CN211462126U - Device for extracting fenchyl alcohol from by-product of borneol production - Google Patents

Device for extracting fenchyl alcohol from by-product of borneol production Download PDF

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Publication number
CN211462126U
CN211462126U CN201921495295.9U CN201921495295U CN211462126U CN 211462126 U CN211462126 U CN 211462126U CN 201921495295 U CN201921495295 U CN 201921495295U CN 211462126 U CN211462126 U CN 211462126U
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pipe
electric
valve
tower
flow
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CN201921495295.9U
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张黎伟
高兴忠
曾类文
普国文
张文俊
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Yunnan Linyuan Spices Co ltd
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Yunnan Linyuan Spices Co ltd
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Abstract

The utility model relates to an ice flakes production facility field especially relates to an extract fenchyl alcohol's device in the accessory substance of following production borneol. The device for extracting fenchyl alcohol from the by-product generated in the production of borneol comprises a rectifying tower (1), a vacuum pump (2), a reflux tank (3), a reflux pump (4), a starting switch (5) and a controller (6); a steam heater (7), a bottom distributor (8), a middle condenser (9), a lower layer filler (10), a middle layer distributor (11), an upper layer filler (12), a liquid collector (13) and a top condenser (14) are sequentially arranged in the rectifying tower (1) from bottom to top. The utility model discloses simple structure, convenient operation, save manual work, fenchyl alcohol product purity height.

