CN111676093A - Copper pipe cooling method eucalyptus oil purification process - Google Patents
Copper pipe cooling method eucalyptus oil purification process Download PDFInfo
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- CN111676093A CN111676093A CN202010541558.6A CN202010541558A CN111676093A CN 111676093 A CN111676093 A CN 111676093A CN 202010541558 A CN202010541558 A CN 202010541558A CN 111676093 A CN111676093 A CN 111676093A
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- copper pipe
- eucalyptus oil
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- 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
- C11B3/12—Refining fats or fatty oils by distillation
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
- F28D7/16—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being arranged in parallel spaced relation
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- Chemical Kinetics & Catalysis (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Microbiology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
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- General Engineering & Computer Science (AREA)
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the field of eucalyptus oil processing, and particularly relates to a copper pipe cooling method eucalyptus oil purification process, wherein a copper pipe cooling type eucalyptus oil purification tank is internally provided with a dense copper pipe, cooling gas is introduced into the copper pipe to maintain the surface temperature of the copper pipe at-30 to-10 ℃, eucalyptus oil mixed gas evaporated by an evaporation device is introduced into the copper pipe cooling type eucalyptus oil purification tank, the copper pipe cooling type eucalyptus oil purification tank is provided with an exhaust safety valve and is connected with a mixed gas return pipe, the eucalyptus oil mixed gas is crystallized on the surface of the copper pipe, after a period of crystallization, a heating medium is introduced into the copper pipe to control the temperature in the copper pipe cooling type eucalyptus oil purification tank, the temperature in the first stage is-30 to 0.5 ℃, the temperature in the second stage is 2 to 10 ℃, the temperature is kept for 1 to 5 hours, and a dissolved substance obtained in the second stage is collected as 1, 8-cineole, and in the third stage, heating to 30-40 ℃, completely removing crystals on the surface of the copper pipe, and then carrying out ultra-cold crystallization on the eucalyptus oil.
Description
Technical Field
The invention belongs to the field of eucalyptus oil processing, and particularly relates to a process for purifying eucalyptus oil by a copper tube cooling method.
Background
The eucalyptus oil is an aromatic essential oil secreted by eucalyptus leaf oil gland cells, and is a mixture containing multiple organic components. Eucalyptus oil can be classified into three categories according to main components and purposes: pharmaceuticals, fragrances, and industrial oils. The most important of them is the medicinal eucalyptus oil, the main component of which is 1, 8-cineole.
The crude eucalyptus oil of the natural product has more impurities, wherein the crude eucalyptus oil mainly contains alpha-pinene, and also contains a small amount of beta-pinene, myrcene, alpha-phellandrene, limonene, p-cymene, gamma-terpinene, linalool and the like. Various impurities and the 1, 8-cineole are isomers or have very similar molecular structures and molecular weights, have similar physicochemical properties and bring great difficulty to the purification of the cineole. Literature research shows that there are many methods for separating eucalyptol, such as supercritical extraction, silica gel column chromatography, chemical reaction, catalytic rectification, low temperature crystallization, and falling film crystallization.
CN102504955B discloses a process for extracting and purifying eucalyptus oil, which utilizes an auxiliary agent to assist vacuum batch rectification to extract high-purity eucalyptus oil; under the condition that the traditional rectification process is not changed greatly, the thermodynamic property of a eucalyptus oil system is changed by adding an auxiliary agent, the separation efficiency is improved, and high-purity eucalyptol and a byproduct alpha-pinene are extracted by adjusting the reflux ratio and the temperature of a tower kettle; the content of the extracted eucalyptol is more than 90 percent, the highest content can reach 96.50 percent, the yield can reach more than 75 percent, the production period is within 6 hours, the process operation is simple, the production process is stable, meanwhile, a byproduct containing about 80 percent of alpha-pinene is obtained, and the additional value of the crude eucalyptus oil is increased.
Most of the existing extraction processes are purified by a reflux condensation method. The traditional low-temperature crystallization purification method is to collect condensed reflux liquid and then cool and crystallize.
Disclosure of Invention
The invention aims to provide a process for purifying eucalyptus oil by a copper tube cooling method, which comprises the steps of directly introducing distilled steam, utilizing a copper tube to extremely rapidly cool steam for crystallization, and then heating and dissolving crystals on the surface of the copper tube to obtain high-purity 1, 8-cineole.
