CN113969212A - Natural aromatic plant multi-element extraction tank and use method thereof - Google Patents

Natural aromatic plant multi-element extraction tank and use method thereof Download PDF

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Publication number
CN113969212A
CN113969212A CN202010715974.3A CN202010715974A CN113969212A CN 113969212 A CN113969212 A CN 113969212A CN 202010715974 A CN202010715974 A CN 202010715974A CN 113969212 A CN113969212 A CN 113969212A
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CN
China
Prior art keywords
extraction
tank
steam
solvent
extraction tank
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Pending
Application number
CN202010715974.3A
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Chinese (zh)
Inventor
康维君
庄伟强
茅富燕
刘伟
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Shanghai Aipu Plant Technology Co ltd
Aipu Spice Group Co ltd
Original Assignee
Shanghai Aipu Plant Technology Co ltd
Aipu Spice Group Co ltd
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Application filed by Shanghai Aipu Plant Technology Co ltd, Aipu Spice Group Co ltd filed Critical Shanghai Aipu Plant Technology Co ltd
Priority to CN202010715974.3A priority Critical patent/CN113969212A/en
Publication of CN113969212A publication Critical patent/CN113969212A/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
    • C11B9/025Recovery by solvent extraction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0207Control systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0288Applications, solvents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D2011/007Extraction using a solvent in the gas phase

Abstract

A natural aromatic plant multi-solvent extraction tank and a using method thereof. The extraction tank is internally provided with a screw conveyor, the extraction tank is provided with a feed inlet, a discharge outlet and a multi-component solvent air inlet, a plurality of gas evaporators connected with the solvent tank are respectively connected with the multi-component solvent air inlet through a gas flow valve and a steam inlet pipe, and the other end of the extraction tank is provided with an air outlet connected with a spice storage tank through an air outlet valve, a condenser and a condenser. Putting natural aromatic plants into an extraction tank, and simultaneously making various extraction solvent steam with different polarities enter the extraction tank to fully contact with the natural aromatic plants until the extraction steam carrying extracted natural aromatic plant aroma components enters a condenser and an aroma collection tank after extraction is finished. The invention can improve the output of natural perfume extracts and is suitable for large-scale extraction of natural aromatic plants. Meanwhile, a plurality of extraction solvents with different polarities are introduced into the extraction tank, so that the extraction efficiency is improved, and the thermal decomposition and loss of aroma substances of different types are avoided.

