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Method for continuously preparing 3, 5-dinitrobenzoic acid by using micro-channel reactor

A technology of dinitrobenzoic acid and microchannel reactor, which is applied in chemical instruments and methods, preparation of nitro compounds, chemical/physics/physicochemical processes, etc. "Warm" risk, long reaction time, etc.

Active Publication Date: 2021-04-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction to prepare 3,5-dinitrobenzoic acid can only take place under the sufficient contact between the reactant and the nitrating agent, and it is difficult to realize the ideal liquid-liquid interphase transfer by paddle stirring in the bottle (kettle) reactor. Quality, thereby the above-mentioned preparation method reaction efficiency is low, and the reaction time is long
The nitration of benzoic acid with nitric acid to prepare 3,5-dinitrobenzoic acid is an exothermic reaction with an exothermic heat of about 296kJ / mol. For a stirred reactor operated in batch mode under normal or near normal pressure, the heat exchange The small area and low heat transfer capacity determine that its stable temperature control effect is poor, and the risk of "flying temperature" is high; its system is open, there are many dead ends in the device, and the process control is in an intermittent fluctuating state, which determines its low stability. poor security

Method used

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  • Method for continuously preparing 3, 5-dinitrobenzoic acid by using micro-channel reactor
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  • Method for continuously preparing 3, 5-dinitrobenzoic acid by using micro-channel reactor

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Embodiment 1

[0031] The microchannel reaction device of the present invention (the reaction device is assembled by 3a (front)+3b (back) channel structure) is divided into preheating zone, reaction zone and quenching zone, according to figure 2connect. By adjusting the flow rate (5-15ml / min) of the pump and the channel length of the microchannel, the reaction residence time is controlled to 180s, the preheating temperature and the reaction temperature are set to 60°C, and the reaction pressure is 5bar. The mixed solution of raw material benzoic acid and fuming sulfuric acid (104%) is passed through the preheating zone A of metering pump 1 input device, concentrated nitric acid (98%) is passed through the preheating zone B of pump 2 input device, fully After preheating, it enters the reaction zone for mixed reaction. Among them, the molar ratio of benzoic acid to concentrated nitric acid is 1:3, and the 3,5-dinitrobenzoic acid product is continuously discharged from the outlet, and the rea...

Embodiment 2

[0040] Microchannel reaction device (3a+3c) of the present invention is divided into preheating zone, reaction zone and quenching zone, according to figure 2 connect. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 210s, the flow rate of the pump is 5-15ml / min, the preheating temperature and the reaction temperature are set at 65°C, and the reaction pressure is 5bar. The mixed solution of raw material benzoic acid and fuming sulfuric acid (104%) is passed through the preheating zone A of metering pump 1 input device, concentrated nitric acid (98%) is passed through the preheating zone B of pump 2 input device, fully After preheating, it enters the reaction zone for mixed reaction. Among them, the molar ratio of benzoic acid to sulfuric acid is 1:6. The 3,5-dinitrobenzoic acid product is continuously discharged from the outlet, and the reaction solution is quenched with ice water, follow...

Embodiment 3

[0048] Microchannel reaction device (3a+3d) of the present invention is divided into preheating zone, reaction zone and quenching zone, according to figure 2 connect. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 240s, the flow rate of the pump is 5-15ml / min, the preheating temperature and the reaction temperature are set at 70°C, and the reaction pressure is 10bar. The mixed solution of raw material benzoic acid and fuming sulfuric acid (104%) is passed through the preheating zone A of metering pump 1 input device, concentrated nitric acid (98%) is passed through the preheating zone B of pump 2 input device, fully After preheating, it enters the reaction zone for mixed reaction. Wherein, the molar ratio of benzoic acid to sulfuric acid is 1:5, and the molar ratio of benzoic acid to nitric acid is 1:4. The 3,5-dinitrobenzoic acid product is continuously discharged from the outlet, and...

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Abstract

The invention discloses a method for continuously preparing 3, 5-dinitrobenzoic acid by using a micro-channel reactor, and belongs to the technical field of organic synthesis processes. According to the method, benzoic acid and concentrated nitric acid are used as raw materials, fuming sulfuric acid is used as a solvent, trifluorosulfonic acid ketone is used as a catalyst, and the preparation process of 3, 5-dinitrobenzoic acid is continuously completed in a micro-channel reactor system. After the raw materials are introduced into the micro-channel reactor through a metering pump, the 3, 5-dinitrobenzoic acid product is obtained through preheating, mixed reaction and separation, the method can strictly control the temperature and the retention time in the reaction process, accurately control the reaction temperature to prevent temperature runaway, and improve the safety of a reaction device; and due to the strong mass transfer effect of the micro-channel reactor, the mass transfer effect among the raw materials in the reaction system is enhanced, and the reaction efficiency and the yield of 3, 5-dinitrobenzoic acid are greatly improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and specifically relates to a method for preparing 3,5-dinitrobenzoic acid through nitration reaction using benzoic acid as a raw material and copper trifluorosulfonate as a catalyst, more specifically in a microchannel A method for continuously preparing 3,5-dinitrobenzoic acid through nitration reaction using benzoic acid as a raw material in a reactor. Background technique [0002] 3,5-Dinitrobenzoic acid is an important fine chemical, pharmaceutical, and dye intermediate, mainly used in the preparation of diatrizoic acid, a diagnostic drug, which is a positive contrast agent for X-ray diagnosis, and is used for the preparation of diatrizoate meglumine, Sodium diatrizoate or compound diatrizoate meglumine injection is mainly used for urography, but also for angiography of cardiovascular, cerebrovascular, peripheral blood vessels, bile duct and various injection methods suc...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/57B01J19/00
Inventor 张跃郭冰蒙严生虎刘建武沈介发辜顺林马晓明陈代祥
Owner CHANGZHOU UNIV
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