In order to achieve the purpose, the invention adopts the following technical scheme: a copper pipe cooling method eucalyptus oil purification process comprises the steps of arranging a dense copper pipe in a copper pipe cooling type eucalyptus oil purification tank, introducing cooling gas into the copper pipe to maintain the surface temperature of the copper pipe at-30 to-10 ℃, introducing eucalyptus oil mixed gas evaporated by an evaporation device into the copper pipe cooling type eucalyptus oil purification tank, arranging an exhaust safety valve in the copper pipe cooling type eucalyptus oil purification tank and connecting the exhaust safety valve with a mixed gas return pipe, crystallizing the eucalyptus oil mixed gas on the surface of the copper pipe, introducing a heating medium into the copper pipe after crystallizing for a period of time, controlling the temperature in the copper pipe cooling type eucalyptus oil purification tank, keeping the temperature at-30-0.5 ℃ in a first stage, keeping the temperature at 2-10 ℃ in a second stage for 1-5 hours, collecting a dissolved substance obtained in the second stage, namely 1, 8-cineole, heating to 30-40 ℃ in a third stage, completely removing the crystallized substance on the surface of the copper pipe, then carrying out ultra-cold crystallization on the eucalyptus oil.
Preferably, the copper pipes are divided into two groups, the copper pipes are driven to rotate through the rotating mechanism, and crystallization on each copper pipe is more uniform.
Preferably, the spray head for spraying the eucalyptus oil mixed gas on the surface of the copper pipe can move up and down, so that the crystallization efficiency is improved.
The invention has the technical effects that: the traditional purification process of recrystallization after condensation reflux is abandoned, the eucalyptus oil is directly crystallized by extremely cooling through a copper pipe, and the product purity can be ensured by collecting the dissolved product with a fixed temperature range after crystallization, so that the purification efficiency is improved, and the purity can reach 99%. Directly cooling for crystallization, and then dissolving at normal temperature, thereby simplifying the process flow.
Drawings
FIG. 1 is a schematic view of a copper tube cooling type eucalyptus oil purification tank;
FIG. 2 is a schematic view showing the connection structure of a reciprocating screw rod and a movable nozzle in a copper pipe cooling type eucalyptus oil purification tank;
FIG. 3 is a schematic structural view of a rack in a copper tube cooling type eucalyptus oil purification tank;
FIG. 4 is a schematic structural view of a copper pipe cooling mechanism in the copper pipe cooling type eucalyptus oil purification tank;
FIG. 5 is a schematic view of the structure of the driving member in the copper tube cooled eucalyptus oil purification tank;
fig. 6 is a schematic structural view of a lower rotating frame and an air duct in the copper pipe cooling type eucalyptus oil purifying tank.
In the figure, 1 tank body, 2 reciprocating screw rod, 3 movable spray head, 4 mixed steam input pipe, 5 copper pipe cooling mechanism, 6 upper rotating frame, 7 lower rotating frame, 8 exhaust pipe, 9 air inlet pipe, 10 driving piece, 11 rack, 12 discharge port, 13 driving motor, 14 fixed frame, 15 limiting rod, 16 thread sleeve, 17 movable block, 18 nozzle, 19 top disc, 20 chassis, 21 copper pipe, 22 sealing ring, 23 air duct, 24 connecting rod, 25 driving shaft, 26 driven shaft, 27 driving gear, 28 transmission gear, 29 one-way bearing, 30 driven gear and driving disc 31.
Detailed Description
The following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
A copper pipe cooling method eucalyptus oil purification process comprises the steps of arranging a dense copper pipe in a copper pipe cooling type eucalyptus oil purification tank, introducing cooling gas into the copper pipe to maintain the surface temperature of the copper pipe at-30 to-10 ℃, introducing eucalyptus oil mixed gas evaporated by an evaporation device into the copper pipe cooling type eucalyptus oil purification tank, arranging an exhaust safety valve in the copper pipe cooling type eucalyptus oil purification tank and connecting the exhaust safety valve with a mixed gas return pipe, crystallizing the eucalyptus oil mixed gas on the surface of the copper pipe, introducing a heating medium into the copper pipe after crystallizing for a period of time, controlling the temperature in the copper pipe cooling type eucalyptus oil purification tank, keeping the temperature at-30-0.5 ℃ in a first stage, keeping the temperature at 2-10 ℃ in a second stage for 1-5 hours, collecting a dissolved substance obtained in the second stage, namely 1, 8-cineole, heating to 30-40 ℃ in a third stage, completely removing the crystallized substance on the surface of the copper pipe, then carrying out ultra-cold crystallization on the eucalyptus oil.
