CN112661601A - Continuous production equipment for trifluoro monochloro chrysanthemic acid - Google Patents
Continuous production equipment for trifluoro monochloro chrysanthemic acid Download PDFInfo
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- CN112661601A CN112661601A CN202011639961.9A CN202011639961A CN112661601A CN 112661601 A CN112661601 A CN 112661601A CN 202011639961 A CN202011639961 A CN 202011639961A CN 112661601 A CN112661601 A CN 112661601A
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- Prior art keywords
- pipeline
- tank
- rectifying tower
- loop reactor
- heat exchanger
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- 238000010924 continuous production Methods 0.000 title claims abstract description 20
- XLOPRKKSAJMMEW-SFYZADRCSA-N Chrysanthemic acid Natural products CC(C)=C[C@@H]1[C@@H](C(O)=O)C1(C)C XLOPRKKSAJMMEW-SFYZADRCSA-N 0.000 title claims abstract description 18
- XLOPRKKSAJMMEW-UHFFFAOYSA-N chrysanthemic acid Chemical compound CC(C)=CC1C(C(O)=O)C1(C)C XLOPRKKSAJMMEW-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000010410 layer Substances 0.000 claims description 8
- 239000000523 sample Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 5
- 239000011229 interlayer Substances 0.000 claims description 3
- 239000012809 cooling fluid Substances 0.000 claims 4
- 239000004078 cryogenic material Substances 0.000 claims 1
- 230000003247 decreasing effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000000110 cooling liquid Substances 0.000 description 10
- 239000002826 coolant Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000008676 import Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 description 2
- BOSAWIQFTJIYIS-UHFFFAOYSA-N 1,1,1-trichloro-2,2,2-trifluoroethane Chemical compound FC(F)(F)C(Cl)(Cl)Cl BOSAWIQFTJIYIS-UHFFFAOYSA-N 0.000 description 1
- -1 2, 2-dichloro-3, 3, 3-trifluoropropyl Chemical group 0.000 description 1
- SPVZAYWHHVLPBN-UHFFFAOYSA-N 3-(2-chloro-3,3,3-trifluoroprop-1-en-1-yl)-2,2-dimethylcyclopropanecarboxylic acid Chemical compound CC1(C)C(C=C(Cl)C(F)(F)F)C1C(O)=O SPVZAYWHHVLPBN-UHFFFAOYSA-N 0.000 description 1
- 239000005874 Bifenthrin Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OMFRMAHOUUJSGP-IRHGGOMRSA-N bifenthrin Chemical compound C1=CC=C(C=2C=CC=CC=2)C(C)=C1COC(=O)[C@@H]1[C@H](\C=C(/Cl)C(F)(F)F)C1(C)C OMFRMAHOUUJSGP-IRHGGOMRSA-N 0.000 description 1
- VEMKTZHHVJILDY-UXHICEINSA-N bioresmethrin Chemical compound CC1(C)[C@H](C=C(C)C)[C@H]1C(=O)OCC1=COC(CC=2C=CC=CC=2)=C1 VEMKTZHHVJILDY-UXHICEINSA-N 0.000 description 1
- 230000000747 cardiac effect Effects 0.000 description 1
- JREFYCQLWZTPLE-UHFFFAOYSA-N chloro 2,2,2-trifluoroacetate Chemical compound FC(F)(F)C(=O)OCl JREFYCQLWZTPLE-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
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Abstract
The invention relates to continuous production equipment of trifluoro monochloro chrysanthemic acid, which comprises a material mixing tank (1), a reaction tank (2), a first rectifying tower (3), a heat exchanger (4), a loop reactor (5), a buffer tank (6), a second rectifying tower (7), a tubular reactor (8) and an extraction tank (9). According to the invention, the heat exchange is carried out between the hot material from the first rectifying tower and the material from the cold loop reactor, so that the heat in the first-step rectifying tower is effectively utilized, and meanwhile, the use of one heat exchanger is reduced, the production cost is reduced, the space is saved, and the production efficiency is improved. The hot gas exhausted from the tops of the two rectifying towers passes through the buffer tank, so that the further preheating of the substances in the buffer tank is realized, and the heat in the whole set of equipment is effectively utilized.
Description
Technical Field
The invention relates to the technical field of chemical equipment, in particular to continuous production equipment of trifluoro monochloro chrysanthemic acid.
