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Continuous reaction device and production method used for producing 3,8-dimethyl-7-chloroquinoline via oxidative cyclisation

A reaction device, dimethyl technology, applied in the direction of organic chemistry, etc., to achieve the effect of increasing yield, increasing product yield, and quality assurance

Inactive Publication Date: 2015-10-14
中农发河南农化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a continuous reaction device and its production method for the legal production of 3,8-dimethyl-7-chloroquinoline by oxidation ring in view of the deficiencies of the existing intermittent production methods

Method used

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  • Continuous reaction device and production method used for producing 3,8-dimethyl-7-chloroquinoline via oxidative cyclisation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] ① Add 412kg of water from the water head tank to the synthesis kettle, open the still circulating water, and add 2484kg from the sulfuric acid head tank (to make about 80% sulfuric acid solution). Control the temperature below 100°C.

[0049] ② Add 650kg of aniline from the aniline high tank, control the temperature at about 100 degrees, and stir for 30 minutes. ③ Add 14kg of catalyst from the sampling port.

[0050] ④ Turn on the steam and heat up to 110°C, start to add 540kg of aldehyde dropwise. During the dropwise addition, the system temperature should not be lower than 130°C. ) content of 0.29%, 3.8-dimethyl-7-chloroquinoline 95.89%. After the reaction is qualified (aniline<0.3%), special attention should be paid to discharging in batches, and the temperature of discharging should be kept between 100-110°C.

Embodiment 2

[0052] ① Add 412kg of water from the head tank to the synthesis kettle, turn on the circulating water, and add 2484kg from the head tank of sulfuric acid (to make about 80% sulfuric acid solution). Control the temperature below 100°C.

[0053] ② Add 650kg of aniline from the aniline high tank, control the temperature at about 100 degrees, and stir for 30 minutes.

[0054] ③ Add 14kg of catalyst 1 from the sampling port.

[0055] ④ Turn on the steam and heat up to 110°C, start to add 540kg of aldehyde dropwise, the temperature of the system should not be lower than 120°C during the dropwise addition, after the dropwise addition, keep the temperature for 1 hour, take a sample for analysis, and analyze 2-methyl-3-chloroaniline (7502 ) content of 0.26%, 3.8-dimethyl-7-chloroquinoline 95.89%. After the reaction is qualified (aniline<0.3%), special attention should be paid to discharging in batches, and the temperature of discharging should be kept between 100-110°C.

[0056] [Af...

Embodiment 3

[0058] Start the metering pump, control the flow rate of 154kg / h to inject 2-methyl-3-chloroaniline into the batching kettle, control the flow rate of 10kg / h to add water once to the batching kettle, start stirring, and use the weighing module to control the system with 1.23kg Add the oxidant quantitatively into the kettle at a decreasing rate of / h to make a mixed solution. When the liquid level in the batching tank is about 50%, the mixed liquid is only exported.

[0059] Open the inlet and outlet valves of the circulating water of the static mixer, the steam of the gas-liquid separator and its steam trap; start the inlet and outlet valves of the heat transfer oil of the tubular continuous reactor and the separator, and start the vacuum system for exhaust gas absorption to make the separator reach a certain level. The vacuum (the first stage is 0.03MPa, the second stage reaches -0.05MPa), and the exhaust gas absorption system is started.

[0060] Open the fresh water valve ...

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Abstract

The invention discloses a continuous reaction device and a production method used for producing 3,8-dimethyl-7-chloroquinoline via oxidative cyclisation. The continuous reaction device composed via combination of a gas-liquid separator and pipeline reactors is applied to industrial production with gas generation, and excellent effect is achieved. Pipeline continuous reaction is widely adopted in chemical production; industrialized production devices provided with pipeline reactors are not applied to production with gas generation; middle gas separation and reactor multi-segment control are adopted. According to the continuous reaction device, a general intermittent device used for oxidative cyclisation is replaced by the continuous reaction device composed via combination of the gas-liquid separator, the pipeline reactors, and ancillary facilities; production efficiency is increased; product yield is increased; automatic control is adopted by operation processes; manual operation is reduced; the production method is safe and reliable; and excellent effect is achieved.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a continuous reaction device and a production method for legally producing 3,8-dimethyl-7-chloroquinoline by oxidation ring. Background technique [0002] Quinazalic acid is a kind of pre-emergence selective herbicide, which is used for the control of broadleaf weeds in cereals, rapeseed, sugar beet and other crops. At present, the production technology of quinoxalic acid is relatively difficult, and there is no other domestic manufacturer except our company. 3,8-dimethyl-7-chloroquinoline is an important intermediate of quinoxalic acid, and its preparation method is the Skraup-oxidation method, which has the following specific methods: [0003] 3.8 -Dimethyl-7-chloroquinoline. The yield of this method is medium and the pollution is serious. [0004] In concentrated sulfuric acid, use iodine to oxidize 2-methyl-7-chloroaniline and 2-methacrolein (methacryl) to obtai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/18
CPCC07D215/18
Inventor 王作祥梁斌
Owner 中农发河南农化有限公司