Firstly, a copper tube cooling type eucalyptus oil purification tank adopted by the process is introduced, the structure of the copper tube cooling type eucalyptus oil purification tank is shown in fig. 1-6, the copper tube cooling type eucalyptus oil purification tank comprises a tank body 1, a vertically arranged reciprocating screw rod 2 is connected in the tank body 1 in a rotating mode, a movable spray head 3 is connected to the reciprocating screw rod 2 in a threaded mode, the lower end of the reciprocating screw rod 2 is connected with the bottom of the tank body 1 in a rotating mode through a fixing frame 14, a gap is reserved between the fixing frame 14 and the side wall of the tank body 1, discharging of finished products is facilitated, a limiting rod 15 penetrates through the movable spray head 3, the limiting rod 15 is fixedly connected to the upper end of the tank body 1, and the movable spray head 3 can be limited by the.
Further, movable nozzle 3 is by thread bush 16, movable block 17 and nozzle 18 constitute, thread bush 16 threaded connection is outside reciprocal lead screw 2, movable block 17 fixed connection is outside thread bush 16, the quantity of nozzle 18 is two, and two nozzle 18 respectively fixed connection correspond in the both sides of movable block 17 and with copper pipe cooling body 5's position, mixed steam input tube 4 is through setting up passageway and two nozzle 18 intercommunications in movable block 17, be equipped with mixed steam input tube 4 on movable nozzle 3, this mixed steam input tube 4 adopts high temperature resistant cold-resistant elastic material to make, make at the in-process that movable nozzle 3 reciprocated, can keep mixed steam's continuation input.
The copper pipe cooling mechanism 5 is arranged on both sides of the reciprocating screw rod 2, the upper end and the lower end of the copper pipe cooling mechanism 5 are respectively and rotatably connected with an upper rotating frame 6 and a lower rotating frame 7, the upper rotating frame 6 is provided with an exhaust pipe 8, the lower rotating frame 7 is provided with an air inlet pipe 9, the copper pipe cooling mechanism 5 is composed of a top disc 19, a bottom disc 20 and a plurality of copper pipes 21, the top disc 19 and the bottom disc 20 are arranged in parallel, the plurality of copper pipes 21 are fixedly connected between the top disc 19 and the bottom disc 20, the axes of the copper pipes 21 are parallel to the axes of the top disc 19 and the bottom disc 20, the upper end of each copper pipe 21 is communicated with the exhaust pipe 8 through a rotary joint rotatably connected on the top disc 19, the bottom disc 20 is hermetically and rotatably connected with a sealing ring 22, the sealing ring 22 is fixedly connected with an air guide pipe 23 communicated with the air inlet pipe 9, this device adopts movable copper pipe 21 for movable shower nozzle 3 only is used in one of them copper pipe 21 at every turn, makes the energy more concentrated, makes eucalyptus oil cooling crystallization attach on copper pipe 21's surface more easily, improves the effect of condensation crystallization greatly.
It should be noted that the air inlet end of the air inlet pipe 9 is connected with a heat medium pipe and a cold air pipe respectively through a three-way valve, and the invention can also lead hot steam into the copper pipe 21 through the heat medium pipe after the cooling crystallization of the eucalyptus oil is completed, so that the eucalyptus oil crystal grains crystallized on the surface of the copper pipe are dissolved to obtain the eucalyptus oil, the crystal does not need to be transferred back and forth, and additional dissolving equipment does not need to be used, so that the invention is simpler and more convenient.
