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Method for preparing 3-fluorobenzotrifluoride based on diazotization of dinitrogen trioxide

A technology of dinitrogen trioxide and fluorobenzotrifluoride, applied in chemical instruments and methods, preparation of halogenated hydrocarbons, disproportionation separation/purification of halogenated hydrocarbons, etc., can solve problems such as long reaction routes, environmental pollution, and complicated processes, Achieve the effect of high production efficiency, energy saving and easy operation

Pending Publication Date: 2022-08-02
SHANGYU XIES CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] At present, the method for industrially producing 3-fluorobenzotrifluoride is mainly to use trifluorotoluene as a raw material, which is sequentially obtained through nitration, hydrogenation reduction, and fluorination. The 3-fluorobenzotrifluoride produced by these reactions has a higher purity, but the reaction The route is long and the process is more complicated, which makes the production cost of the product higher, and the production process will cause serious pollution to the environment

Method used

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  • Method for preparing 3-fluorobenzotrifluoride based on diazotization of dinitrogen trioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) be that the fluoroboric acid solution of 25% by mass concentration and m-amino trifluorotoluene are pumped into the salt-forming microchannel reactor with the flow velocity of 9g / min, 1.5g / min respectively and carry out the salt-forming reaction at 15 ℃, After the salt is formed, it enters the diazonium salt tubular reactor;

[0028] (2) Introduce dinitrogen trioxide into the diazonium salt tubular reactor at a flow rate of 0.35g / min and carry out the diazotization reaction at -5°C, and the diazonium salt solution and the acid solution generated by the reaction enter the diazonium salt solution and the acid solution. The nitrogen salt is temporarily stored in the kettle, and subjected to continuous centrifugal treatment, the diazonium salt obtained by centrifugation is dried, and the dried diazonium salt is subjected to thermal decomposition treatment at 600 ° C, and the thermal decomposition rate is controlled to 2g / min; The mother liquor is concentrated, the mass ...

Embodiment 2

[0031] (1) be that the fluoroboric acid solution of 25% by mass concentration and m-amino trifluorotoluene are pumped into the salt-forming microchannel reactor with the flow velocity of 10g / min, 1.55g / min respectively and carry out the salt-forming reaction at 10 DEG C, After the salt is formed, it enters the diazonium salt tubular reactor;

[0032] (2) Introduce dinitrogen trioxide into the diazonium salt tubular reactor at a flow rate of 0.4 g / min and carry out the diazotization reaction at -5°C, and the diazonium salt solution and the acid solution generated by the reaction enter the diazonium salt solution and the acid solution. The nitrogen salt is temporarily stored in the kettle, and subjected to continuous centrifugal treatment, the diazonium salt obtained by centrifugation is dried, and the dried diazonium salt is subjected to thermal decomposition treatment at 700 ° C, and the thermal decomposition rate is controlled to 3g / min; The mother liquor is concentrated, the...

Embodiment 3

[0035] (1) be that the fluoroboric acid solution of 25% by mass concentration and m-amino trifluorotoluene are pumped into the salt-forming microchannel reactor with the flow velocity of 10g / min, 1.65g / min respectively and carry out the salt-forming reaction at 10 ℃, After the salt is formed, it enters the diazonium salt tubular reactor;

[0036] (2) Introduce dinitrogen trioxide into the diazonium salt tubular reactor at a flow rate of 0.5 g / min and carry out the diazotization reaction at -5°C, and the diazonium salt solution and the acid solution generated by the reaction enter the diazonium salt solution and the acid solution. The nitrogen salt is temporarily stored in the kettle, and subjected to continuous centrifugal treatment, the diazonium salt obtained by centrifugation is dried, and the dried diazonium salt is subjected to thermal decomposition treatment at 650 ° C, and the thermal decomposition rate is controlled to 2-3 g / min; centrifugal treatment The rear mother l...

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Abstract

The invention discloses a method for preparing 3-fluorobenzotrifluoride based on diazotization of dinitrogen trioxide, which comprises the following steps: pumping a fluoboric acid solution and m-aminobenzotrifluoride into a salifying micro-channel reactor for reaction, feeding a product into a diazonium salt tubular reactor, and introducing dinitrogen trioxide for reaction, a product enters a diazonium salt temporary storage kettle and then is subjected to continuous centrifugal treatment, and diazonium salt is dried and subjected to thermal decomposition treatment; the centrifuged mother liquor is concentrated, and waste water obtained during concentration is used for preparing a fluoboric acid solution again; gas generated during thermal decomposition treatment of the diazonium salt is sprayed and absorbed by acid liquor, and residues generated during thermal decomposition treatment are used for wastewater treatment; the sprayed and absorbed liquid is layered, an oil layer is pumped into a rectifying tower to be rectified, a target product is obtained, and a water layer is used for preparing a fluoboric acid solution. According to the method, waste liquid and solid waste in production are recycled, resources are effectively saved, and the product is high in yield and purity.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing 3-fluorotrifluorotoluene based on diazonium trioxide diazotization. Background technique [0002] 3-Fluorotrifluorotoluene, also known as m-fluorotrifluorotoluene, is an intermediate product in the production of o-trifluoromethylaniline. Due to its high efficiency and low toxicity, o-trifluoromethylaniline is an important intermediate in the synthesis of pesticides and medicines. In recent years, with the continuous development of downstream products of o-trifluoromethylaniline, its demand has increased year by year. [0003] At present, the method for industrially producing 3-fluorotrifluorotoluene mainly uses trifluorotoluene as a raw material, which is obtained through nitration, hydrogenation reduction, and fluorination in turn. The 3-trifluorotoluene obtained by these reactions has a higher purity, but the reaction The route is long and the ...

Claims

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Application Information

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IPC IPC(8): C07C25/13C07C17/093C07C17/38C07C17/383
CPCC07C17/093C07C17/38C07C17/383C07C245/20C07C209/00C07C25/13C07C211/52
Inventor 解卫宇陈少君刘杰顾林江徐巧巧卢晓健宋小艳解海翔
Owner SHANGYU XIES CHEM IND
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