CN211255771U - Production process system of menthyl acetate - Google Patents
Production process system of menthyl acetate Download PDFInfo
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- CN211255771U CN211255771U CN201922263776.3U CN201922263776U CN211255771U CN 211255771 U CN211255771 U CN 211255771U CN 201922263776 U CN201922263776 U CN 201922263776U CN 211255771 U CN211255771 U CN 211255771U
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Abstract
The utility model discloses a production process system of menthyl acetate. The reaction separation kettle of the production process system is provided with a kettle body and a tower body; the tower body is communicated with a condensing system; the condensing system is respectively communicated with the pressure reduction system, the acetic acid collecting tank, the front fraction collecting tank and the menthyl acetate collecting tank; the metering system is used for inputting raw materials into the kettle body; the temperature control system is used for controlling the temperature of the liquid in the kettle body; the reaction separation kettle is used for reaction of acetic anhydride and menthol, acetic acid recovery, front cut fraction recovery and menthyl acetate recovery; the condensing system is used for the total reflux of condensed liquid in the reaction process and partial reflux in the subsequent process; the pipeline of the condensing system communicated with the pressure reducing system is also provided with an air vent which is in an open state in the reaction and acetic acid recovery process and is in a closed state in the front fraction and menthyl acetate recovery process; the pressure reduction system is opened only during the recovery of the front distillate and the menthyl acetate so as to maintain the negative pressure in the reaction separation kettle. The production process system can reduce the use of equipment.
Description
Technical Field
The utility model relates to a production process system of menthyl acetate.
Background
At present, a plurality of methods for preparing menthyl acetate are disclosed in the prior art, wherein in the methods for preparing menthyl acetate, firstly, some methods adopt acetic acid or acetyl chloride and menthol as raw materials, and most reactions of the methods need acid as a catalyst, involve water washing and are not environment-friendly; secondly, allyl acetate or vinyl ester and menthol are used for ester exchange reaction for preparation, and the raw material (allyl acetate or vinyl ester) is relatively expensive and is not suitable for industrial production.
At present, acetic anhydride and menthol are used as raw materials in the preparation method of menthyl acetate, and in the preparation methods, microwave heating technology, infrared heating technology, ionic liquid or super-strong solid acid or alkali is used. The preparation methods have the following defects: in the microwave and infrared heating technologies, the equipment is expensive and cannot be industrially implemented; in the preparation method using ionic liquid, there is a drawback in that menthyl acetate cannot be extracted from ionic liquid even with a large amount of solvent; the preparation method which adopts super-strong solid acid as the catalyst relates to the links of neutralization and washing, and is not economical and environment-friendly.
For example, Oppenheim, Justus Liebigs Annalen der Chemie,1861,120(3), 350-.
A process for the preparation of menthyl acetate from acetic anhydride and menthol and K, K and 395 is disclosed in the literature (E.Rafiee, Sh.Tangestanenejad, M.H.Habibi, I.Mohammadpoor-Balthork, and V.Mirkhani, Russian Journal of Organic Chemistry,2005,41(3), 393.)5CoW12O40·3H2O is a catalyst, and the generated acetic acid needs to be neutralized with sodium bicarbonate, so water washing and liquid separation are involved.
The document (Aus d. laboratory at. d. german Anton Deppe Sohne, Chemische Berichte,1926,59,2303.) discloses a method for preparing menthyl acetate, which uses acetic anhydride and menthol as raw materials, uses phosphoric acid and the like as catalysts, mainly aims at researching the configuration isomerization problem of the menthol in the reaction, and the preparation method needs neutralization, water washing, drying, filtering and further distillation to obtain the menthyl acetate.