Description

Device for extracting fenchyl alcohol from by-product of borneol production
Technical Field
The utility model relates to an ice flakes production facility field especially relates to an extract fenchyl alcohol's device in the accessory substance of following production borneol.
Background
Fenchyl alcohol, also known as cumyl alcohol, known under the chemical name 1, 3, 3-trimethyl-2-norbornanol, has a camphor-like odor with a citrus note, has a bitter lime-like flavor, is slightly soluble in water, is soluble in ethanol, and is found in natural mixtures in spruce oil and pine oil. The main application is as follows: in GB 2760-1996, food flavors are defined which are approved for use. Fenchyl alcohol is widely used in costustoot, grass, citrus or certain floral essences and cosmetics, can also be used in daily chemicals such as antiperspirants, fabric softeners and liquid detergents, and can also be esterified with various organic acids to obtain fenchyl alcohol ester perfume. Currently fenchyl alcohol is obtained mainly by two routes, one is by organic synthesis, for example, starting with fenchyl ketone, by grignard reaction with ethylmagnesium bromide or by reduction with sodium alkoxide. The second method is separation and extraction from natural essential oil containing fenchyl alcohol.
The synthesis of borneol has many technical routes, and the most mature and industrialized production is that alpha-pinene is extracted from turpentine, and the alpha-pinene and anhydrous oxalic acid are subjected to esterification reaction under the catalysis of an acid catalyst to generate borneol oxalate, and then the borneol oxalate is subjected to saponification reaction with sodium hydroxide to obtain crude borneol, and the crude borneol is further purified to obtain the target product of borneol.
In the esterification reaction process of borneol production, due to the isomerization of alpha-pinene, besides the target product of borneol oxalate, a large amount of isomerization products such as camphene, dipentene, camphor, fenchyl alcohol ester, terpineol ester, other linalool ester and the like are generated. In the current production mode, only the by-products in the borneol production are simply divided into light components (light oil) and heavy components, the heavy components are mixed into borneol oxalate for saponification, and then alcohol mixtures such as fenchyl alcohol, terpineol, other linalools and the like are generated in addition to the target product borneol, wherein the fenchyl alcohol is mainly used, the content is about 40-60%, and 17-20% of borneol (borneol and isoborneol) is dissolved.
When the alcohol mixture is traditionally fractionated, because the temperature at the top of the tower is not easy to control, the borneol is easy to block the pipeline of the rectifying tower, and the production is stopped.
Disclosure of Invention
Aiming at the defects of the prior art, the utility model provides a device which has simple structure, convenient operation, labor saving and high purity of fenchyl alcohol product and can extract fenchyl alcohol from the by-product of borneol production; the problem that a rectifying tower is easily blocked in the conventional fractionation is effectively solved.
In order to achieve the above object, the utility model discloses the technical solution who adopts is:
the device for extracting fenchyl alcohol from the by-product generated in the production of borneol comprises a rectifying tower, a vacuum pump, a reflux tank, a reflux pump, a starting switch and a controller;
a steam heater, a bottom distributor, a middle condenser, a lower layer filler, a middle layer distributor, an upper layer filler, a liquid collector and a top condenser are sequentially arranged in the rectifying tower from bottom to top;
a liquid discharge pipe is arranged at the lowest part of the rectifying tower, and an electric liquid discharge valve is arranged on the liquid discharge pipe;
the steam heater is connected with a steam pipe, and an electric steam inlet flow valve is arranged on the steam pipe; a feeding pipe is arranged in the middle of the rectifying tower, and an electric feeding valve is arranged on the feeding pipe; the middle condenser is connected with a middle cold water inlet pipe, and an electric middle cold water inlet flow valve is arranged on the middle cold water inlet pipe; the top condenser is connected with a top cold water inlet pipe, and an electric top cold water inlet flow valve is arranged on the top cold water inlet pipe; the liquid collector is connected with the reflux tank through the liquid outlet pipe; the reflux tank is connected with a liquid inlet of a reflux pump through a circulating pipe, a liquid outlet of the reflux pump is connected with a conveying pipe, the conveying pipe is connected with a reflux pipe and a finished product pipe, and the other end of the reflux pipe is connected with the middle part of the rectifying tower; the return pipe is provided with an electric return flow valve and a return liquid flow sensor, and the finished product pipe is provided with an electric finished product flow regulating valve and a finished product liquid flow sensor;
the top end of the rectifying tower is provided with an evacuation pipe and a vacuum degree sensor, and the evacuation pipe is provided with a vacuum pump and an electric vacuum flow valve;
a tower kettle temperature sensor, a tower middle temperature sensor and a tower top temperature sensor are sequentially arranged on the side of the rectifying tower from bottom to top;
the starting switch, backward flow liquid flow sensor, finished product liquid flow sensor, vacuum sensor, tower cauldron temperature sensor, tower temperature sensor and top of the tower temperature sensor pass through the signal line and link to each other with the controller, the controller passes through the control line and vacuum pump, the backwash pump, electronic tapping valve, electronic steam flow valve, electronic feed valve, electronic middle part advances cold water flow valve, electronic top advances cold water flow valve, electronic backward flow valve, electronic finished product flow control valve and electronic vacuum flow valve link to each other.