Description

Natural aromatic plant multi-element extraction tank and use method thereof
Technical Field
The invention relates to natural spice extraction equipment, in particular to a natural aromatic plant multi-element extraction tank and a using method thereof.
Background
The chemical components of plant constituents can be divided into three major classes, the first class of high volatile substances with molecular weight below 200, for example: alcohols, ketones, aldehydes, esters, sulfur-containing compounds, and the like; a second group of components having a molecular weight of 200 to 400, for example: sesquiterpenes, diterpenes, triterpenes, various oxygen-containing derivatives thereof, amino acids, and the like; the third class is macromolecular compounds with molecular weights above 400, such as: tannins, peptides, polysaccharides, starch, and the like. The preparation of natural perfume by extracting the aroma components from natural aromatic plants is a long-standing, old and effective method, which is spread to the present for hundreds of years.
The plant perfume extracting method includes steam distillation, solvent extraction, supercritical fluid extraction, etc. The steam distillation method is the most commonly used method, and comprises various forms of water distillation, direct steam distillation, rotary cone stripping distillation and the like, and is suitable for extracting some natural perfumes with low aroma component boiling points, and the high-quality plant essential oil is extracted by using the steam distillation at present. The solvent extraction method is suitable for natural perfume with fragrance components which are easy to change by heating or with a part of fragrance components dissolved in water. Supercritical fluid extraction, which uses supercritical fluid, most commonly supercritical carbon dioxide, to extract various flavors and pigments from natural plant materials has become a common technique in the food industry.
These single solvent extraction systems are well developed technologies, but most of them cannot simultaneously satisfy the requirements of large extraction capacity and low solubility of the extractant in the extracted medium in the extraction process. The multi-element extraction system has attracted attention because of its advantages of high selectivity, good separation effect, high extraction efficiency, high mass transfer rate, etc. besides the characteristics of single solvent extraction system. At present, the research of multi-element extraction system relates to a plurality of fields of petrochemical industry, biochemical industry, pharmaceutical industry and the like, and the research is developed from a binary extractant system to a ternary and quaternary extractant system.
The traditional single solvent extraction method of natural aromatic plants has the defects of low moisture content, strong aroma or high boiling point of aroma components. The traditional production mode can not meet the market demand. Therefore, it is desirable to design a device and a method for rapidly producing natural perfume in large quantities by introducing a multi-solvent extraction system on the basis of ensuring the extraction quality of natural perfume plants.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the multi-element extraction tank capable of continuously extracting the natural perfume and the using method thereof, which can improve the output of the extracted product of the natural perfume and are suitable for quickly and massively extracting the natural essential oil.
In order to achieve the purpose, the invention provides a natural aromatic plant multi-component solvent extraction tank, which comprises an extraction tank, a gas inlet and a gas outlet of multi-component solvent steam, wherein a spiral conveyor fixed on a central shaft is arranged in the extraction tank, the central shaft is connected with a motor, and a feed inlet and a discharge outlet are arranged at two opposite ends of the extraction tank.
And a gas inlet valve is also arranged between the steam inlet pipe and the multi-component solvent steam inlet.
One end of the condenser is provided with a gas outlet to discharge the extraction solvent such as carbon dioxide which is still gaseous after being condensed. The other end of the condenser is connected with the spice storage tank.
The extraction tank is a sealed tank body provided with a heat-insulating layer.
The invention also provides a use method of the natural aromatic plant multi-solvent extraction tank, which comprises the following steps:
(1) filling natural aromatic plants into a sealed extraction tank provided with a heat-insulating layer through a feed inlet, conveying the natural aromatic plants into the extraction tank through a screw conveyor in the extraction tank, opening a gas inlet valve, closing a gas outlet valve, allowing a plurality of extraction solvents to form steam through a gas evaporator respectively, adjusting the flow through a flow valve, allowing the steam to enter a steam inlet pipe to allow the steam to enter the extraction tank from a gas inlet of multi-element solvent steam on one side of the sealed extraction tank and form pressure, and extracting the natural aromatic plants through the steam of the plurality of extraction solvents;