The literature (Y.Nakae, I.Kusaki, and T.Sato, Lithium perchlorate catalysis of alcohol under mill reactions, Synlett,2001,10, 1584) -1586 discloses a method for preparing menthyl acetate, which uses acetic anhydride and menthol as raw materials, uses Lithium perchlorate as a catalyst, and needs neutralization, water washing, drying, filtering, and then distilling to obtain menthyl acetate.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to provide a production process system of menthyl acetate in order to overcome the defect that does not have the production process system that uses menthol and acetic anhydride as the technology of raw materials preparation menthyl acetate that can satisfy not add the catalyst among the prior art yet.
The utility model discloses an above-mentioned technical problem is solved through following technical scheme:
the utility model provides a production process system of menthyl acetate, which comprises a metering system, a temperature control system, a reaction separation kettle, a condensing system, a pressure reduction system, an acetic acid collecting tank, a front fraction collecting tank and a menthyl acetate collecting tank; the reaction separation kettle is provided with a kettle body and a tower body which is positioned above the kettle body and communicated with the kettle body; the tower body is communicated with the condensing system; the condensing system is also communicated with the pressure reduction system, the acetic acid collecting tank, the front distillate collecting tank and the menthyl acetate collecting tank respectively; the metering system is used for inputting acetic anhydride and menthol into the kettle body before reaction; the temperature control system is used for controlling the temperature of the liquid in the kettle body; the reaction separation kettle is used for the reaction of acetic anhydride and menthol, the recovery of acetic acid after the reaction is finished, and the recovery of front fraction and the recovery of menthyl acetate after the recovery of acetic acid; the condensation system is used for the total reflux of the condensed liquid in the reaction process and the partial reflux of the condensed liquid in the subsequent process; a pipeline of the condensing system communicated with the pressure reduction system is also provided with a switchable vent, the vent is in an open state in the reaction process and the acetic acid recovery process, and the vent is in a closed state in the front fraction recovery process and the menthyl acetate recovery process; the pressure reduction system is opened only in the processes of front fraction recovery and menthyl acetate recovery so as to maintain the negative pressure in the reaction separation kettle.
The utility model discloses in, preferably, the production technology system still is equipped with acetic anhydride raw materials storage tank and menthol raw materials storage tank, acetic anhydride raw materials storage tank with menthol raw materials storage tank respectively with the measurement system intercommunication.
In the utility model, preferably, the metering system inputs acetic anhydride and menthol into the kettle body in a molar amount of acetic anhydride larger than that of menthol. More preferably, the metering system inputs acetic anhydride and menthol into the kettle body according to the mass ratio of 1: 1.5.
The utility model discloses in, the cauldron body still is equipped with the leakage fluid dram of switch, the leakage fluid dram is in order to discharge for the open mode after the menthyl acetate is retrieved the internal liquid of cauldron.
The utility model discloses in, preferably, the cauldron body still is equipped with raw materials entry, raw materials entry is located the top of the cauldron body, the measurement system with raw materials entry connects.
The utility model discloses in, the tower body can be located according to the conventionality in this field directly over the cauldron body.
The utility model discloses in, preferably, temperature control system still is used for control the tower body with gaseous temperature in the pipeline of condensing system intercommunication.
The utility model discloses in, condensing system can locate according to the conventionality in this field the top of tower body.
The utility model discloses in, preferably, condensing system is the double-layered shell type condenser, the outside of double-layered shell type condenser is cold fluid channel. More preferably, the cold fluid channel is provided with a cooling water inlet and a cooling water outlet.
In the utility model, the subsequent process refers to the acetic acid recovery process, the front cut recovery process and the menthyl acetate recovery process after the reaction.
The utility model discloses a method for using of production technology system as follows: after mixing acetic anhydride and menthol with certain proportion, warp metering system sends into the cauldron is internal, temperature control system will liquid in the cauldron body heats to the definite temperature after and stops the heating, because exothermic reaction is after the reaction initiation, the heat that the reaction produced can make the material in the reaction system (including reactant and result) become steam and rise to condensation system, through the condensation after and automatic backward flow extremely the cauldron is internal, this kind of automatic backward flow play a stirring effect, so, the utility model discloses a production technology system need not have the agitator, can make the raw materials misce bene in the reaction process promptly. After refluxing for about 4-5 hours, recovering the generated acetic acid at normal pressure, storing the acetic acid in the acetic acid collecting tank, starting the pressure reducing system, distilling the front cut fraction to the front cut fraction collecting tank at reduced pressure, and continuing distilling at reduced pressure to distill the menthyl acetate out to the menthyl acetate collecting tank.
