CN218357425U - Device for producing cyhaloacid by continuous cyclization desolventizing of lifting film - Google Patents
Device for producing cyhaloacid by continuous cyclization desolventizing of lifting film Download PDFInfo
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- CN218357425U CN218357425U CN202221706730.XU CN202221706730U CN218357425U CN 218357425 U CN218357425 U CN 218357425U CN 202221706730 U CN202221706730 U CN 202221706730U CN 218357425 U CN218357425 U CN 218357425U
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- cauldron
- cyclization
- kettle
- film evaporator
- saponification
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Abstract
The utility model relates to a chemical synthesis technical field, concretely relates to with continuous cyclization desolventizing production kungfu sour device of lift membrane, including addition cauldron, cyclization cauldron, saponification cauldron and acidizing cauldron, addition cauldron and cyclization cauldron intercommunication, the cyclization cauldron is through climbing-film evaporator, separator, falling-film evaporator and saponification cauldron intercommunication in proper order, saponification cauldron and acidizing cauldron intercommunication. The utility model discloses after using the lift film evaporation ware to replace desolventizing cauldron, equipment cost, maintenance cost and energy consumption etc. have been practiced thrift greatly.
Description
Technical Field
The utility model relates to a chemical synthesis technical field, concretely relates to produce sour device of time with continuous cyclization exsolution of lift membrane.
Background
The production route of the cyhalothrin is generally that cuprous chloride and monoethanolamine are added into a tert-butyl alcohol solution to carry out positive pressure reaction to generate an addition product of chlorofluoromethyl, then the addition product is subjected to cyclization reaction with potassium tert-butoxide in a mixed solution of DMF and tert-butyl alcohol to generate a cyclic compound 1R, 3cis-dichlorofluthrin, the cyclic compound is subjected to hydrolysis dechlorination (commonly known as saponification) reaction with a KOH aqueous solution, and finally, the cyhalothrin is obtained by using inorganic acid to carry out acidification.
At the present stage, the cyclization procedure mostly adopts batch type equipment such as desolventizing kettles and the like for production, the equipment quantity is large, the operation safety coefficient is low, and the adverse conditions of high energy consumption, low yield and the like exist.
SUMMERY OF THE UTILITY MODEL
To the many, the factor of safety low grade technical problem of equipment quantity that use desolventizing cauldron to exist in the sour production cyclization process of kungfu, the utility model provides a device with sour production kungfu of lift membrane continuous cyclization desolventizing uses the lift film evaporation ware to replace after the desolventizing cauldron, has practiced thrift equipment cost, maintenance cost and energy consumption etc. greatly.
The technical scheme of the utility model as follows:
the utility model provides a device for producing cyhalofugic acid with continuous cyclization desolvation of lift membrane, includes addition cauldron, cyclization cauldron, saponification cauldron and acidizing cauldron, addition cauldron and cyclization cauldron intercommunication, the cyclization cauldron is in proper order through climbing film evaporator, separator, falling film evaporator and saponification cauldron intercommunication, saponification cauldron and acidizing cauldron intercommunication.
Further, the circulating reactor also comprises a metering tank, and the circulating reactor is communicated with the climbing film evaporator through the metering tank.
Further, the device also comprises a tert-butyl alcohol recovery tank, and the separator is communicated with the tert-butyl alcohol recovery tank.
Further, the separator is communicated with the tert-butyl alcohol recovery tank through a first cooling device and a first separation device in sequence.
Further, the device also comprises a DMF recovery tank, and the falling-film evaporator is communicated with the DMF recovery tank.
Further, the falling-film evaporator is communicated with the DMF recovery tank through a second cooling device and a second separation device in sequence.
Further, the device also comprises a cyclic compound receiving tank, and the falling film evaporator is communicated with the saponification kettle through the cyclic compound receiving tank.
The beneficial effects of the utility model reside in that:
the device adopts the climbing-film evaporator and the falling-film evaporator to replace a desolventizing kettle, firstly, the tertiary butanol is separated out through the climbing-film evaporator, then, DMF is separated out through the falling-film evaporator, and finally, the desolventizing and rising of the cyclopolymer are realized; the falling film evaporator can continuously desolventize, realize automatic control, reduce personnel; the production efficiency of the kungfu acid is improved, the yield is improved, the operation parameters are reduced, and the safety factor is increased; the floor area is small, the equipment quantity is small, the investment is reduced, and the later-stage equipment maintenance cost is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of the structure of the apparatus of embodiment 1.
In the figure, 1-addition kettle, 2-cyclization kettle, 3-metering tank, 4-climbing-film evaporator, 5-separator, 6-first cooling device, 7-first separation device, 8-tert-butyl alcohol recovery tank, 9-falling-film evaporator, 10-second cooling device, 11-second separation device, 12-DMF recovery tank, 13-cyclic compound receiving tank, 14-saponification kettle, and 15-acidification kettle.
