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Method for continuously preparing aniline diazonium salt and phenylhydrazine hydrochloride on basis of microreactor

A technology of phenylhydrazine hydrochloride and microreactor, which is applied in chemical instruments and methods, hydrazine preparation, chemical/physical/physical-chemical reactors, etc., can solve the problem of long reaction time of phenylhydrazine hydrochloride, excess reaction raw materials, discontinuous reaction, etc. problems, to achieve the effect of shortening the reaction time, increasing the reaction temperature, and improving the process safety

Inactive Publication Date: 2019-03-22
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims at defects such as long reaction time for preparing phenylhydrazine hydrochloride in the prior art, large process energy consumption, discontinuous reaction, excess reaction raw materials, etc., and proposes a continuous preparation method of aniline diazonium salt and phenylhydrazine hydrochloride based on a microreactor,

Method used

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  • Method for continuously preparing aniline diazonium salt and phenylhydrazine hydrochloride on basis of microreactor
  • Method for continuously preparing aniline diazonium salt and phenylhydrazine hydrochloride on basis of microreactor
  • Method for continuously preparing aniline diazonium salt and phenylhydrazine hydrochloride on basis of microreactor

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Experimental program
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Effect test

Embodiment 1

[0030] In the reactor 1 shown in the figure, the capillary is 1000 mm long and arranged in a folded line with a bend angle of 120° and a pitch of 80 mm. Such as figure 1 , sodium nitrite Q1, aniline salt and hydrochloric acid mixed solution Q2 are respectively injected into a T-shaped micro-mixer with an inner diameter of 0.5mm through a fluid pump, and the injection volume flow rate is 8mL / min, and the molar ratio is sodium nitrite: aniline: Hydrochloric acid=1:1.01:2.15. The capillary microchannel is built in a water bath at 15°C to make the reaction process reach the state, and the obtained diazonium solution is directly injected into the reduction reaction kettle for subsequent reactions. The reaction kettle contains a mixture of ammonium sulfite and ammonium bisulfite prepared in advance. After the reactor has collected a certain amount of mixed fluid from the microreactor, continue to keep warm at 80°C for 1 hour, and finally add strong acid to keep warm for 15 minutes...

Embodiment 2

[0032] In the reactor 2 shown in the figure, the capillary is 1000mm long and is helical. The diameter of the helix is ​​80mm and the pitch is 30mm. Such as figure 1 , sodium nitrite Q1, aniline salt and hydrochloric acid mixed solution Q2 are respectively injected into a T-shaped micro-mixer with an inner diameter of 0.5 mm through a fluid pump, and the injection volume flow rate is 10 mL / min, and the molar ratio is sodium nitrite: aniline: Hydrochloric acid=1:1.01:2.15. The capillary microchannel is built in a water bath at 20°C to make the reaction process reach the state, and the obtained diazonium solution is directly injected into the reduction reaction kettle for subsequent reactions. The reaction kettle contains a mixture of ammonium sulfite and ammonium bisulfite prepared in advance. After the reactor has collected a certain amount of mixed fluid from the microreactor, continue to keep warm at 80°C for 1 hour, and finally add strong acid to keep warm for 15 minutes...

Embodiment 3

[0034] In reactor 3 as shown in the figure, the capillary is 1000mm long and is in a straight line, such as figure 1 , sodium nitrite Q1, aniline salt and hydrochloric acid mixed solution Q2 are respectively injected into a T-shaped micro-mixer with an inner diameter of 0.5 mm through a fluid pump, and the injection volume flow rate is 8 mL / min, and the molar ratio is sodium nitrite: aniline: hydrochloric acid =1:1.01:2.15. The capillary microchannel is built in a 30°C water bath to make the reaction process reach the state, and the obtained diazonium solution is directly injected into the reduction reaction kettle for subsequent reactions. The reaction kettle contains a mixture of ammonium sulfite and ammonium bisulfite prepared in advance. After the reactor has collected a certain amount of mixed fluid from the microreactor, continue to keep warm at 80°C for 1 hour, and finally add strong acid to keep warm for 15 minutes. The sample was obtained after cooling crystallizati...

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Abstract

The invention relates to a method for continuously preparing aniline diazonium salt and phenylhydrazine hydrochloride on the basis of a microreactor. An aniline salt and acid mixture and an nitrite aqueous solution which are prepared at a normal temperature are continuously injected into the microreactor to carry out diazotization reaction, and by the steps of reduction, acid precipitation and filtration, the phenylhydrazine hydrochloride is obtained. The method is easy to operate, the temperature of the diazotization reaction is high, the dosages of the reactants approximate the stoichiometric ratio, the time of the diazotization reaction is short, the yield is high, the aniline diazonium salt and the phenylhydrazine hydrochloride can be continuously produced, the energy consumption is reduced, the safety of the process is increased, and the method is applicable to industrial production.

Description

technical field [0001] The invention relates to a technique in the field of fine chemical industry, in particular to a continuous preparation method of aniline diazonium salt and phenylhydrazine hydrochloride based on a microreactor. Background technique [0002] Phenylhydrazine hydrochloride is an important chemical raw material, pesticide and pharmaceutical intermediate. The preparation of phenylhydrazine hydrochloride requires two-step reaction preparation of aniline diazotization and diazonium salt reduction. In a traditional tank reactor, the diazotization reaction time of aniline is more than 30 minutes, and the reaction temperature is -5-0°C, while the formation of aniline hydrochloride requires a further reduction reaction of aniline diazonium salt, and the reaction temperature generally used is Above 60°C. The temperature difference between the diazotization and reduction reactions is large, resulting in high energy consumption in the process. The diazonium salt ...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/22C07C245/20B01J19/00
CPCB01J19/0093B01J2219/00795B01J2219/00889C07C241/02C07C245/20C07C243/22
Inventor 苏远海查理濮鑫商敏静
Owner SHANGHAI JIAO TONG UNIV
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