The utility model discloses an actively advance the effect and lie in: the utility model discloses a production process system of menthyl acetate can satisfy the technique that uses menthol and acetic anhydride as raw materials preparation menthyl acetate that does not add the catalyst, and the reaction all goes on in a reaction separation cauldron with the separation, and need not the washing cauldron. Therefore, the occupied area can be saved, the use of equipment is reduced, the equipment investment is reduced, and the production efficiency of the equipment is improved.
Drawings
Fig. 1 is a schematic diagram of a production process system of menthyl acetate according to an embodiment of the present invention.
Description of reference numerals:
metering system 1
Kettle body 3
Pressure reducing system 6
Acetic acid collection tank 7
Front fraction collection tank 8
Menthyl acetate collecting tank 9
Acetic anhydride raw material storage tank 11
Menthol raw material storage tank 12
Detailed Description
The present invention will be more clearly and completely described below with reference to the accompanying drawings.
Example 1
The production process system of the menthyl acetate shown in the figure 1 comprises a metering system 1, a temperature control system 2, a reaction separation kettle, a condensing system 5, a pressure reduction system 6, an acetic acid collecting tank 7, a front fraction collecting tank 8 and a menthyl acetate collecting tank 9; the reaction separation kettle is provided with a kettle body 3 and a tower body 4 which is positioned above the kettle body 3 and communicated with the kettle body 3; the tower body 4 is communicated with a condensing system 5; the condensing system 5 is also respectively communicated with a pressure reduction system 6, an acetic acid collecting tank 7, a front fraction collecting tank 8 and a menthyl acetate collecting tank 9; the metering system 1 is used for inputting acetic anhydride and menthol into the kettle body 3 before reaction; the temperature control system 2 is used for controlling the temperature of the liquid in the kettle body 3; the reaction separation kettle is used for the reaction of acetic anhydride and menthol, the recovery of acetic acid after the reaction is finished, and the recovery of front distillate and the recovery of menthyl acetate after the recovery of acetic acid; the condensing system 5 is used for the total reflux of the condensed liquid in the reaction process and the partial reflux of the condensed liquid in the subsequent process; a switchable vent 10 is further arranged on a pipeline for communicating the condensing system 5 with the pressure reducing system 6, the vent 10 is in an open state in the reaction process and the acetic acid recovery process, and the vent 10 is in a closed state in the front fraction recovery process and the menthyl acetate recovery process; the pressure reducing system 6 is opened only during the front distillate recovery and the menthyl acetate recovery to maintain the negative pressure in the reaction separation kettle.
Wherein, the production process system is also provided with an acetic anhydride raw material storage tank 11 and a menthol raw material storage tank 12, and the acetic anhydride raw material storage tank 11 and the menthol raw material storage tank 12 are respectively communicated with the metering system 1.
Wherein the metering system 1 is used for inputting acetic anhydride and menthol into the kettle body 3 before reaction, and the metering system 1 is used for inputting the acetic anhydride and the menthol into the kettle body 3 according to the mass ratio of 1: 1.5.
Wherein, cauldron body 3 still is equipped with the leakage fluid dram that can switch, and the leakage fluid dram is the liquid in order to discharge cauldron body 3 for the open mode after the menthyl acetate is retrieved.
Wherein, cauldron body 3 still is equipped with the raw materials entry, and the raw materials entry is located the top of cauldron body 3, and measurement system 1 is connected with the raw materials entry.
Wherein, the tower body 4 is arranged right above the kettle body 3.