(2) the natural aromatic plant enters an extraction tank through a screw conveyor and fully contacts with steam of a plurality of extraction solvents in the extraction tank to generate natural aromatic plant aroma components;
(3) after extraction is finished, opening an air outlet valve, and allowing the steam carrying extracted natural aromatic plant aroma components to enter a condenser from an air outlet of the extraction tank and leave the extraction tank;
(4) collecting the cooled liquid to obtain natural perfume extract.
Furthermore, the gas valve controls the extraction pressure in the tank to be 100 kPa-250 kPa.
Furthermore, the gas flow valve respectively controls the solvent steam flow to be 5L/Min-300L/Min, and the dosage of the natural aromatic plants filled into the feed inlet of the extraction tank is between 100g and 100 kg.
Further, the extraction time of the natural aromatic plants is 60-360 minutes.
Furthermore, the extraction solvents with different polarities are extracted from the natural aromatic plants by steam generated by a gas evaporator, and the extraction solvents include water, ethanol, acetone, ethyl acetate and carbon dioxide.
The extraction tank temperature, pressure and extraction solvent vapor volume ratio can be set according to the desired process conditions.
The invention has the advantages that:
1. the multi-element extraction tank for continuously extracting the natural perfume and the use method thereof have the advantages of low cost, convenient cleaning and continuous and mass production;
2. the plurality of gas evaporators connected with the extraction tank can respectively adjust the steam of various solvents through the gas flow valve and then enter the extraction tank, and can respectively and simultaneously introduce various extraction solvents with different polarities into the extraction tank, so that the extraction efficiency is improved.
3. By controlling the type of the extraction solvent steam introduced into the extraction tank and matching with proper extraction temperature and pressure control, the thermal decomposition and loss of aroma substances of different types can be avoided, and the natural perfume can be extracted quickly.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 chromatogram of example one;
FIG. 3 chromatogram of example two.
In the figure: the device comprises a storage tank 1, an extraction tank 2, a screw conveyor 3, a gas inlet of multi-component solvent vapor 4, a gas evaporator A5, a gas evaporator B6, a gas evaporator C7, a flow valve A8, a flow valve B9, a flow valve C10, a vapor inlet pipe 11, a gas inlet valve 12, a gas outlet valve 13, a spice storage tank 14, a condenser 15, a gas outlet 16, a gas outlet 17, a material inlet 18, a waste material outlet 19 and a waste material tank 20.
Detailed Description
Embodiments of the invention are further described below with reference to the accompanying drawings:
example one
Referring to fig. 1, in the multi-solvent extraction tank for natural aromatic plants of this embodiment, an extraction tank 2 is a sealed tank body provided with a heat insulation layer, the extraction tank 2 is connected to a storage tank 1, one end of the extraction tank 2 is provided with an air inlet 4 for multi-solvent steam, the other end of the extraction tank is provided with an air outlet 17, a screw conveyor 3 fixed on a central shaft is arranged in the extraction tank 2, the central shaft is connected to a motor (not shown in the figure) to drive the screw conveyor 3 fixed on the central shaft to rotate around the center to convey the natural aromatic plants, and a feed inlet 18 and a waste outlet 19 are arranged at two opposite ends of the extraction tank 2. Extract jar 2 one end and be equipped with the air inlet 4 of many first solvent steam on 19 upper portions of waste outlet, the gas evaporation ware that the several links to each other with the solvent jar links to each other through gas flow valve and steam intake pipe 11 respectively, and the embodiment is that three gas evaporation ware links to each other with three flow valve respectively to control each solvent steam's inflow flow respectively: the gas evaporator A5 is connected with a flow valve A8, the gas evaporator B6 is connected with a flow valve B9, and the gas evaporator C7 is connected with a flow valve C10. The three flow valves are connected with a steam inlet pipe 11 through pipelines, the steam inlet pipe 11 is connected with an air inlet 4 of multi-element solvent steam, and an air inlet valve 12 is further arranged between the steam inlet pipe 11 and the air inlet 4 of the multi-element solvent steam to control the total flow and/or pressure of the solvent steam. The other end of the extraction tank 2 is provided with an air outlet 17 at the lower part of the feed inlet 18, the air outlet 17 is connected with a condenser 15 through an air outlet valve 13, so that the extracted natural aromatic plant aroma components carried by the extracted steam leave the extraction tank 2 from the air outlet 17 of the extraction tank 2 and enter the condenser 15 for cooling, and the other end of the condenser 15 is connected with a spice storage tank 14 to collect the cooled liquid, namely the obtained natural spice extract. The condenser 15 is provided at its upper end with a gas discharge port 16.
The use method of the natural aromatic plant multi-solvent extraction tank of the embodiment comprises the following steps:
