Method for synthesizing 2,5-dichloroaniline by micro-channel reactor

A microchannel reactor, the technology of dichloroaniline, is applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, preparation of organic compounds, etc. Sufficient, obvious magnifying effect, etc.

Inactive Publication Date: 2017-04-19
HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The nitration reaction is a strong exothermic reaction. It needs to be controlled at a relatively low temperature when operating in a conventional reactor. The heat released by the reaction cannot be taken away in time, the reaction temperature cannot be accurately controlled, and the heterogeneous reaction is stirred. Insufficient and other shortcomings, it is easy to cause side reactions such as multiple nitrification and oxidation, the process operation is very complicated, the amplification effect is obvious, the energy consumption is high, and the yield is low
[0006] 2. Catalytic hydrogenation reaction is a typical gas-liquid-solid three-phase reaction. When operating in a reactor, in order to ensure

Method used

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  • Method for synthesizing 2,5-dichloroaniline by micro-channel reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0053] (1) Weigh 300g of 1,4-dichlorobenzene and dissolve it in 2L of dichloromethane as material 1, measure 400ml of concentrated nitric acid as material 2, and measure 600mL of concentrated sulfuric acid as material 3;

[0054] (2) The flow velocity of control material 1 is 15ml / min; The flow velocity of control material 2 is 8min / min; The flow velocity of control material 3 is 12min / min; Reaction temperature is 35 ℃, and the mol ratio of o-difluorobenzene and nitric acid is 1 :2.5; The mol ratio of nitric acid and the vitriol oil is 1:2.0; The residence time of reaction is 70s;

[0055] (3) When each material in the reactor reaches a steady state, collect the reaction liquid flowing out from the reactor outlet, and feed 120 minutes of material 1 (that is, 1800ml of material 1, 260.0g of 1,4-dichlorobenzene) to correspond to The reaction solution of the reaction solution is an example, separate liquid, keep the organic phase, extract the acid layer once with 500ml of dichlor...

Embodiment 2

[0060] In the screening and optimization process of process parameters, the parameters such as the concentration of reaction raw materials, molar ratio, residence time have been explored, and the corresponding parameters of corresponding steps are changed on the basis of the operation steps of Example 1, and other parameter conditions are all constant. The results are summarized as follows:

[0061] 1. Nitrification reaction:

[0062]

[0063] 2. Catalytic hydrogenation reaction:

[0064]

[0065]

[0066] 3. Pd / C recovery application experiment:

[0067]

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Abstract

The invention provides a method for synthesizing 2,5-dichloroaniline by a micro-channel reactor. A nitratlon reaction and a catalytic hydrogenation reaction are performed by using the micro-channel reactor. The method comprises the following steps of nitratlon reaction: raw materials of nitro-p-dichlorobenzene are dissolved into an organic solvent, and are preheated; concentrated nitric acid and concentrated sulfuric acid are mixed and are preheated; the materials enter a reaction module group to take a reaction after the preheating; and an intermediate product of 2,5-Dichloronitrobenzene is obtained after the refining; and catalytic hydrogenation reaction: the 2,5-Dichloronitrobenzene is dissolved into a solvent; Pd-loaded active carbon catalysts are added; dechlorination inhibitors are added, and then, preheating is performed; after the materials are preheated, hydrogen gas enters the reaction module group to take a reaction; and post-treatment is performed to obtain the 2,5-dichloroaniline. The method provided by the invention has the advantages that the mixing effect is good; the temperature and material proportion control is precise; the reaction yield and the product purity are improved; the reaction is safe and stable; the time is short; no amplification effect exists; and wide application prospects are realized in industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing 2,5-dichloroaniline. Background technique [0002] 2,5-Dichloroaniline is an important fine chemical intermediate, widely used in the production of fine chemicals such as dyes, medicines, spices and rubber additives. Its structure is as follows: [0003] [0004] In the agricultural industry, 2,5-dichloroaniline is mainly used for synthesizing the herbicide dicamba, and in the dye industry for synthesizing ice-dyeing dye scarlet base GG, printing and dyeing scarlet cloth color developer; it is also used in the manufacture of nitrogen fertilizer synergists, Such as N-2,5-dichlorophenylsuccinamic acid. Therefore, the market prospect of domestic production of 2,5-dichloroaniline is broad. At present, the domestic production method of 2,5-dichloroaniline mainly uses 1,4-dichlorobenzene as the starting material, and 2,5-dichloroaniline is obtained after...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/52B01J19/00
CPCC07C201/08B01J19/0093C07C209/365C07C205/12C07C211/52
Inventor 刘桂梅任吉秋杨昆安永生
Owner HEILONGJIANG XINCHUANG BIOLOGICAL TECH DEV CO LTD
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