Wherein, the temperature control system 2 is also used for controlling the temperature of the gas in the pipeline communicated with the tower body 4 and the condensing system 5.
Wherein the condensing system 5 is arranged above the tower body 4.
Wherein the condensing system 5 is a jacketed condenser, and a cold fluid channel is arranged outside the jacketed condenser; the cold fluid channel is provided with a cooling water inlet and a cooling water outlet.
The use method of the production process system comprises the following steps: mix the back well with acetic anhydride and menthol with certain proportion, send into the cauldron body 3 through measurement system 1 in, the heating is stopped after the liquid heating in the cauldron body 3 of temperature control system 2 reaches the uniform temperature, because exothermic reaction after the reaction initiation, the heat that the reaction produced can make the material in the reaction system (including reactant and result) become steam and rise to condensing system 5, in the automatic reflux to cauldron body 3 after the condensation, this kind of automatic reflux plays a stirring effect, so, the utility model discloses a production technology system need not have the agitator, can make the raw materials misce bene in the reaction sequence promptly. After refluxing for about 4-5 hours, recovering the generated acetic acid at normal pressure, storing the acetic acid in an acetic acid collecting tank 7, starting a pressure reduction system 6, distilling the front cut fraction to a front cut fraction collecting tank 8 under reduced pressure, and continuing distilling under reduced pressure to distill the menthyl acetate into a menthyl acetate collecting tank 9.
Application example 1
Taking a 500-liter kettle body as an example, in the application embodiment, the internal temperature refers to the temperature of liquid in the kettle body, and the top temperature refers to the temperature of gas in a pipeline for communicating the tower body with the condensing system.
The production process system of menthyl acetate of example 1 is adopted, 170 kg of acetic anhydride and 255 kg of menthol are added into the kettle body through the metering system respectively, the temperature control system is started, heating is stopped when the internal temperature reaches 90 ℃, at this time, the reaction is started and boiling reflux occurs, the internal temperature starts to rise, when the internal temperature rises to 145 ℃, the internal temperature does not rise any more, but still keeps the reflux state, and the reflux is continued for 5 hours (if the reaction reflux is not obvious, the temperature control system can be started to heat properly to keep the reflux state). Then, recovering acetic acid under normal pressure, heating to an internal temperature of 190 ℃ (the top temperature is controlled not to exceed 116 ℃), and stopping heating after the amount of the recovered acetic acid is about 92 kilograms, so that the internal temperature is reduced to about 50 ℃. Thereafter, the pressure reducing system was opened to gradually raise the temperature, from which time the internal temperature was 123 ℃ C (top temperature 111 ℃ C.) and the front fraction were collected, and from which time 316.8 kg of menthyl acetate was collected at 124 ℃ C (top temperature 113 ℃ C.).
Effect data
In the above table, the acetic acid yield refers to the ratio of the mass of the obtained acetic acid in the recovery process of acetic acid to the theoretical mass of acetic acid, and the acetic acid purity refers to the purity of the obtained acetic acid in the recovery process of acetic acid; the yield of the menthyl acetate refers to the ratio of the mass of the obtained menthyl acetate in the recovery process of the menthyl acetate to the theoretical mass of the menthyl acetate, and the purity of the menthyl acetate refers to the purity of the obtained menthyl acetate in the recovery process of the menthyl acetate.
Therefore, the utility model discloses a production process system of acetic acid menthyl ester can match the technique that uses menthol and acetic anhydride as raw materials preparation acetic acid menthyl ester that does not add the catalyst, and the reaction all goes on in a reaction separation cauldron with the separation, and need not the washing cauldron, so, can practice thrift and take up an area of, reduces the use of equipment, reduces the equipment investment, has improved the production efficiency of equipment.