The upper rotating frame 6 is provided with a driving part 10 for driving the copper pipe cooling mechanism 5 to rotate in a single direction, the driving part 10 is composed of an L-shaped connecting rod 24 fixedly connected to the upper rotating frame 6, a driving shaft 25 and a driven shaft 26, the driving shaft 25 and the driven shaft 26 are both horizontally and rotatably connected between the connecting rod 24 and the upper rotating frame 6, the driving shaft 25 is fixedly connected with a driving gear 27 and a transmission gear 28, the driving gear 27 is fixedly connected with the driving shaft 25 through a single-direction bearing 29, the driven shaft 26 is fixedly connected with a driven gear 30 and a driving disc 31, the driven gear 30 is meshed with the transmission gear 28, the driving disc 31 acts on the upper surface of the top disc 19, it should be noted that the driving disc 31 is wound with a circle of friction ring, the friction ring is made of rubber material, the friction force between the driving disc 31 and the top disc 19 is, and driven gear 30 and drive gear 28 drive ratio, can realize, when drive gear 27 rotates certain angle, make copper pipe cooling body 5 rotate certain angle, realize the replacement between different copper pipes 21, through setting up driving piece 10, at the in-process that movable shower nozzle 3 reciprocated, can act on copper pipe cooling body 5, make copper pipe cooling body 5 periodically rotate, thereby can switch over different copper pipes 21 in proper order, realize better condensation effect.
Fixedly connected with and driving piece 10 complex rack 11 on the movable shower nozzle 3, rack 11 is L type rack, be equipped with tooth on the vertical section of L type rack, through setting up L type rack, realized the dislocation set between driving piece 10 and the copper pipe 21, avoid taking place to interfere between the two, rack 11 fixed connection is on the lateral wall of movable block 17, the bottom of jar body 1 is equipped with discharge gate 12, the upper end fixedly connected with of jar body 1 is used for driving motor 13 of reciprocal lead screw 2.
Example 1
When the device is used, eucalyptus oil mixed gas is firstly input from the mixed steam input pipe 4, cooling gas is input from the air inlet pipe 9, the mixed steam is discharged from a safety valve of a pressure relief opening above the tank body 1, the cooling gas is discharged from the air outlet pipe 8, the temperature of the surface of the copper pipe 21 is controlled to be maintained at-30 ℃, then the driving motor 13 is started, the driving motor 13 drives the reciprocating screw rod 2 to rotate in size, the movable spray head 3 can reciprocate up and down along the reciprocating screw rod 2, the nozzle of the movable spray head 3 can move up and down along the copper pipe 21 close to the movable spray head, when the high-temperature mixed steam contacts the low-temperature copper pipe 21, the phenomenon of extremely cold crystallization can occur, and the eucalyptus oil is cooled and crystallized.
Meanwhile, along with the up-and-down movement of the movable nozzle 3, the rack 11 will act on the driving member 10 when moving to the uppermost end, specifically, the rack 11 is engaged with the driving gear 27, and since the driving gear 27 is fixedly connected with the driving shaft 25 through the one-way bearing 29, the rack 11 will drive the driving shaft 25 to rotate a certain angle in one direction in the up-and-down movement, so that the driving gear 28 rotates, the driving gear 28 further drives the driven gear 30 engaged therewith to rotate, further, the driven shaft 26 and the driving disk 31 fixedly connected to the driven shaft 26 rotate, since the driving disk 31 contacts with the top disk 19, the top disk 19 will be driven to rotate and move by a certain angle, so that the copper tube 21 facing the position of the nozzle 18 is changed, that is, along with the continuous up-and-down movement of the movable nozzle 3, each copper tube 21 will sequentially contact with the nozzle 18, so as to condense and, compared with the traditional fixed copper tube, the nozzle 18 moves up and down along the copper tube 21, so that the crystallization distribution on a single copper tube 21 is more uniform, the effect is more excellent, and under the action of the driving piece 10, the copper tubes 21 are sequentially and alternately operated, so that the crystallization on the copper tubes 21 is more uniform, and the better crystallization effect is realized.
Finally, after crystallization is finished, a heat medium or hot water is input from the air inlet pipe 9, the temperature of the copper pipe 21 is raised, the temperature is controlled to be lower than 0 ℃ for 1 hour, substances with melting points lower than that of 1, 8-cineole are separated firstly, then the temperature is raised to 2 ℃, the temperature is kept for 5 hours, the eucalyptus oil crystal grains on the surface of the copper pipe 21 are dissolved, 1, 8-cineole is obtained, then the temperature is raised to 40 ℃ to remove impurities on the surface of the copper pipe, and the purity of the 1, 8-cineole reaches 99.6% through detection.