Background
Trifluoro-monochloro chrysanthemic acid is called cyhalothrin, the chemical name of which is 3- (2-chloro-3, 3, 3-trifluoro-propen-1-yl) -2, 2-dimethyl cyclopropane carboxylic acid, and is an important intermediate of pyrethroids such as cyhalothrin, bifenthrin, heptafluoropenthrin, heptafluoromethyl ether and the like. The structural formula is as follows:
the methyl ester of cardiac acid and trifluoro trichloroethane are used as initial raw materials to prepare 3, 3-dimethyl-4, 6, 6-trichloro-7, 7, 7-trifluoro heptanoate through addition reaction; then the cis-trans-3- (2, 2-dichloro-3, 3, 3-trifluoropropyl) -2, 2-dimethyl cyclic carboxylate is prepared by cyclization reaction of the cis-trans-3- (2, 2-dichloro-3, 3, 3-trifluoropropyl) -potassium tert-butoxide; finally, the 3- (2-chlorine-3, 3, 3-trifluoro-propylene-1-group) -2, 2-dimethyl cyclopropane carboxylic acid, namely trifluoro monochloro chrysanthemic acid, is produced by saponification reaction with potassium hydroxide.
Although the existing continuous production equipment for the monochlorotrifluoroanthemic acid realizes the continuous production of the monochlorotrifluoroanthemic acid, the existing continuous production equipment is not enough to save space and is inconvenient for effectively utilizing materials and heat. Therefore, the invention designs the continuous production equipment of the monochlorotrifluoroethanoic acid, which saves space and is convenient for effectively utilizing heat.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides continuous production equipment of trifluoro monochloro chrysanthemic acid, and the specific technical scheme is as follows:
a continuous production device of trifluoro monochloro chrysanthemic acid comprises a material mixing tank (1), a reaction tank (2), a first rectifying tower (3), a heat exchanger (4), a loop reactor (5), a buffer tank (6), a second rectifying tower (7), a tubular reactor (8) and an extraction tank (9),
the material mixing tank (1) is connected with the reaction tank (2) through a pipeline, the bottom end of the reaction tank (2) is connected with the first rectifying tower (3) through a pipeline, the bottom end of the first rectifying tower (3) is connected with a hot liquid inlet of the heat exchanger (4) through a pipeline, a hot liquid outlet of the heat exchanger (4) is connected with the loop reactor (5) through a pipeline, the discharge hole of the loop reactor (5) is connected with the first cold liquid inlet of the heat exchanger (4) through a pipeline, the first cold liquid outlet of the heat exchanger (4) is connected with the buffer tank (6) through a pipeline, the buffer tank (6) is connected with the second rectifying tower (7) through a pipeline, the second rectifying tower (7) is connected with the tubular reactor (8) through a pipeline, the liquid outlet of the tubular reactor (8) is connected with the extraction tank (9) through a pipeline, and the material discharged from the extraction tank (9) is the liquid of the monochlorotrifluoroanthemic acid.
Furthermore, the heat exchanger (4) comprises a first cooling liquid pipeline (401) and a second cooling liquid pipeline (402), common cooling oil is introduced into the second cooling liquid pipeline (402), and low-temperature materials discharged from the loop reactor are introduced into the first cooling liquid pipeline (401).
Further, the outer wall of loop reactor (5) on be provided with coolant oil intermediate layer (501), inlet and the liquid outlet of coolant oil intermediate layer (501) pass through the pipeline and be connected with cooling oil tank (502), be provided with measuring pump (503) on the pipeline, be convenient for the loop reactor cooling, loop reactor (5) inside be provided with a plurality of temperature monitoring probe (504), temperature detecting probe (504) and measuring pump (503) all be connected with automatic control device through the pipeline, guarantee that the temperature in the loop reactor is even.
Furthermore, the outer wall of the buffer tank (6) is provided with a heat insulation layer (601) to prevent the temperature of the heated material from being reduced in low-temperature weather.
Further, buffer tank (6) in be provided with two heating tube way (602), the import of a heating tube way is connected with the upper end gas outlet of first rectifying tower (3), the import of another heating tube way is connected with the gas outlet of second rectifying tower (7), further heats the material in buffer tank (6), realizes thermal effective utilization.
The invention has the beneficial effects that: the invention relates to 3 non-reactions, wherein one step of reaction is carried out in a cold loop reactor, and materials discharged from the loop reactor need to be heated and then enter a rectifying tower for rectification, and finally, the trifluoro monochloro chrysanthemic acid is obtained. According to the invention, the heat exchange is carried out between the hot material from the first rectifying tower and the material from the cold loop reactor, so that the heat in the first-step rectifying tower is effectively utilized, and meanwhile, the use of one heat exchanger is reduced, the production cost is reduced, the space is saved, and the production efficiency is improved.