extracting the vanilla extract by using a multi-solvent extraction tank. See fig. 1.
(1) 10kg of crushed vanilla bean powder is stored in a storage tank 1 and is connected with an extraction tank 2 through a feed inlet 18 of the extraction tank 2, the vanilla bean powder is filled into the sealed extraction tank 2 provided with a heat-insulating layer through the feed inlet 18 and is sent into the extraction tank 2 through a screw conveyer 3 in the extraction tank 2, the temperature of the extraction tank 2 is firstly controlled to 100 ℃, a gas inlet valve 12 is opened, and a gas outlet valve 13 is closed. Several extraction solvents with different polarities are respectively vaporized by a gas evaporator, and the used extraction solvents include but are not limited to water, ethanol, acetone, ethyl acetate and carbon dioxide. In this example, three extraction solvents are respectively passed through a gas evaporator to form steam, and in this example, water and ethanol are used as extraction solvents, and carbon dioxide is introduced. Carbon dioxide is used as an extraction solvent and is also used for increasing the extraction pressure in the tank. After the flow is regulated by the three flow valves, water, ethanol vapor and carbon dioxide enter the vapor inlet pipe 11, so that the vapor enters the extraction tank 2 from the air inlet 4 on one side of the sealed extraction tank 2 and forms pressure. The gas flow valves respectively control the flow rate of the solvent steam to be 5L/Min-300L/Min. The water, ethanol and carbon dioxide in the embodiment are heated and vaporized in the steam generator A5, the steam generator B6 and the steam generator C7 before entering the extraction tank 2, and the flow rate of the water vapor is controlled to be 15L/min, the flow rate of the ethanol vapor is controlled to be 30L/min and the flow rate of the carbon dioxide is controlled to be 40L/min through the flow rate valve A8, the flow rate valve B9 and the flow rate valve C10. The feeding is continued until the required pressure in the tank is reached, and the gas inlet valve 12 is adjusted to control the extraction pressure in the tank to be 100 kPa-250 kPa. This example continues the steam feed until the pressure in the extraction tank 2 stabilizes at 150 kPa. The gas inlet valve 12 is closed. The feed rate was controlled at this time as follows: 1 kg/min. Extracting the vanilla bean powder by using the steam of the three extraction solvents;
(2) the extraction tank 2 is provided with a screw conveyor 3 rotating around the axis in the tank body, and the vanilla bean powder is driven by the blades of the screw conveyor 3 to move towards the other end. The vanilla bean powder enters an extraction tank 2 through a screw conveyor 3 and is fully contacted with extraction steam in the extraction tank 2, so that aroma components in the vanilla beans are separated and are fully contacted in the extraction tank 2, the extraction time of natural aromatic plants is 60-360 minutes, and the extraction time of the embodiment is 120 minutes;
(3) after extraction is finished, a gas outlet valve 13 is opened, and the extracted natural vanilla components carried by the extraction steam leave the extraction tank 2 from a gas outlet 17 of the extraction tank 2; and enters a condenser 15, and carbon dioxide is discharged through a gas outlet 16 after being separated;
(4) the cooled liquid, i.e. the condensed vanilla extract, is collected in the flavor reservoir 14. The chromatogram of the vanilla extract is shown in FIG. 2. The extracted vanilla waste passes from the waste outlet 19 into a canister 20.
Example two
The same as in the first embodiment, except that: extracting tea leaf extract with multi-element extraction tank. 20kg of the crushed tea leaves were stored in a storage tank 1. Similar to example one, water, ethanol and carbon dioxide were used as extraction solvents. The temperature of the extraction tank 2 is controlled to 110 ℃, the gas inlet valve 12 is opened, and the gas outlet valve 13 is closed. Before entering the extraction tank 2, water, ethanol and carbon dioxide are heated and vaporized in a steam generator A5, a steam generator B6 and a steam generator C7, the flow rate of the water is 20L/min, the flow rate of the ethanol steam is 20L/min and the flow rate of the carbon dioxide is 60L/min under the control of a flow valve A8, a flow valve B9 and a flow valve C10, the water, the ethanol and the carbon dioxide are continuously introduced until the pressure in the tank reaches 200kPa, and a gas inlet valve 12 is closed. The feed rate at the feed port 18 was controlled to be 1 kg/min. The tea powder is pushed by the blades of the screw conveyor 3 to move towards the other end, and the tea is fully contacted with the extraction steam in the extraction tank 2, and the extraction time is 240 minutes. And after extraction is finished, opening a gas outlet valve 13, enabling the extracted steam carrying tea volatile components to leave the extraction tank 2 from a gas outlet 17 and to be recycled into a condenser 15, discharging the separated carbon dioxide through a gas outlet 16, and enabling the condensed tea extract to enter a spice storage tank 14. The chromatogram of the tea extract is shown in FIG. 3. The extracted tea leaf waste enters the canister 20 from the waste outlet 19.

