CN111138308B - Chloroamide synthetic reaction system - Google Patents
Chloroamide synthetic reaction system Download PDFInfo
- Publication number
- CN111138308B CN111138308B CN201911051282.7A CN201911051282A CN111138308B CN 111138308 B CN111138308 B CN 111138308B CN 201911051282 A CN201911051282 A CN 201911051282A CN 111138308 B CN111138308 B CN 111138308B
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- CN
- China
- Prior art keywords
- chloroamide
- reaction kettle
- dichloromethane
- metering tank
- kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 62
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 114
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 50
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 10
- GPRQWDZTBQWUAT-UHFFFAOYSA-N 1-tert-butyl-3-ethoxybenzene Chemical compound CCOC1=CC=CC(C(C)(C)C)=C1 GPRQWDZTBQWUAT-UHFFFAOYSA-N 0.000 claims abstract description 9
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 4
- -1 amide acetal Chemical class 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims description 17
- 239000012074 organic phase Substances 0.000 claims description 9
- 239000002351 wastewater Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000005897 Etoxazole Substances 0.000 description 2
- 238000010640 amide synthesis reaction Methods 0.000 description 2
- IXSZQYVWNJNRAL-UHFFFAOYSA-N etoxazole Chemical compound CCOC1=CC(C(C)(C)C)=CC=C1C1N=C(C=2C(=CC=CC=2F)F)OC1 IXSZQYVWNJNRAL-UHFFFAOYSA-N 0.000 description 2
- 230000000895 acaricidal effect Effects 0.000 description 1
- 239000000642 acaricide Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/12—Preparation of carboxylic acid amides by reactions not involving the formation of carboxamide groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A chloroamide synthesis reaction system comprises a hydrochloric acid metering tank, a first dichloromethane metering tank, a second dichloromethane metering tank, an aluminum trichloride preparation kettle, a first chloroamide reaction kettle, a second chloroamide reaction kettle, a water diversion tank and a mortar pump; the top of the first dichloromethane metering tank and the top of the second dichloromethane metering tank are connected with a dichloromethane feeding pipeline, a discharge hole at the bottom of the first dichloromethane metering tank is connected to an aluminum trichloride preparation kettle through a pipeline, the top of the hydrochloric acid metering tank is connected with a hydrochloric acid feeding pipeline and a water conveying pipeline, and the bottom of the hydrochloric acid metering tank is connected to the tops of the first chloroamide reaction kettle and the second chloroamide reaction kettle through a hydrochloric acid conveying pipeline; the tops of the first chloroamide reaction kettle and the second chloroamide reaction kettle are connected with a m-tert-butyl phenetole feeding pipeline and are provided with an amide acetal feeding port. The synthesis reaction system has the advantages of simple structure, high synthesis efficiency, and effectively improved product quality and production efficiency.
Description
Technical Field
The invention relates to the field of chemical reaction equipment, in particular to a chloro-amide synthesis reaction system.
Background
Etoxazole is a novel acaricide with a special structure, and an intermediate of the etoxazole production process is chloramid. The existing chloro-amide synthesis reaction system has complex structure, low synthesis efficiency, and lower product quality and production efficiency.
Disclosure of Invention
The invention aims to provide a chloroamide synthesis reaction system aiming at the defects.
A synthetic reaction system of chloroamide, it includes hydrochloric acid metering tank, first dichloromethane metering tank, second dichloromethane metering tank, aluminium trichloride prepares the cauldron, first chloroamide reaction kettle, second chloroamide reaction kettle, water knockout drum and mortar pump;
the top of the first dichloromethane metering tank and the top of the second dichloromethane metering tank are connected with a dichloromethane feeding pipeline, a discharge port at the bottom of the first dichloromethane metering tank is connected to the aluminum trichloride preparation kettle through a pipeline, an aluminum trichloride feeding port is arranged at the top of the aluminum trichloride preparation kettle, and a discharge port at the bottom of the aluminum trichloride preparation kettle is connected to the first chloroamide reaction kettle and the second chloroamide reaction kettle through an aluminum trichloride solution conveying pipeline; the bottom of the second dichloromethane metering tank is connected with a dichloromethane conveying pipeline, and the dichloromethane conveying pipeline is connected to the first chloroamide reaction kettle and the second chloroamide reaction kettle;
the top of the hydrochloric acid metering tank is connected with a hydrochloric acid feeding pipeline and a water feeding pipeline, and the bottom of the hydrochloric acid metering tank is connected to the tops of the first chloroamide reaction kettle and the second chloroamide reaction kettle through a hydrochloric acid conveying pipeline;
the tops of the first and second chloroamide reaction kettles are connected with a m-tert-butyl phenetole feeding pipeline and provided with an amide acetal feeding port, and the bottoms of the first and second chloroamide reaction kettles are provided with a product discharging port and connected to the water diversion tank through a pipeline;
the inlet end of the mortar pump is connected with the bottom of the water diversion tank through a pipeline, and the outlet end of the mortar pump is connected with the organic phase discharging pipe and the waste water discharging pipe through pipelines.