Example 2
Introducing cooling gas into the copper pipe to maintain the surface temperature of the copper pipe at-30 to-10 deg.C, introducing eucalyptus oil mixed gas evaporated by an evaporation device into the copper pipe cooling type eucalyptus oil purification tank, arranging an exhaust safety valve in the copper pipe cooling type eucalyptus oil purification tank and connecting with a mixed gas return pipe, crystallizing the eucalyptus oil mixed gas on the surface of the copper pipe, after crystallizing for a period of time, introducing a heating medium into the copper pipe, controlling the temperature in the copper pipe cooling type eucalyptus oil purification tank, controlling the temperature in the first stage to be-30-0.5 ℃ and the time to be 2 hours, the second stage is 2-10 deg.C for 1 hr, collecting the dissolved substance obtained in the second stage as 1, 8-cineole, heating to 30 deg.C above to completely remove the crystal on the surface of copper tube, then, the eucalyptus oil is crystallized in an extremely cold way, and the purity of the 1, 8-cineole reaches 99.1 percent through detection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (3)
1. A copper pipe cooling method eucalyptus oil purification process is characterized in that: the copper pipe cooling type eucalyptus oil purifying tank is internally provided with a dense copper pipe, cooling gas is introduced into the copper pipe to maintain the surface temperature of the copper pipe at-30 to-10 ℃, eucalyptus oil mixed gas evaporated by an evaporation device is introduced into the copper pipe cooling type eucalyptus oil purifying tank, the copper pipe cooling type eucalyptus oil purifying tank is provided with an exhaust safety valve and is connected with a mixed gas return pipe, the eucalyptus oil mixed gas is crystallized on the surface of the copper pipe, after crystallizing for a period of time, introducing a heating medium into the copper pipe, controlling the temperature in the copper pipe cooling type eucalyptus oil purification tank, wherein the temperature in the first stage is-30-0.5 ℃, the temperature in the second stage is 2-10 ℃, and keeping the temperature for 1-5 hours, collecting the dissolved substance obtained in the second stage as 1, 8-cineole, heating to 30-40 deg.C in the third stage, completely removing the crystal on the surface of copper tube, and performing ultra-cold crystallization of cineole.
2. The copper pipe cooling method eucalyptus oil purification process as claimed in claim 1, wherein the copper pipe cooling method eucalyptus oil purification process comprises the following steps: the copper pipes are divided into two groups and driven to rotate by a rotating mechanism.
3. The copper pipe cooling method eucalyptus oil purification process as claimed in claim 1, wherein the copper pipe cooling method eucalyptus oil purification process comprises the following steps: the spray head for spraying the eucalyptus oil mixed gas on the surface of the copper pipe can move up and down.
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| CN202010541558.6A CN111676093A (en) | 2020-06-15 | 2020-06-15 | Copper pipe cooling method eucalyptus oil purification process |
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| CN202010541558.6A CN111676093A (en) | 2020-06-15 | 2020-06-15 | Copper pipe cooling method eucalyptus oil purification process |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109887A (en) * | 1994-12-28 | 1995-10-11 | 天津大学 | Process for preparing high-purity natural eudesmin |
| CN204447373U (en) * | 2015-02-09 | 2015-07-08 | 江西北辰德天然生物科技有限公司 | The water circulation system that a kind of medicinal plants cooling condensation is extracted |
| CN109293671A (en) * | 2018-09-04 | 2019-02-01 | 中粮德信行健康产业有限公司 | A kind of purification process of Cineole |
-
2020
- 2020-06-15 CN CN202010541558.6A patent/CN111676093A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109887A (en) * | 1994-12-28 | 1995-10-11 | 天津大学 | Process for preparing high-purity natural eudesmin |
| CN204447373U (en) * | 2015-02-09 | 2015-07-08 | 江西北辰德天然生物科技有限公司 | The water circulation system that a kind of medicinal plants cooling condensation is extracted |
| CN109293671A (en) * | 2018-09-04 | 2019-02-01 | 中粮德信行健康产业有限公司 | A kind of purification process of Cineole |
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Application publication date: 20200918 |
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