The lower layer filler and the upper layer filler are XX-double-edge corrugated fillers.
The controller is a DCS host.
The signal lines and the control lines are shielding lines.
When the device works, a starting switch is pressed down, a controller controls an electric feed valve to be opened, an alcohol mixture subjected to freezing crystallization and centrifugal separation is input into a rectifying tower, the alcohol mixture falls after being distributed by a bottom distributor, the controller controls the electric feed valve to be closed after a certain time, a vacuum pump runs, an electric steam inlet flow valve, an electric middle part cold water inlet flow valve, an electric top cold water inlet flow valve and an electric vacuum flow valve are opened, the vacuum degree is controlled to be less than-0.06 MPa, the temperature of a tower kettle is controlled to be 135-140 ℃, the temperature in the tower is controlled to be 118-126 ℃, the temperature at the top of the tower is controlled to be 40-60 ℃, after a period of time, gas evaporated by heating of the alcohol mixture through a steam heater is condensed to a certain temperature in a middle condenser, so that a substance with a certain boiling point falls in a liquefied manner, and other evaporated substances are, and the rest evaporated substances are subjected to liquefaction and falling of partial substances after being treated by the upper-layer filler, are uniformly distributed by the middle-layer distributor and then fall on the lower-layer filler for treatment, and finally, the rest evaporated substances are cooled by the top condenser, collected by the liquid collector and flow into the reflux tank. The controller controls the reflux pump to operate, the electric reflux flow valve and the electric finished product flow regulating valve to be opened, the reflux ratio is adjusted to be 5:1-8:1, the finished product flow rate is 200L/h, and a fenchyl alcohol product with the purity of more than or equal to 96% is obtained; when the finished product flow rate is less than 200L/h, the controller controls the vacuum pump and the reflux pump to stop running, the electric steam inlet flow valve, the electric middle cold water inlet flow valve, the electric top cold water inlet flow valve, the electric vacuum flow valve, the electric reflux flow valve and the electric finished product flow regulating valve are closed, the electric liquid discharge valve is opened, the mixture of other fusel dissolved borneol is discharged from the liquid discharge pipe, and after the discharge is finished for a period of time. The controller controls the electric bleeder valve to close and complete the extraction of fenchyl alcohol from the by-product of borneol production.
Advantageous effects
1. The utility model discloses simple structure, convenient operation, save manual work, fenchyl alcohol product purity height.
2. The utility model discloses a tower cauldron temperature sensor and by the electronic steam flow valve regulation flow that advances of controller control, thereby not block up the pipeline and the energy saving with the borneol evaporation with the temperature control of tower cauldron in the within range that needs.
3. The utility model discloses a middle part condenser makes the boiling point fall in the material liquefaction under the uniform temperature to guarantee the high-efficient work of packing.
4. The utility model discloses a backward flow liquid flow sensor, finished product liquid flow sensor and by electronic backward flow valve of controller control, electronic finished product flow control valve regulated flow, with the backward flow ratio control in certain extent to controller control automatic shutdown heating when the finished product velocity of flow is less than a definite value, thereby guarantee finished product quality and the energy saving.
5. The utility model discloses a vacuum sensor and by controller control electric vacuum flow valve regulated flow, with vacuum control in the within range that needs, guaranteed to draw going on and the energy saving of fenchyl alcohol work.
6. The utility model discloses the filler adopts XX-two cutting edge ripple packs, can make the fenchyl alcohol product purity that obtains high.
7. The utility model discloses signal line and control line adopt the shielded wire, have higher transmission rate and good anti electromagnetic interference ability, guaranteed to draw the safety of fenchyl alcohol during operation.
8. The utility model discloses the controller carries out automated control to each equipment for the DCS host computer, and control accuracy is high.
9. The utility model discloses can control temperature, velocity of flow, vacuum, reflux ratio, be difficult for blockking up the rectifying column when making the fractionation to obtain the fenchyl alcohol product that purity is more than or equal to 96%.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
1-rectifying tower, 2-vacuum pump, 3-reflux tank, 4-reflux pump, 5-start switch, 6-controller, 7-steam heater, 8-bottom distributor, 9-middle condenser, 10-lower filler, 11-middle distributor, 12-upper filler, 13-liquid collector, 14-top condenser, 15-liquid discharge pipe, 16-electric liquid discharge valve, 17-steam pipe, 18-electric steam inlet flow valve, 19-feed pipe, 20-electric feed valve, 21-middle cold water inlet pipe, 22-electric middle cold water inlet flow valve, 23-top cold water inlet pipe, 24-electric top cold water inlet flow valve, 25-liquid outlet pipe, 26-circulating pipe, 27-conveying pipe, etc, 28-a return pipe, 29-a finished product pipe, 30-an electric return flow valve, 31-a return liquid flow sensor, 32-an electric finished product flow regulating valve, 33-a finished product liquid flow sensor, 34-a vacuum pipe, 35-a vacuum degree sensor, 36-an electric vacuum flow valve, 37-a tower kettle temperature sensor, 38-a tower middle temperature sensor and 39-a tower top temperature sensor.