The hot gas exhausted from the tops of the two rectifying towers passes through the buffer tank, so that the further preheating of the substances in the buffer tank is realized, and the heat in the whole set of equipment is effectively utilized.
Drawings
FIG. 1 is a schematic structural diagram of a continuous production apparatus for trifluoro monochloro chrysanthemic acid according to an embodiment of the present invention.
FIG. 2 is a schematic structural diagram of a loop reactor of a continuous production apparatus for trifluoro monochloro chrysanthemic acid according to an embodiment of the present invention.
FIG. 3 is a schematic diagram showing a detailed structure of a section of a loop reactor of a continuous production apparatus of chlorotrifluoro-chrysanthemic acid according to an embodiment of the present invention.
Fig. 4 is a schematic structural diagram of a buffer tank of a continuous production apparatus of trifluoro monochloro chrysanthemic acid in an embodiment of the present invention.
The method comprises the following steps of 1-a material mixing tank, 2-a reaction tank, 3-a first rectifying tower, 4-a heat exchanger, 401-a first cooling liquid pipeline, 402-a second cooling liquid pipeline, 5-a loop reactor, 501-a cooling oil interlayer, 502-a cooling oil tank, 503-a metering pump, 504-a temperature detection probe, 6-a buffer tank, 601-a heat insulation layer, 602-a heating pipeline, 7-a second rectifying tower, 8-a tubular reactor and 9-an extraction tank.
The specific implementation mode is as follows:
for the purpose of promoting an understanding of the invention, reference will now be made in detail to the embodiments of the invention illustrated in the accompanying drawings.
It should be understood that the structures, ratios, sizes, and the like shown in the drawings and described in the specification are only used for matching with the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions under which the present invention can be implemented, so that the present invention has no technical significance, and any structural modification, ratio relationship change, or size adjustment should still fall within the scope of the present invention without affecting the efficacy and the achievable purpose of the present invention.
Examples
With reference to figures 1 to 4 of the drawings,
a continuous production device of trifluoro monochloro chrysanthemic acid comprises a material mixing tank 1, a reaction tank 2, a first rectifying tower 3, a heat exchanger 4, a loop reactor 5, a buffer tank 6, a second rectifying tower 7, a tubular reactor 8 and an extraction tank 9,
the material mixing tank 1 is connected with the reaction tank 2 through a pipeline, the bottom end of the reaction tank 2 is connected with the first rectifying tower 3 through a pipeline, the bottom end of the first rectifying tower 3 is connected with a hydrothermal solution inlet of the heat exchanger 4 through a pipeline, a hydrothermal solution outlet of the heat exchanger 4 is connected with the loop reactor 5 through a pipeline, a discharge port of the loop reactor 5 is connected with a first cold solution inlet of the heat exchanger 4 through a pipeline, a first cold solution outlet of the heat exchanger 4 is connected with the buffer tank 6 through a pipeline, the buffer tank 6 is connected with the second rectifying tower 7 through a pipeline, the second rectifying tower 7 is connected with the tubular reactor 8 through a pipeline, a liquid outlet of the tubular reactor 8 is connected with the extraction tank 9 through a pipeline, and the material discharged from the extraction tank 9 is trifluoro monochloro chrysanthemic acid liquid.
Further, the heat exchanger 4 comprises a first cooling liquid pipeline 401 and a second cooling liquid pipeline 402, wherein common cooling oil is introduced into the second cooling liquid pipeline 402, and the low-temperature material from the loop reactor is introduced into the first cooling liquid pipeline 401.
Further, be provided with coolant oil intermediate layer 501 on the outer wall of loop reactor 5, coolant oil intermediate layer 501's inlet and liquid outlet pass through the pipeline and are connected with cooling oil tank 502, are provided with measuring pump 503 on the pipeline, are convenient for cool down for loop reactor, and loop reactor 5 is inside to be provided with a plurality of temperature monitoring probe 504, and temperature monitoring probe 504 and measuring pump 503 all are connected with automatic control device through the pipeline, guarantee that the temperature in the loop reactor is even.
Further, the outer wall of the buffer tank 6 is provided with a heat insulation layer 601, so that the temperature of the material after temperature rise is prevented from being reduced in low-temperature weather.
Further, be provided with two heating tube 602 in the buffer tank 6, the import of a heating tube is connected with the upper end gas outlet of first rectifying column 3, and the import of another heating tube is connected with the gas outlet of second rectifying column 7, further heats the material in the buffer tank 6, realizes thermal effective utilization.
The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and also comprise the technical scheme formed by equivalent replacement of the technical features. The present invention is not limited to the details given herein, but is within the ordinary knowledge of those skilled in the art.