Although specific embodiments of the present invention have been described above, it will be understood by those skilled in the art that this is by way of example only and that the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the spirit and the principles of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (9)
1. The production process system of the menthyl acetate is characterized by comprising a metering system, a temperature control system, a reaction separation kettle, a condensing system, a pressure reduction system, an acetic acid collecting tank, a front fraction collecting tank and a menthyl acetate collecting tank; the reaction separation kettle is provided with a kettle body and a tower body which is positioned above the kettle body and communicated with the kettle body; the tower body is communicated with the condensing system; the condensing system is also communicated with the pressure reduction system, the acetic acid collecting tank, the front distillate collecting tank and the menthyl acetate collecting tank respectively; the metering system is used for inputting acetic anhydride and menthol into the kettle body before reaction; the temperature control system is used for controlling the temperature of the liquid in the kettle body; the reaction separation kettle is used for the reaction of acetic anhydride and menthol, the recovery of acetic acid after the reaction is finished, and the recovery of front fraction and the recovery of menthyl acetate after the recovery of acetic acid; the condensation system is used for the total reflux of the condensed liquid in the reaction process and the partial reflux of the condensed liquid in the subsequent process; a pipeline of the condensing system communicated with the pressure reduction system is also provided with a switchable vent, the vent is in an open state in the reaction process and the acetic acid recovery process, and the vent is in a closed state in the front fraction recovery process and the menthyl acetate recovery process; the pressure reduction system is opened only in the processes of front fraction recovery and menthyl acetate recovery so as to maintain the negative pressure in the reaction separation kettle.
2. The system of claim 1, further comprising an acetic anhydride storage tank and a menthol storage tank, wherein the acetic anhydride storage tank and the menthol storage tank are respectively connected to the metering system.
3. The system of claim 1, wherein the tank is further provided with a discharge port that can be opened and closed, and the discharge port is opened after recovery of menthyl acetate to discharge the liquid in the tank.
4. The menthyl acetate production process system of claim 1, wherein the tank body is further provided with a raw material inlet, the raw material inlet is positioned at the top of the tank body, and the metering system is connected with the raw material inlet.
5. The menthyl acetate production process system of claim 1, wherein the tower is located directly above the kettle.
6. The system according to claim 1, wherein the temperature control system is further configured to control the temperature of the gas in a conduit connecting the tower to the condensing system.
7. The menthyl acetate production process system of claim 1, wherein said condensing system is located above said column.
8. The menthyl acetate production process system of claim 1, wherein the condensing system is a jacketed condenser, and the outside of the jacketed condenser is a cold fluid channel.
9. The menthyl acetate production process system of claim 8 wherein said cold fluid channel is provided with a cooling water inlet and a cooling water outlet.
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| CN201922263776.3U CN211255771U (en) | 2019-12-16 | 2019-12-16 | Production process system of menthyl acetate |
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| CN201922263776.3U CN211255771U (en) | 2019-12-16 | 2019-12-16 | Production process system of menthyl acetate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114621090A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Method for preparing methyl propionate by adopting condensation reactor |
| CN114874094A (en) * | 2022-05-05 | 2022-08-09 | 山东新和成药业有限公司 | Method for synthesizing menthyl acetate |
-
2019
- 2019-12-16 CN CN201922263776.3U patent/CN211255771U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114621090A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Method for preparing methyl propionate by adopting condensation reactor |
| CN114621090B (en) * | 2020-12-11 | 2023-08-25 | 中国科学院大连化学物理研究所 | Method for preparing methyl propionate by adopting condensation reactor |
| CN114874094A (en) * | 2022-05-05 | 2022-08-09 | 山东新和成药业有限公司 | Method for synthesizing menthyl acetate |
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Address after: 201416 Shanghai city Fengxian District new economic zone Shen Xinlin Highway No. 559 Patentee after: PuJie flavor (Shanghai) Co.,Ltd. Address before: 201416 Shanghai city Fengxian District new economic zone Shen Xinlin Highway No. 559 Patentee before: SHANGHAI PU-JIE FRAGRANCE Co.,Ltd. |
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