Detailed Description
As shown in fig. 1, the apparatus for extracting fenchyl alcohol from by-products of ice production comprises a rectifying tower 1, a vacuum pump 2, a reflux tank 3, a reflux pump 4, a start switch 5 and a controller 6;
a steam heater 7, a bottom layer distributor 8, a middle condenser 9, a lower layer filler 10, a middle layer distributor 11, an upper layer filler 12, a liquid collector 13 and a top condenser 14 are sequentially arranged in the rectifying tower 1 from bottom to top;
a liquid discharging pipe 15 is arranged at the lowest part of the rectifying tower 1, and an electric liquid discharging valve 16 is arranged on the liquid discharging pipe 15;
the steam heater 7 is connected with a steam pipe 17, and an electric steam inlet flow valve 18 is arranged on the steam pipe 17; a feeding pipe 19 is arranged in the middle of the rectifying tower 1, and an electric feeding valve 20 is arranged on the feeding pipe 19; the middle condenser 9 is connected with a middle cold water inlet pipe 21, and an electric middle cold water inlet flow valve 22 is arranged on the middle cold water inlet pipe 21; the top condenser 14 is connected with a top cold water inlet pipe 23, and an electric top cold water inlet flow valve 24 is arranged on the top cold water inlet pipe 23; the liquid collector 13 is connected with the reflux tank 3 through a liquid outlet pipe 25; the reflux tank 3 is connected with a liquid inlet of a reflux pump 4 through a circulating pipe 26, a liquid outlet of the reflux pump 4 is connected with a conveying pipe 27, the conveying pipe 27 is connected with a reflux pipe 28 and a finished product pipe 29, and the other end of the reflux pipe 28 is connected with the middle part of the rectifying tower 1; the return pipe 28 is provided with an electric return flow valve 30 and a return liquid flow sensor 31, and the finished product pipe 29 is provided with an electric finished product flow regulating valve 32 and a finished product liquid flow sensor 33;
the top end of the rectifying tower 1 is provided with an evacuation pipe 34 and a vacuum degree sensor 35, and the evacuation pipe 34 is provided with a vacuum pump 2 and an electric vacuum flow valve 36;
a tower kettle temperature sensor 37, a tower middle temperature sensor 38 and a tower top temperature sensor 39 are sequentially arranged on the rectifying tower 1 side from bottom to top;
the starting switch 5, the reflux liquid flow sensor 31, the finished product liquid flow sensor 33, the vacuum degree sensor 35, the tower kettle temperature sensor 37, the tower temperature sensor 38 and the tower top temperature sensor 39 are connected with the controller 6 through signal lines, and the controller 6 is connected with the vacuum pump 2, the reflux pump 4, the electric tapping valve 16, the electric steam inlet flow valve 18, the electric feed valve 20, the electric middle cold water inlet flow valve 22, the electric top cold water inlet flow valve 24, the electric reflux flow valve 30, the electric finished product flow regulating valve 32 and the electric vacuum flow valve 36 through control lines.
The lower layer filler 10 and the upper layer filler 12 are XX-double-edge corrugated fillers.
The controller 6 is a DCS host.
The signal lines and the control lines are shielding lines.
When the device works, the starting switch 5 is pressed, the controller 6 controls the electric feed valve 20 to be opened, the alcohol mixture which is subjected to freezing crystallization and centrifugal separation treatment is input into the rectifying tower 1, the alcohol mixture falls after being distributed by the bottom distributor 8, the controller 6 controls the electric feed valve 20 to be closed after a certain time, the vacuum pump 2 operates, the electric steam flow valve 18, the electric middle cold water flow valve 22, the electric top cold water flow valve 24 and the electric vacuum flow valve 36 are opened, the vacuum degree is controlled to be less than-0.06 MPa, the temperature of the tower kettle is controlled to be 135 ℃ -140 ℃, the temperature in the tower is controlled to be 118 ℃ -126 ℃, the temperature of the tower top is controlled to be 40 ℃ -60 ℃, after a period of time, the alcohol mixture is heated and evaporated by the steam heater 7, the gas is condensed to a certain temperature in the middle condenser 9, and the substance with a boiling point at a, other evaporation materials are treated by the lower layer filler 10, partial evaporation materials are liquefied and fall, the rest evaporation materials are treated by the upper layer filler 12, partial evaporation materials are liquefied and fall, are uniformly distributed by the middle layer distributor 11 and then fall on the lower layer filler 10 for treatment, and finally the rest evaporation materials are cooled by the top condenser 14, collected by the liquid collector 13 and flow into the reflux tank 3. The controller 6 controls the reflux pump 4 to operate, the electric reflux flow valve 30 and the electric finished product flow regulating valve 32 to be opened, the reflux ratio is adjusted to be 5:1-8:1, the finished product flow rate is 200L/h, and a fenchyl alcohol product with the purity of more than or equal to 96% is obtained; when the finished product flow rate is less than 200L/h, the controller 6 controls the vacuum pump 2 and the reflux pump 4 to stop running, the electric steam inlet flow valve 18, the electric middle cold inlet flow valve 22, the electric top cold inlet flow valve 24, the electric vacuum flow valve 36, the electric reflux flow valve 30 and the electric finished product flow regulating valve 32 are closed, the electric liquid discharge valve 16 is opened, the mixture of other fusel dissolved borneol is discharged from the liquid discharge pipe 15, and after a period of time is finished. Controller 6 controls the closing of the electric bleeder valve 16 to complete the extraction of fenchyl alcohol from the by-product of ice-sheet production.