Detailed Description
In order to make the technical solutions in the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts shall belong to the protection scope of the present invention.
Example 1
A device for producing cyhalothric acid by using a lifting membrane to continuously cyclize and desolventize comprises an addition kettle 1, a cyclization kettle 2, a metering tank 3, a climbing-film evaporator 4, a separator 5, a first cooling device 6, a first separation device 7, a tert-butyl alcohol recovery tank 8, a falling-film evaporator 9, a second cooling device 10, a second separation device 11, a DMF (dimethyl formamide) recovery tank 12, a cyclics receiving tank 13, a saponification kettle 14 and an acidification kettle 15, wherein the addition kettle 1 is communicated with the cyclization kettle 2, the cyclization kettle 2 is communicated with the saponification kettle 14 through the metering tank 3, the climbing-film evaporator 4, the separator 5, the falling-film evaporator 9 and the cyclics receiving tank 13 in sequence, and the saponification kettle 14 is communicated with the acidification kettle 15;
the separator 5 is also communicated with a tertiary butanol recovery tank 8 through a first cooling device 6 and a first separation device 7 in sequence;
the falling-film evaporator 9 is also communicated with the DMF recovery tank 2 through a second cooling device 10 and a second separation device 11 in sequence.
The working principle of the device is as follows:
reacting raw materials in an addition kettle to form an addition product, then feeding the addition product into a cyclization kettle to perform cyclization reaction with potassium tert-butoxide to obtain a cyclization product, wherein the cyclization product flows out of the cyclization kettle, is metered by a metering tank and then enters a climbing film evaporator, the temperature is controlled to be about 85 ℃, tert-butyl alcohol in the cyclization product is separated under normal pressure, and the part of tert-butyl alcohol is cooled, subjected to gas-liquid separation, then fed into a tert-butyl alcohol recovery tank for temporary storage, dried and recycled; then the cyclic compound enters a falling film evaporator, the temperature is controlled to be about 120 ℃, the pressure is controlled to be about-0.098 Mpa, DMF in the cyclic compound is separated, and the part of DMF enters a DMF recovery tank for recycling after being cooled and separated; the remaining cyclic compound enters a cyclic compound receiving tank and is used for subsequent saponification and acidification treatments. According to actual needs, the first cooling device and the second cooling device can be provided as a plurality of sets of series or parallel coolers, and the first separation device and the second separation device can be provided as a plurality of sets of series or parallel gas-liquid separators.
The device uses one climbing-film evaporator and one falling-film evaporator to replace fifteen original 6300L desolventizing kettles, the occupied area is reduced by 60 percent, and the yield is improved by 50 percent.
Although the present invention has been described in detail by referring to the drawings in conjunction with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and substance of the present invention, and these modifications or substitutions are intended to be included within the scope of the present invention/any person skilled in the art can easily think of changes or substitutions within the technical scope of the present invention.
Claims (7)
1. The device for producing the cyhalothrin acid by using the lifting film continuous cyclization desolventizing is characterized by comprising an addition kettle, a cyclization kettle, a saponification kettle and an acidification kettle, wherein the addition kettle is communicated with the cyclization kettle, the cyclization kettle is communicated with the saponification kettle sequentially through a lifting film evaporator, a separator and a falling film evaporator, and the saponification kettle is communicated with the acidification kettle.
2. The apparatus of claim 1, further comprising a metering tank, wherein the cyclization tank is in communication with the rising film evaporator via the metering tank.
3. The apparatus of claim 1, further comprising a tertiary butanol recovery tank, the separator in communication with the tertiary butanol recovery tank.
4. The apparatus of claim 3, wherein the separator is in communication with a tertiary butanol recovery tank through a first cooling device, a first separation device, in that order.
5. The apparatus of claim 1, further comprising a DMF recovery tank, the falling film evaporator being in communication with the DMF recovery tank.
6. The apparatus of claim 5, wherein the falling film evaporator is in communication with the DMF recovery tank via the second cooling means and the second separating means in that order.
7. The apparatus of claim 1, further comprising an annulus receiving tank, wherein the falling film evaporator is in communication with the saponification vessel through the annulus receiving tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221706730.XU CN218357425U (en) | 2022-07-04 | 2022-07-04 | Device for producing cyhaloacid by continuous cyclization desolventizing of lifting film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221706730.XU CN218357425U (en) | 2022-07-04 | 2022-07-04 | Device for producing cyhaloacid by continuous cyclization desolventizing of lifting film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN218357425U true CN218357425U (en) | 2023-01-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202221706730.XU Active CN218357425U (en) | 2022-07-04 | 2022-07-04 | Device for producing cyhaloacid by continuous cyclization desolventizing of lifting film |
Country Status (1)
| Country | Link |
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| CN (1) | CN218357425U (en) |
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2022
- 2022-07-04 CN CN202221706730.XU patent/CN218357425U/en active Active
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