in that: the distillation time in the step (2) is 3 h.
CN202010537895.8A 2020-06-13 2020-06-13 Rose essential oil extraction method Pending CN111635828A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112280620A (en) * 2020-10-28 2021-01-29 宁波捷通机械有限公司 A kind of aromatic plant extract distillation concentration processing method
CN117866708A (en) * 2023-12-29 2024-04-12 南寅科技(云南)有限公司 Preparation method of rose absolute
CN118006392A (en) * 2024-02-28 2024-05-10 新疆农业大学 A method for extracting rose essential oil by ultrasonic-assisted steam distillation

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101280243A (en) * 2008-06-04 2008-10-08 杨利民 Method for extracting rose essence oil and rose absolute by water vapor water distillation technology
CN104818122A (en) * 2015-05-22 2015-08-05 西昌昌泰香料有限责任公司 Preparation technique of rose essential oil
CN105779133A (en) * 2016-05-26 2016-07-20 陕西恒芳玫瑰开发有限公司 Stage extraction method for rose essential oil
CN105820879A (en) * 2015-01-05 2016-08-03 达金兰 Preparation method of rose essential oil
CN105969528A (en) * 2016-06-14 2016-09-28 云南金大康农业科技有限公司 Extracting method for rose essential oil

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101280243A (en) * 2008-06-04 2008-10-08 杨利民 Method for extracting rose essence oil and rose absolute by water vapor water distillation technology
CN105820879A (en) * 2015-01-05 2016-08-03 达金兰 Preparation method of rose essential oil
CN104818122A (en) * 2015-05-22 2015-08-05 西昌昌泰香料有限责任公司 Preparation technique of rose essential oil
CN105779133A (en) * 2016-05-26 2016-07-20 陕西恒芳玫瑰开发有限公司 Stage extraction method for rose essential oil
CN105969528A (en) * 2016-06-14 2016-09-28 云南金大康农业科技有限公司 Extracting method for rose essential oil

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112280620A (en) * 2020-10-28 2021-01-29 宁波捷通机械有限公司 A kind of aromatic plant extract distillation concentration processing method
CN117866708A (en) * 2023-12-29 2024-04-12 南寅科技(云南)有限公司 Preparation method of rose absolute
CN118006392A (en) * 2024-02-28 2024-05-10 新疆农业大学 A method for extracting rose essential oil by ultrasonic-assisted steam distillation

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Application publication date: 20200908