And heat exchange jackets are arranged outside the first chloroamide reaction kettle and the second chloroamide reaction kettle.
The stirring devices are arranged at the top of the kettle body of the aluminum trichloride preparation kettle, the first chloroamide reaction kettle and the second chloroamide reaction kettle.
And flow control valves are arranged on the aluminum trichloride solution conveying pipeline, the dichloromethane conveying pipeline, the hydrochloric acid conveying pipeline, the m-tert-butyl phenetole conveying pipeline, the organic phase discharging pipe and the wastewater discharging pipe.
The invention has the advantages that: the synthesis reaction system has the advantages of simple structure, high synthesis efficiency, and effectively improved product quality and production efficiency.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
As shown in the attached drawing, the synthesis reaction system of the chloramid comprises a hydrochloric acid metering tank 1, a first dichloromethane metering tank 2, a second dichloromethane metering tank 3, an aluminum trichloride preparation kettle 4, a first chloramid reaction kettle 5, a second chloramid reaction kettle 6, a water diversion tank 7 and a mortar pump 8;
the tops of the first dichloromethane metering tank 2 and the second dichloromethane metering tank 3 are connected with a dichloromethane feeding pipeline 9, the discharge port at the bottom of the first dichloromethane metering tank 2 is connected to the aluminum trichloride preparation kettle 4 through a pipeline, an aluminum trichloride feed port 10 is arranged at the top of the aluminum trichloride preparation kettle 4, and the discharge port at the bottom of the aluminum trichloride preparation kettle 4 is connected to the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6 through an aluminum trichloride solution conveying pipeline 11; the bottom of the second dichloromethane metering tank 3 is connected with a dichloromethane conveying pipeline 12, and the dichloromethane conveying pipeline 12 is connected to the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6;
the top of the hydrochloric acid metering tank 1 is connected with a hydrochloric acid feeding pipeline 13 and a water feeding pipeline 20, and the bottom of the hydrochloric acid metering tank 1 is connected to the tops of the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6 through a hydrochloric acid conveying pipeline 14;
the tops of the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6 are connected with a m-tert-butyl phenetole feeding pipeline 15 and provided with an amide acetal feeding port 16, and the bottoms of the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6 are provided with a product discharging port and connected to the water diversion tank 7 through pipelines;
the inlet end of the mortar pump 8 is connected with the bottom of the water diversion tank 7 through a pipeline, and the outlet end is connected with the organic phase discharging pipe 17 and the wastewater discharging pipe 18 through pipelines.
And heat exchange jackets 19 are arranged outside the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6.
The stirring devices are arranged at the top of the kettle body of the aluminum trichloride preparation kettle 4, the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6.
The aluminum trichloride solution conveying pipeline 11, the dichloromethane conveying pipeline 12, the hydrochloric acid conveying pipeline 14, the m-tert-butyl phenetole conveying pipeline 15, the organic phase discharging pipe 17 and the waste water discharging pipe 18 are all provided with flow control valves.
Working principle: the first chloroamide reaction kettle 5 and the second chloroamide reaction kettle 6 respectively receive dichloromethane conveyed by the second dichloromethane metering tank 3, m-tert-butyl phenetole conveyed by the m-tert-butyl phenetole conveying pipeline 15 and the prepared aluminum trichloride solution conveyed by the aluminum trichloride preparation kettle 4, then a stirring device is started to react, the reaction temperature in the reaction kettle is regulated through a heat exchange jacket, after the reaction is completed, the hydrochloric acid solution conveyed by the hydrochloric acid metering tank 1 is added, after the reaction is completed, the product is conveyed into the water diversion tank 7 to separate an organic phase from wastewater, and then the organic phase and the wastewater are conveyed and discharged through an organic phase discharging pipe 17 and a wastewater discharging pipe 18 respectively through a mortar pump 8. The synthesis reaction system has the advantages of simple structure, high synthesis efficiency, and effectively improved product quality and production efficiency.
