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A kind of method utilizing microreactor to prepare diazonium salt

A technology of microreactor and diazonium salt, which is applied in the direction of organic chemistry, can solve the problem of clogged microchannels, etc., and achieve the effect of continuous process, high raw material utilization rate and excellent mass transfer

Inactive Publication Date: 2018-07-17
上海睿瓦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides a method for preparing diazonium salts using a microreactor, which solves the problem that organic amines are insoluble in acids or form insoluble salts with acids to block microchannels in the process of preparing diazonium salts in microreactors

Method used

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  • A kind of method utilizing microreactor to prepare diazonium salt

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Embodiment 1

[0023] in such as figure 1In the reaction device shown, the sodium nitrite solution and o-ethylaniline are fed from B and C respectively at a flow rate of 1.1ml / min and 1ml / min (the molar ratio of sodium nitrite and o-ethylaniline is 1:1). The tube is injected into the first micro-mixer 1 (inner interdigitated micro-mixer, SIMM-V2, IMM, Germany, the inner diameter of the mixing channel is 45 μm), and then the mixed solution passes through the first micro-channel a (inner diameter: 0.3 mm, residence time 0.2 s) enter the second micro-mixer 2 (inner diameter 1mm) and the hydrochloric acid injected by feed pipe A at a flow rate of 2.4ml / min (hydrochloric acid and o-ethylaniline molar ratio is 2.8:1) in the constant temperature reaction bath T1 (- 5 ℃), then enter the second microchannel b (inner diameter: 1mm) to continue the reaction for 10s, and the obtained diazonium salt solution is collected with a round-bottomed flask E equipped with potassium iodide, and the round-bottomed...

Embodiment 2

[0025] in such as figure 1 In the reaction device shown, the sodium nitrite solution and o-ethylaniline are fed from B and C at a flow rate of 1.44ml / min and 1ml / min respectively (the molar ratio of sodium nitrite to o-ethylaniline is 1.05:1). The tube is injected into the first micro-mixer 1 (inner interdigitated micro-mixer, SIMM-V2, IMM, Germany, the inner diameter of the mixing channel is 45 μm), and then the mixed solution passes through the first micro-channel a (inner diameter: 0.3 mm, residence time 0.5 s) Enter the second micro-mixer 2 (inner diameter 5mm) and the hydrochloric acid injected from the feed pipe A at a flow rate of 4ml / min (the molar ratio of hydrochloric acid to o-ethylaniline is 3.2:1) in the constant temperature reaction bath T1 (0°C ), and then enter the second microchannel b (inner diameter: 1mm) to continue the reaction for 10s, and the obtained diazonium salt solution is collected with a round-bottomed flask E equipped with potassium iodide, and t...

Embodiment 3

[0027] in such as figure 1 In the reaction device shown, the sodium nitrite solution and o-ethylaniline are fed from B and C respectively at a flow rate of 1.44ml / min and 1ml / min (the molar ratio of sodium nitrite to o-ethylaniline is 1.1:1). The tube is injected into the first micromixer 1 (interdigital micromixer, SIMM-V2, IMM, Germany, the inner diameter of the mixing channel is 45 μm), and then the mixed solution passes through the first microchannel a (0.3mm, residence time 0.5s) Enter the second micro-mixer 2 (inner diameter 9mm) and the hydrochloric acid injected from the feed pipe A at a flow rate of 4ml / min (the molar ratio of hydrochloric acid to o-ethylaniline is 4:1) in the constant temperature reaction bath T1 (40°C) Mix, then enter the second microchannel b (inner diameter: 1mm) to continue the reaction for 2s, and the obtained diazonium salt solution is collected with a round-bottomed flask E equipped with potassium iodide, and the round-bottomed flask E is plac...

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Abstract

The invention provides a method for preparing diazonium salt by utilizing a micro-reactor. The method comprises the following steps: firstly, preparing a nitrite solution and an organic amine into oil-water emulsion through a micro-mixer; enabling the oil-water emulsion to react with an introduced acid in a micro-channel to obtain the diazonium salt. The size of the salt formed by the contact of the oil-water emulsion and the acid is very small, and the salt can be consumed rapidly when reacting with nitrous acid, so that a pipeline is not blocked. The method provided by the invention is convenient and rapid to operate and short in reaction time; the defect that the diazonium salt is decomposed, caused by the fact that the temperature is too high, is avoided, and industrial production can be realized.

Description

technical field [0001] The invention relates to a method for preparing diazonium salts, in particular to a method for preparing diazonium salts using a microreactor. Background technique [0002] Diazonium salt is an important class of intermediates, which are mainly used in the synthesis of medicine, spices and dyes. [0003] In industry, the preparation of diazonium salt is generally carried out in a reaction kettle by first dissolving organic amine in acid, and then slowly adding sodium nitrite aqueous solution dropwise under stirring conditions. Due to the strong exothermic process, if the temperature is not well controlled, the diazonium salt will lose nitrogen to produce aromatic hydrocarbons, couples and other by-products when the temperature is out of control, and even explode. In order to minimize the influence of heat release, sodium nitrite solution is generally added dropwise slowly, but this method has problems such as time-consuming and discontinuous process. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C245/20
CPCC07C245/20
Inventor 张利雄王超曾昌凤
Owner 上海睿瓦科技有限公司
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