Self-powered continuous nitration method and device

An automatic and continuous technology, applied in chemical instruments and methods, preparation of nitro compounds, preparation of organic compounds, etc., can solve the problems of large accumulation of materials and heat, high risk of reaction process, and high risk of thermal runaway. Increased heat exchange area, reduced risk of thermal runaway, effect of short residence time

Active Publication Date: 2021-07-16
SHENYANG RES INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process is a batch process, and the total reaction time exceeds 10 hours. The material and heat accumulation in the reactor is very large. Once thermal runaway occurs, the temperature of the material itself will rise rapidly, causing decomposition, and the reaction process is very dangerous.
[0004] In 2017, Liu Dong et al. reported (Pesticides, 2017,56(1):878-881) and patent CN 106083596B that a three-pot series device was used for continuous nitration to prepare 2,5-dichloronitrobenzene. The nitration reaction temperature was 60 ~70℃, residence time 2~7h, 2,5-dichloronitrobenzene content above 99.5%, however, the reactor of this process is still a reactor, and the risk of thermal runaway is high

Method used

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  • Self-powered continuous nitration method and device
  • Self-powered continuous nitration method and device
  • Self-powered continuous nitration method and device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Such as figure 1 As shown, the device of the present invention includes an automatic power generation chamber 4 and two sections of circulation chambers, wherein the automatic power generation chamber 4 is provided with a rotating shaft 3 rotating in the horizontal direction and an impeller 5 integrated with the rotating shaft, and the design of the impeller angle should meet Circulation technical parameter requirements. The lower end of the automatic power generation chamber 4 is fixedly connected to the upper end of the first-stage circulation chamber, and the lower end of the first-stage circulation chamber is slowed down by the amplifying connecting pipe 11 and then connected to the lower end of the second-stage circulation chamber, and the upper end of the second-stage circulation chamber is connected to the automatic The force generating chambers 4 are connected so as to form a complete circulation. The first-stage circulation chamber is filled with heat exchange...

Embodiment 2

[0040] Utilize the device described in Example 1 to prepare 4-chloro-3,5-dinitrobenzotrifluoride using 4-chloro-3-nitrobenzotrifluoride

[0041]

[0042] In this example, 4-chloro-3-nitrobenzotrifluorotoluene, fuming nitric acid (content 98%) and fuming sulfuric acid (content 106.8%) are used as raw materials to generate 4-chloro-3-nitro Trifluorotoluene is an example, fuming nitric acid and fuming sulfuric acid are formulated into mixed acid according to the mass ratio of 1:4.45, and then the waste acid after nitrification is added through the feed port of the device to make a base, accounting for about 85% of the total volume- 90%, turn on the explosion-proof motor 1 and heat up to 118°C after the circulation of the motor is stable, mix 4-chloro-3-nitrobenzotrifluorotoluene and mixed acid at a mass ratio of 1:3.93, and then continuously add it to the reactor from the feed port after mixing. Adjust the heat exchange medium to control the temperature in the reactor to 120° ...

Embodiment 3

[0044] Preparation of 4-chloro-3,5-dinitrobenzotrifluoride from 4-chloro-3-nitrobenzotrifluoride

[0045]

[0046] In this example, 4-chloro-3-nitrotrifluorotoluene, fuming nitric acid (content 98%) and fuming sulfuric acid (content 104.5%) were used as raw materials to generate 4-chloro-3-nitrotrifluorotoluene through automatic nitration. Fluorotoluene as an example, mix fuming nitric acid and fuming sulfuric acid at a mass ratio of 1:6.67, control the temperature at 125°C, and simultaneously mix 4-chloro-3-nitrobenzotrifluoride and mixed acid at a mass ratio of 1:6.93 Feed from the kinetic reactor with a residence time of 2.5 hours. After the reaction, the material enters the layered kettle, cools down to 100°C, and stands still for 30 minutes. The organic phase is washed with aqueous sodium carbonate solution to pH = 8-9, and the product 4-chloro-3,5-dinitrobenzotrifluoride is obtained. , the content is 96.5%, and the yield is 94.2%. Using an automatic power reactor, o...

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Abstract

The invention belongs to the technical field of organic synthesis application, and particularly relates to a self-powered continuous nitration method and device. According to the method, a raw material (or a raw material solution) and mixed acid (or nitric acid) are added into a self-powered continuous reactor at the same time, reaction feed liquid continuously and circularly flows, is mixed and reacts in a tube pass through self-propelling force generated by stirring of an impeller, the mass and heat transfer process is completed, and the target requirement is met. According to the invention, the mass transfer and heat transfer efficiency can be improved, the heat exchange and heat transfer capabilities are improved, the reaction time is shortened, the risk degree of art is reduced, the thermal runaway risk is avoided, the reaction safety is improved, and the realization of chemical industry intrinsic safety large scale production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, and in particular relates to a method and a device for automatic dynamic continuous nitration. Background technique [0002] Nitrification reaction is widely used in fine chemical industry such as medicine and pesticide. Concentrated nitric acid and mixed acid are usually used as nitrating agents, which have the characteristics of large reaction heat release, heterogeneous mass transfer and heat transfer. The traditional process mostly adopts intermittent or semi-batch kettle type, etc. The kettle type process is batch production, the technology is backward, the material volume of a single kettle is large, the efficiency of mass transfer and heat transfer is poor, and the dispersion of materials is relatively slow, which easily leads to the accumulation of raw materials The heating and cooling is conducted through the jacket, the distance between the jacket wall and the cent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/14C07C205/12C07C201/08C07C205/06C07C205/22B01J19/18B01J19/00
CPCC07C201/14C07C201/08B01J19/18B01J19/0053B01J19/0013B01J2219/00092C07C205/12C07C205/06C07C205/22
Inventor 程春生明旭魏振云雷京盖永明李全国孔蓉马晓华杨兆国
Owner SHENYANG RES INST OF CHEM IND
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