Claims (10)

1. The utility model provides a natural fragrant plant many first solvents extraction jar, including the extraction jar, many first solvent steam's air inlet and gas outlet, be equipped with the auger delivery ware of fixing on the center pin in the extraction jar, the center pin links to each other with the motor, the double-phase opposite end side of extraction jar is equipped with feed inlet and discharge gate, the one end of its characterized in that extraction jar is equipped with many first solvent steam's air inlet, the several links to each other through gas flow valve and steam intake pipe respectively with the gas evaporator that the solvent jar links to each other, this steam intake pipe links to each other with many first solvent steam's air inlet, the other end of extraction jar is equipped with the gas outlet, this gas outlet links to each other through gas outlet valve and condenser, condenser and spices holding vessel link to each other.
2. The multi-solvent extraction tank of natural aromatic plants as claimed in claim 1, wherein a gas inlet valve is further disposed between the steam inlet pipe and the inlet of the multi-solvent steam.
3. The multi-solvent extraction tank of natural aromatic plants as claimed in claim 1, wherein the condenser has a gas outlet at one end and is connected to a perfume storage tank at the other end.
4. The multi-solvent extraction tank of natural aromatic plants according to claim 1, wherein the extraction tank is a sealed tank body provided with an insulating layer.
5. The use method of the natural aromatic plant multi-solvent extraction tank comprises the following steps:
(1) filling natural aromatic plants into a sealed extraction tank provided with a heat-insulating layer through a feed inlet, conveying the natural aromatic plants into the extraction tank through a screw conveyor in the extraction tank, opening a gas inlet valve, closing a gas outlet valve, allowing a plurality of extraction solvents to form steam through a gas evaporator respectively, adjusting the flow through a flow valve, allowing the steam to enter a steam inlet pipe, allowing the steam to enter the extraction tank from a gas inlet of multi-element solvent steam on one side of the sealed extraction tank, forming pressure, and extracting the natural aromatic plants through the steam of the plurality of extraction solvents;
(2) the natural aromatic plant enters an extraction tank through a screw conveyor and fully contacts with steam of a plurality of extraction solvents in the extraction tank to generate natural aromatic plant aroma components;
(3) after extraction is finished, opening an air outlet valve, and allowing the steam carrying extracted natural aromatic plant aroma components to enter a condenser from an air outlet of the extraction tank and leave the extraction tank;
(4) collecting the cooled liquid to obtain natural perfume extract.
6. The method of claim 5, wherein the gas valve controls the extraction pressure in the tank to be 100kPa to 250 kPa.
7. The method of claim 5, wherein the gas flow valves are used to control the flow rate of the solvent vapor to be 5L/Min-300L/Min.
8. The method as claimed in claim 5, wherein the amount of the natural aromatic plant filled in the inlet of the extraction tank is between 100g and 100 kg.
9. The method of claim 5, wherein the plurality of extraction solvents are different polarity extraction solvents, the extraction solvent is water, ethanol, acetone, ethyl acetate, and carbon dioxide, and the vapor is generated by a gas evaporator to extract the natural aromatic plant.
10. The method of using the multi-solvent extraction tank for natural aromatic plants according to claim 5, wherein the extraction time of natural aromatic plants is 60-360 minutes.
CN202010715974.3A 2020-07-23 2020-07-23 Natural aromatic plant multi-element extraction tank and use method thereof Pending CN113969212A (en)

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CN202010715974.3A CN113969212A (en) 2020-07-23 2020-07-23 Natural aromatic plant multi-element extraction tank and use method thereof

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114849275A (en) * 2022-05-18 2022-08-05 郑州远洋油脂工程技术有限公司 Ethanol extraction process of powdery material
CN115433637A (en) * 2022-09-29 2022-12-06 东莞市鸿馥生物科技有限公司 Preparation method of green tea spice

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114849275A (en) * 2022-05-18 2022-08-05 郑州远洋油脂工程技术有限公司 Ethanol extraction process of powdery material
CN115433637A (en) * 2022-09-29 2022-12-06 东莞市鸿馥生物科技有限公司 Preparation method of green tea spice

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