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Method for preparing diazonium salt by utilizing micro-reactor

A technology of micro-reactor and diazonium salt, which is applied in the direction of organic chemistry, can solve the problems of blocking micro-channels, achieve continuous process, high utilization rate of raw materials, and avoid the effect of sudden temperature rise

Inactive Publication Date: 2016-06-22
上海睿瓦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Method for preparing diazonium salt by utilizing micro-reactor

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Embodiment 1

[0023] In such figure 1 In the reaction device shown, the sodium nitrite solution and o-ethylaniline are fed from B and C at flow rates of 1.1ml / min and 1ml / min respectively (the molar ratio of sodium nitrite to o-ethylaniline is 1:1) The tube is injected into the first micromixer 1 (internal interdigital micromixer, SIMM-V2, IMM, Germany, mixing channel inner diameter 45μm), and then the mixed solution passes through the first microchannel a (inner diameter: 0.3mm, residence time 0.2 s) Enter the second micromixer 2 (inner diameter 1mm) and the hydrochloric acid injected from the feed pipe A at a flow rate of 2.4ml / min (the molar ratio of hydrochloric acid to o-ethylaniline 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, the diazonium salt solution is collected in a round bottom flask E containing potassium iodide, the round bottom flask E is placed in a constant temperat...

Embodiment 2

[0025] In such figure 1 In the reaction device shown, sodium nitrite solution and o-ethylaniline are fed from B and C at flow rates of 1.44ml / min and 1ml / min (the molar ratio of sodium nitrite to o-ethylaniline is 1.05:1). The tube is injected into the first micro-mixer 1 (internal interdigital micro-mixer, SIMM-V2, IMM, Germany, mixing channel inner diameter 45μm), and then the mixed solution passes through the first microchannel a (inner diameter: 0.3mm, residence time 0.5 s) Enter the micro-second 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 thermostatic reaction bath T1 (0℃ ), and then enter the second microchannel b (inner diameter: 1mm) to continue the reaction for 10s, and the diazonium salt solution is collected in a round-bottom flask E containing potassium iodide. The round-bottom flask E is placed in a constant temperature reactio...

Embodiment 3

[0027] In such figure 1 In the reaction device shown, the sodium nitrite solution and o-ethylaniline are fed from B and C at flow rates 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 (internal interdigital micromixer, SIMM-V2, IMM, Germany, the inner diameter of the mixing channel is 45μm), 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 thermostatic reaction bath T1 (40°C) Mix, then enter the second microchannel b (inner diameter: 1mm) to continue the reaction for 2s, and the diazonium salt solution is collected in a round-bottom flask E containing potassium iodide. The round-bottom flask E is placed in a constant temperature reaction ba...

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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 salt, in particular to a method for preparing diazonium salt by using a microreactor. Background technique [0002] Diazonium salts are an important class of intermediates, mainly used in the synthesis of medicines, perfumes and dyes. [0003] The preparation of diazonium salt in industry is generally carried out by dissolving organic amine in acid in a reaction kettle, and then slowly adding sodium nitrite aqueous solution dropwise under stirring conditions. Due to the strong exotherm of the process, if the temperature is not well controlled, the diazonium salt will lose nitrogen when the temperature is out of control to produce by-products such as aromatics and coupling compounds, and even explode. In order to minimize the effect of the exotherm, the sodium nitrite solution is generally added dropwise slowly, but this approach has problems such as time-consuming and discontinuous process. In order ...

Claims

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Application Information

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Patent Type & Authority Applications(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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