2, 5-dichloronitrobenzene and micro-channel continuous synthesis process thereof

A technology of dichloronitrobenzene and a synthesis process, which is applied in the preparation of nitro compounds, organic chemistry, chemical/physical/physical chemical processes, etc., can solve the problems of long production cycle, high safety risk, low heat transfer efficiency and the like, Achieve the effect of short reaction time, reduced safety risk and simple process

Pending Publication Date: 2021-05-11
NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the domestic industrial production of 2,5-dichloronitrobenzene mainly adopts kettle-type batch process and kettle-type continuous process. However, the nitration process is a high-risk process. The traditional kettle-type nitration process has low heat transfer efficiency and large stock. , long production cycle, low production efficiency, and high safety risks. Many safety problems will inevitably lead to accidents, such as the explosion of Jilin Petrochemical Bibenzene Plant, the explosion of Tianjin Yikun Fine Chemical Technology Development Co., Ltd., and the "3.21 Xiangshui" in Yancheng, Jiangsu. "Accident etc.

Method used

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  • 2, 5-dichloronitrobenzene and micro-channel continuous synthesis process thereof

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Experimental program
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Effect test

Embodiment 1

[0053] Embodiment 1 of the present invention provides a kind of microchannel continuous synthesis process of 2,5-dichloronitrobenzene, such as figure 1 As shown, the details are as follows:

[0054](1) Weigh 250g of raw material p-dichlorobenzene and heat it to a molten state as FlowA, measure 80mL of fuming nitric acid and 140mL of sulfuric acid to prepare a mixed acid as FlowB, and measure 150mL of sulfuric acid as FlowC;

[0055] (2) After the preheating microchannel reactor is completed, the flow rate of Control FlowA is 14mL / min to feed to reaction module one, the flow rate of Control FlowB is 17mL / min to feed in the preheating module, and the flow rate of Control Flow C is 11mL Feed material to reaction module two per minute, the reaction temperature zone one is 70°C, and the temperature zone two is 100°C for reaction. The molar ratio of p-dichlorobenzene to fuming nitric acid is 1:1.05, and the total amount of fuming nitric acid and sulfuric acid The mass ratio of the ...

Embodiment 2

[0058] Embodiment 2 of the present invention provides a kind of microchannel continuous synthesis process of 2,5-dichloronitrobenzene, specifically as follows:

[0059] (1) Weigh 500g of raw material p-dichlorobenzene and heat it to a molten state as Flow A, measure 160mL of fuming nitric acid and 280mL of sulfuric acid to prepare a mixed acid as Flow B, and measure 300mL of sulfuric acid as Flow C;

[0060] (2) After the preheating microchannel reactor is completed, the flow rate of Control FlowA is 28mL / min to feed to reaction module one, the flow rate of Control FlowB is 34mL / min to feed in the preheating module, and the flow rate of Control Flow C is 19mL Feed material to reaction module two per minute, the reaction temperature zone one is 70°C, and the temperature zone two is 100°C for reaction. The molar ratio of p-dichlorobenzene to fuming nitric acid is 1:1.05, and the total amount of fuming nitric acid and sulfuric acid The mass ratio of the amount is 1:3.8, and the r...

Embodiment 3

[0063] Embodiment 3 of the present invention provides a kind of microchannel continuous synthesis technique of 2,5-dichloronitrobenzene, specifically as follows:

[0064] (1) Take by weighing 250g raw material p-dichlorobenzene and be heated to molten state as FlowA, measure the sulfuric acid that the fuming nitric acid of 80mL and the embodiment 1 of 140mL reclaim are mixed into mixed acid as Flow B, measure the reclaimed of embodiment 1 of 150mL Sulfuric acid as Flow C;

[0065] (2) After the preheating microchannel reactor is completed, the flow rate of Control FlowA is 14mL / min to feed to reaction module one, the flow rate of Control FlowB is 17mL / min to feed in the preheating module, and the flow rate of Control Flow C is 11mL Feed to the reaction module two per minute, the reaction temperature temperature zone one is 70°C, and the temperature zone two is 100°C for the reaction. The molar ratio of p-dichlorobenzene and fuming nitric acid is 1:1.05, and the fuming nitric a...

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Abstract

The invention relates to the field of synthesis of 2, 5-dichloronitrobenzene, in particular to 2, 5-dichloronitrobenzene and a micro-channel continuous synthesis process thereof. The micro-channel continuous synthesis process of the 2, 5-dichloronitrobenzene comprises the following steps of preheating mixed acid by a micro-channel reactor preheating module, reacting the mixed acid with paradichlorobenzene in a molten state in a micro-channel reactor reaction module I, continuously reacting in a micro-channel reactor reaction module II containing sulfuric acid to obtain a reaction solution, layering, and washing and layering an organic layer by an alkali solution, thereby obtaining the product. The mixed acid is fuming nitric acid and sulfuric acid. The micro-channel continuous synthesis process of 2, 5-dichloronitrobenzene belongs to a solvent-free micro-channel process and is green and safe, the raw material conversion rate is 100 wt%, the yield is 99.5 wt% or above, the product purity is 99.9 wt% or above, and the product can be subjected to subsequent reaction without rectification and purification.

Description

technical field [0001] The invention relates to the field of 2,5-dichloronitrobenzene synthesis, more specifically, the invention relates to a 2,5-dichloronitrobenzene and a microchannel continuous synthesis process thereof. Background technique [0002] At present, the domestic industrial production of 2,5-dichloronitrobenzene mainly adopts kettle-type batch process and kettle-type continuous process. However, the nitration process is a high-risk process. The traditional kettle-type nitration process has low heat transfer efficiency and large stock. , long production cycle, low production efficiency, and high safety risks. Many safety problems will inevitably lead to accidents, such as the explosion of Jilin Petrochemical Bibenzene Plant, the explosion of Tianjin Yikun Fine Chemical Technology Development Co., Ltd., and the "3.21 Xiangshui" in Yancheng, Jiangsu. "Accidents etc. With the increasingly strict domestic safety production policy, the traditional tank-type contin...

Claims

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Application Information

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IPC IPC(8): C07C205/12C07C201/08B01J19/00
CPCC07C201/08B01J19/0093B01J2219/00871C07C205/12Y02P20/10
Inventor 沈书群茅佳荣徐伟刘卫卫秦燕
Owner NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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