Claims (5)

1. The device for extracting fenchyl alcohol from the by-product generated in the production of borneol is characterized by comprising a rectifying tower (1), a vacuum pump (2), a reflux tank (3), a reflux pump (4), a starting switch (5) and a controller (6);
a steam heater (7), a bottom distributor (8), a middle condenser (9), a lower layer filler (10), a middle layer distributor (11), an upper layer filler (12), a liquid collector (13) and a top condenser (14) are sequentially arranged in the rectifying tower (1) from bottom to top;
a liquid discharging pipe (15) is arranged at the lowest part of the rectifying tower (1), and an electric liquid discharging valve (16) is arranged on the liquid discharging pipe (15);
the steam heater (7) is connected with a steam pipe (17), and an electric steam inlet flow valve (18) is arranged on the steam pipe (17); a feeding pipe (19) is arranged in the middle of the rectifying tower (1), and an electric feeding valve (20) is arranged on the feeding pipe (19); the middle condenser (9) is connected with a middle cold water inlet pipe (21), and an electric middle cold water inlet flow valve (22) is arranged on the middle cold water inlet pipe (21); the top condenser (14) is connected with a top cold water inlet pipe (23), and an electric top cold water inlet flow valve (24) is arranged on the top cold water inlet pipe (23); the liquid collector (13) is connected with the reflux tank (3) through a liquid outlet pipe (25); the reflux tank (3) is connected with a liquid inlet of a reflux pump (4) through a circulating pipe (26), a liquid outlet of the reflux pump (4) is connected with a conveying pipe (27), the conveying pipe (27) is connected with a reflux pipe (28) and a finished product pipe (29), and the other end of the reflux pipe (28) is connected with the middle part of the rectifying tower (1); an electric backflow flow valve (30) and a backflow liquid flow sensor (31) are arranged on the backflow pipe (28), and an electric finished product flow regulating valve (32) and a finished product liquid flow sensor (33) are arranged on the finished product pipe (29);
the top end of the rectifying tower (1) is provided with a vacuum-pumping pipe (34) and a vacuum degree sensor (35), and the vacuum-pumping pipe (34) is provided with a vacuum pump (2) and an electric vacuum flow valve (36);
a tower kettle temperature sensor (37), a tower middle temperature sensor (38) and a tower top temperature sensor (39) are sequentially arranged on the rectifying tower (1) side from bottom to top;
starting switch (5), backward flow liquid flow sensor (31), finished product liquid flow sensor (33), vacuum sensor (35), tower cauldron temperature sensor (37), tower middle temperature sensor (38) and top of the tower temperature sensor (39) link to each other with controller (6) through the signal line, controller (6) pass through control line and vacuum pump (2), backwash pump (4), electronic tapping valve (16), electronic steam flow valve (18) of advancing, electronic feed valve (20), electronic middle part advances cold water flow valve (22), electronic top advances cold water flow valve (24), electronic backward flow valve (30), electronic finished product flow control valve (32) and electronic vacuum flow valve (36) link to each other.
2. The apparatus for extracting fenchyl alcohol from by-products of the production of ice flakes according to claim 1, wherein the lower layer of packing (10) and the upper layer of packing (12) are XX-double-spike corrugated packing.
3. The apparatus for extracting fenchyl alcohol from by-products from the production of ice flakes according to claim 1 or 2, wherein the controller (6) is a DCS master.
4. The apparatus of claim 1 or 2, wherein the signal and control lines are shielded lines.
5. The apparatus of claim 3, wherein the signal and control lines are shielded lines.
CN201921495295.9U 2019-09-10 2019-09-10 Device for extracting fenchyl alcohol from by-product of borneol production Active CN211462126U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201921495295.9U CN211462126U (en) 2019-09-10 2019-09-10 Device for extracting fenchyl alcohol from by-product of borneol production

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201921495295.9U CN211462126U (en) 2019-09-10 2019-09-10 Device for extracting fenchyl alcohol from by-product of borneol production

Publications (1)

Publication Number Publication Date
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Legal Events

Date Code Title Description
GR01 Patent grant
GR01 Patent grant
PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of utility model: A device for extracting fenpropanol from byproducts of borneol production

Effective date of registration: 20230620

Granted publication date: 20200911

Pledgee: Yuxi Branch of Postal Savings Bank of China Co.,Ltd.

Pledgor: YUNNAN LINYUAN SPICES CO.,LTD.

Registration number: Y2023980045104