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Process for synthesizing nitro diether by adopting narrow-distance parallel plate reactor

A parallel plate, nitro bis-ether technology, applied in the direction of ester reaction to prepare ether, chemical/physical/physical chemical reactor details, chemical/physical/physical chemical fixed reactor, etc., can solve the problem of high energy consumption and cost problems, achieving shorter reaction times, lower risk, and lower risk of explosion

Pending Publication Date: 2021-01-05
西安本清化学技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, in the nitrification process of this process, due to the extremely fast reaction heat release in the currently used kettle-type nitrification reaction, for the safety of nitrification, it must be carried out at a low temperature of -10°C to 30°C, and the reaction time is as long as 5 to 6 hours, and the energy cost is high. Higher, and cannot solve the danger of nitrification reaction from the essence of process safety

Method used

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  • Process for synthesizing nitro diether by adopting narrow-distance parallel plate reactor
  • Process for synthesizing nitro diether by adopting narrow-distance parallel plate reactor
  • Process for synthesizing nitro diether by adopting narrow-distance parallel plate reactor

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Experimental program
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Effect test

Embodiment 1

[0040] Such as figure 1 Shown, a kind of technique that adopts narrow-distance parallel plate reactor to synthesize nitrobisethers specifically comprises the following steps:

[0041] 1) Preparation of 1,3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene and solvent mixed solution:

[0042] 400kg of solid 1,3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene is dropped into a stainless steel mixing kettle with heating and stirring, and then by mass ratio (solvent: 1,3-bis[ 2-Chloro-4-(trifluoromethyl)phenoxy]benzene) 3:1 transport the dichloroethane from the dichloroethane storage tank to the stainless steel mixing kettle through the pump, start stirring and heating after the solvent is added, After the solid material is completely dissolved, the mixed solution is pumped to the mixed solution raw material tank through the mixing tank;

[0043] 2) Preparation of mixed acid:

[0044] The fuming nitric acid with a mass concentration of 98% is transported from the nitric acid stor...

Embodiment 2

[0054] A process for synthesizing nitrobisethers using narrow-distance parallel plate reactors, specifically comprising the following steps:

[0055] 1) Preparation of 1,3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene and solvent mixed solution:

[0056] 400kg of solid 1,3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene is dropped into a stainless steel mixing kettle with heating and stirring, and then by mass ratio (solvent: 1,3-bis[ 2-Chloro-4-(trifluoromethyl)phenoxy]benzene) 3:1 Transport the petroleum ether from the petroleum ether storage tank to the stainless steel mixing kettle through the pump, start stirring and heating after the solvent is added, and wait until the solid material is completely After dissolving, the mixed solution is pumped to the mixed solution raw material tank through the mixing tank;

[0057] 2) Preparation of mixed acid:

[0058] The nitric acid with a mass concentration of 68% is transported from the nitric acid storage tank to the static m...

Embodiment 3

[0068] A process for synthesizing nitrobisethers using narrow-distance parallel plate reactors, comprising the following steps:

[0069] 1) 1) Preparation of 1,3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene and solvent mixed solution:

[0070] 400kg of solid 1,3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene is dropped into a stainless steel mixing kettle with heating and stirring, and then by mass ratio (solvent: 1,3-bis[ 2-Chloro-4-(trifluoromethyl)phenoxy]benzene) 3:1 Send equal volumes of dichloroethane and petroleum ether from the dichloroethane storage tank and petroleum ether storage tank to the stainless steel mixing tank respectively. After the addition of the solvent, start stirring and heating. After the solid material is completely dissolved, the mixed solution is pumped to the mixed solution raw material tank through the mixing kettle;

[0071] 2) Preparation of mixed acid

[0072] The fuming nitric acid with a mass concentration of 75% is transported from t...

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Abstract

The invention belongs to the technical field of chemical engineering, and discloses a process for synthesizing an intermediate nitrodiether of oxyfluorfen by adopting a narrow-distance parallel platereactor, which comprises the following steps: by using 3, 4-dichlorobenzotrifluoride and resorcinol as raw materials, condensing to obtain 1, 3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene, and carrying out a nitration reaction process on 1, 3-bis[2-chloro-4-(trifluoromethyl)phenoxy]benzene and a nitrating agent in a narrow-distance parallel plate reactor, so that nitro diether is prepared. Thecontinuous narrow-distance parallel plate reaction is adopted, so that huge heat generated by the reaction can be quickly removed, the reaction temperature can be controlled at 50-95 DEG C, the reaction time is greatly shortened, and the molar equivalent of reaction substances in the reaction process is extremely small, so that the reaction is intrinsically safe, the reaction risk is reduced, andthe process safety is improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a production process of oxyfluorfen intermediate, in particular to a nitrobisether (1,3-bis[ 2-Chloro-4-(trifluoromethyl)phenoxy]-4-nitrobenzene). Background technique [0002] Oxyfluorfen is a contact herbicide, developed by Rohm and Haas Company (now Dow) in 1975, the English name is oxyfluorfen; chemical name: 2-chloro-4-trifluoromethylphenyl -3'-Ethoxy-4'-nitrophenyl ether; chemical formula: C 5 h 11 C 1 f 3 NO 4 , which belongs to fluorine-containing diphenyl ethers, is a selective, pre-emergence or post-emergence contact herbicide at an ultra-low dosage. Applicable to rice, soybean, wheat, cotton, corn, oil palm, vegetables and orchards, etc., the dosage is 1~2g active ingredient / 100m 2 . Oxyfluorfen is a very important herbicide in current agricultural production. It has been widely used at home and abroad, with a large amount of use and broad prospects. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/12C07C41/16C07C43/29B01J19/24B01J19/00
CPCC07C201/08C07C41/16B01J19/249B01J19/0053B01J19/006B01J2219/2453B01J2219/2462B01J2219/2469B01J2219/2486C07C43/29C07C205/12
Inventor 曹彬薛群翔王荣
Owner 西安本清化学技术有限公司
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