Claims (5)
1. A continuous production device of trifluoro monochloro chrysanthemic acid is characterized by comprising a material mixing tank (1), a reaction tank (2), a first rectifying tower (3), a heat exchanger (4), a loop reactor (5), a buffer tank (6), a second rectifying tower (7), a tubular reactor (8) and an extraction tank (9),
the material mixing tank (1) is connected with the reaction tank (2) through a pipeline, the bottom end of the reaction tank (2) is connected with the first rectifying tower (3) through a pipeline, the bottom end of the first rectifying tower (3) is connected with a hot liquid inlet of the heat exchanger (4) through a pipeline, a hot liquid outlet of the heat exchanger (4) is connected with the loop reactor (5) through a pipeline, the discharge hole of the loop reactor (5) is connected with the first cold liquid inlet of the heat exchanger (4) through a pipeline, the first cold liquid outlet of the heat exchanger (4) is connected with the buffer tank (6) through a pipeline, the buffer tank (6) is connected with the second rectifying tower (7) through a pipeline, the second rectifying tower (7) is connected with the tubular reactor (8) through a pipeline, the liquid outlet of the tubular reactor (8) is connected with the extraction tank (9) through a pipeline, and the material discharged from the extraction tank (9) is the liquid of the monochlorotrifluoroanthemic acid.
2. A plant for the continuous production of trifluoro-monochloro-chrysanthemic acid according to claim 1, characterized in that said heat exchanger (4) comprises a first cooling fluid conduit (401) and a second cooling fluid conduit (402), said second cooling fluid conduit (402) being fed with a common cooling oil, said first cooling fluid conduit (401) being fed with the cryogenic material coming out of the loop reactor.
3. The continuous production equipment of trifluoro monochloro chrysanthemic acid according to claim 1, characterized in that, the outer wall of the loop reactor (5) is provided with a cooling oil interlayer (501), the liquid inlet and the liquid outlet of the cooling oil interlayer (501) are connected with a cooling oil tank (502) through a pipeline, a metering pump (503) is arranged on the pipeline, which is convenient for cooling the loop reactor, a plurality of temperature monitoring probes (504) are arranged inside the loop reactor (5), and the temperature monitoring probes (504) and the metering pump (503) are both connected with an automatic control device through a pipeline, thereby ensuring the uniform temperature inside the loop reactor.
4. The continuous production equipment of trifluoro monochloro chrysanthemic acid according to claim 1, characterized in that the outer wall of the buffer tank (6) is provided with an insulating layer (601) to prevent the temperature of the material from decreasing after the temperature is raised in low temperature weather.
5. The continuous production equipment of the trifluoro monochloro chrysanthemic acid according to claim 2, characterized in that, two heating pipelines (602) are arranged in the buffer tank (6), the inlet of one heating pipeline is connected with the upper end gas outlet of the first rectifying tower (3), the inlet of the other heating pipeline is connected with the gas outlet of the second rectifying tower (7), and the materials in the buffer tank (6) are further heated, so as to realize the effective utilization of heat.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011639961.9A CN112661601A (en) | 2020-12-31 | 2020-12-31 | Continuous production equipment for trifluoro monochloro chrysanthemic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011639961.9A CN112661601A (en) | 2020-12-31 | 2020-12-31 | Continuous production equipment for trifluoro monochloro chrysanthemic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112661601A true CN112661601A (en) | 2021-04-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011639961.9A Pending CN112661601A (en) | 2020-12-31 | 2020-12-31 | Continuous production equipment for trifluoro monochloro chrysanthemic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112661601A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503582A (en) * | 2014-09-23 | 2016-04-20 | 连云港市华通化学有限公司 | Continuous production method for trifluoro monochloro chrysanthemic acid |
| CN214830025U (en) * | 2020-12-31 | 2021-11-23 | 南京伟鑫生物医药有限公司 | Continuous production equipment for trifluoro monochloro chrysanthemic acid |
-
2020
- 2020-12-31 CN CN202011639961.9A patent/CN112661601A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503582A (en) * | 2014-09-23 | 2016-04-20 | 连云港市华通化学有限公司 | Continuous production method for trifluoro monochloro chrysanthemic acid |
| CN214830025U (en) * | 2020-12-31 | 2021-11-23 | 南京伟鑫生物医药有限公司 | Continuous production equipment for trifluoro monochloro chrysanthemic acid |
Non-Patent Citations (1)
| Title |
|---|
| 何相助 等: "企业合理用能诊断", 湖南科学技术出版社, pages: 107 * |
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