Claims (1)
1. The chloramid synthesis reaction system is characterized by comprising a hydrochloric acid metering tank (1), a first dichloromethane metering tank (2), a second dichloromethane metering tank (3), an aluminum trichloride preparation kettle (4), a first chloramid reaction kettle (5), a second chloramid reaction kettle (6), a water diversion tank (7) and a mortar pump (8);
the top of the first dichloromethane metering tank (2) and the top of the second dichloromethane metering tank (3) are connected with a dichloromethane feeding pipeline (9), a discharge hole at the bottom of the first dichloromethane metering tank (2) is connected to the aluminum trichloride configuration kettle (4) through a pipeline, an aluminum trichloride feeding hole (10) is formed in the top of the aluminum trichloride configuration kettle (4), and the discharge hole at the bottom of the aluminum trichloride configuration kettle (4) is connected to the first chloroamide reaction kettle (5) and the second chloroamide reaction kettle (6) through an aluminum trichloride solution conveying pipeline (11); the bottom of the second dichloromethane metering tank (3) is connected with a dichloromethane conveying pipeline (12), and the dichloromethane conveying pipeline (12) is connected to the first chloroamide reaction kettle (5) and the second chloroamide reaction kettle (6);
the top of the hydrochloric acid metering tank (1) is connected with a hydrochloric acid feeding pipeline (13) and a water feeding pipeline (20), and the bottom of the hydrochloric acid metering tank (1) is connected to the tops of the first chloroamide reaction kettle (5) and the second chloroamide reaction kettle (6) through a hydrochloric acid conveying pipeline (14);
the tops of the first chloroamide reaction kettle (5) and the second chloroamide reaction kettle (6) are connected with a m-tert-butyl phenetole feeding pipeline (15) and provided with an amide acetal feeding port (16), and the bottoms of the first chloroamide reaction kettle (5) and the second chloroamide reaction kettle (6) are provided with product discharging ports and are connected to the water diversion tank (7) through pipelines;
the inlet end of the mortar pump (8) is connected with the bottom of the water diversion tank (7) through a pipeline, and the outlet end of the mortar pump is connected with the organic phase discharging pipe (17) and the wastewater discharging pipe (18) through pipelines;
the outside of the first chloroamide reaction kettle (5) and the second chloroamide reaction kettle (6) is provided with a heat exchange jacket (19);
the aluminum trichloride preparing kettle (4), the first chloroamide reaction kettle (5) and the second chloroamide reaction kettle (6) are provided with stirring devices at the top parts of the kettle bodies;
the device is characterized in that flow control valves are arranged on the aluminum trichloride solution conveying pipeline (11), the dichloromethane conveying pipeline (12), the hydrochloric acid conveying pipeline (14), the m-tert-butyl phenetole conveying pipeline (15), the organic phase discharging pipe (17) and the wastewater discharging pipe (18).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911051282.7A CN111138308B (en) | 2019-10-31 | 2019-10-31 | Chloroamide synthetic reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911051282.7A CN111138308B (en) | 2019-10-31 | 2019-10-31 | Chloroamide synthetic reaction system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111138308A CN111138308A (en) | 2020-05-12 |
| CN111138308B true CN111138308B (en) | 2024-01-30 |
Family
ID=70516920
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911051282.7A Active CN111138308B (en) | 2019-10-31 | 2019-10-31 | Chloroamide synthetic reaction system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111138308B (en) |
-
2019
- 2019-10-31 CN CN201911051282.7A patent/CN111138308B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| 几个重要杀虫剂的合成;程志明;;今日农药(09);第17-21页 * |
| 除螨剂乙螨唑的合成研究;朱龙;;科技创新与生产力(11);第109-111页 * |
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| Publication number | Publication date |
|---|---|
| CN111138308A (en) | 2020-05-12 |
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