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Method for preparing 2-cyanoethyl-5-norbornadiene-2-aldehyde in micro-structural reactor

A microstructure reactor, cyanoethyl technology, applied in chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc., can solve the problem of producing a large amount of solid residue, the need to grind the catalyst into powder, and the large amount of acrylonitrile used problems, to achieve the effect of less solid residue, less aggregation, and strong mass and heat transfer capabilities

Inactive Publication Date: 2016-11-16
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is that in the prior art, the consumption of acrylonitrile is large, a large amount of solid residues are produced, nitrogen protection is needed, the catalyst needs to be ground into powder, etc., to provide a fast and efficient method for preparing 2- The method of cyanoethyl-5-norbornene-2-aldehyde

Method used

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  • Method for preparing 2-cyanoethyl-5-norbornadiene-2-aldehyde in micro-structural reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Such as figure 1 Shown: 5-norbornene-2-aldehyde A1 is transported into the first micro-mixer B1 (T-shaped three-way mixer, inner diameter: 1mm) to mix with the catalyst solution transported by A2, and the temperature of the first constant temperature water area D1 is 25°C , residence time 10s, then mixed with the acrylonitrile transported by A3 in the second micro-mixer B2 (T-type three-way mixer, inner diameter: 1mm), after mixing, enter (microchannel reactor) residence time extension tube C (inner diameter: 1mm), the temperature of the second constant temperature water area D2 is 60°C, the residence time is 7min, and finally enters the product collection bottle E. The mass ratio of feed 5-norbornene-2-aldehyde, acrylonitrile, toluene, potassium tert-butoxide to tert-butanol is 1:0.7:3:0.015, and the concentration of the tert-butanol solution of potassium tert-butoxide is 10 wt%. Total flow rate 1.143 mL / min. The solid content in the reaction solution was 1.24‰, and ...

Embodiment 2

[0020] Such as figure 1 Shown: 5-norbornene-2-aldehyde is transported by A1 into the first micro-mixer B1 (T-shaped three-way mixer, inner diameter: 1mm) and mixed with the catalyst solution transported by A2, the temperature of the first constant temperature water area D1 is 25 ℃, the residence time is 10s, and then mixed with the acrylonitrile second micro-mixer B2 (T-type three-way mixer, inner diameter: 1mm) delivered by A3, after mixing, it enters (microchannel reactor) residence time extension tube C (inner diameter: 1mm), the temperature of the second constant temperature water area D2 is 50°C, the residence time is 5min, and finally enters the product collection bottle E. The mass ratio of feed 5-norbornene-2-aldehyde, acrylonitrile, toluene, potassium tert-butoxide to tert-butanol is 1:1.47:3:0.02, and the concentration of the tert-butanol solution of potassium tert-butoxide is 14.8wt%. , the total flow rate is 1.78mL / min. The solid content in the reaction solution ...

Embodiment 3

[0022] Such as figure 1 Shown: 5-norbornene-2-aldehyde is transported by A1 into the first micro-mixer B1 (T-shaped three-way mixer, inner diameter: 1mm) and mixed with the catalyst solution transported by A2, the temperature of the first constant temperature water area D1 is 10 ℃, residence time 60s, and then mixed with the acrylonitrile second micro-mixer B2 (T-shaped three-way mixer, inner diameter: 1mm) delivered by A3, and then enter (microchannel reactor) residence time extension tube C (inner diameter: 1mm), the temperature of the second constant temperature water area D2 is 60°C, the residence time is 7min, and finally enters the product collection bottle E. The mass ratio of feed 5-norbornene-2-aldehyde, acrylonitrile, toluene, potassium tert-butoxide to tert-butanol is 1:0.9:2:0.015, and the concentration of the tert-butanol solution of potassium tert-butoxide is 10wt% total Flow rate 1.244mL / min. The solid content in the reaction solution was 2.71‰, and the conver...

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Abstract

The invention relates to a method for preparing 2-cyanoethyl-5-norbornadiene-2-aldehyde in a micro-structural reactor. The method comprises the specific steps that a tert-butyl alcohol solution of tert-butyl alcohol salt is used as a catalyst, toluene is used as a solvent, 5-norbornadiene-2-aldehyde and acrylonitrile serve as raw materials, mixing is performed in a micro-mixer of the micro-structural reactor, then the mixture enters a stay time extension tube to generate the 2-cyanoethyl-5-norbornadiene-2-aldehyde through reaction. The catalyst tert-butyl alcohol solution is dissolved in tert-butyl alcohol and then is dissolved in the toluene so that the catalyst can be evenly dispersed in a whole reaction system, the catalytic efficiency is improved, and raw material aggregation is reduced. Meanwhile, the method has the advantage of having string mass and heat transfer capability by utilizing the micro-structural reactor, and the reaction rate, selectivity and yield are greatly improved.

Description

technical field [0001] The invention relates to a method for 2-cyanoethyl-5-norbornene-2-aldehyde, in particular to a method for preparing 2-cyanoethyl-5-norbornene-2-aldehyde in a microstructure reactor method. Background technique [0002] CNC is an important intermediate product in the synthesis of 2-chloro-5-chloromethylpyridine from cyclopentadiene. In industrial production, 5-norbornene-2-aldehyde and acrylonitrile are used as raw materials, toluene is used as solvent, tert-butanol and potassium hydroxide are used as catalysts to react to obtain CNC. Because there are many materials involved in this reaction and the reaction time is long, some synthetic methods with different material ratios and reaction times have appeared. In patent CN101279931, CNC is prepared by first mixing potassium hydroxide, tert-butanol and toluene, adding AN under nitrogen protection, adding NC dropwise at about 30°C for 3 hours, and keeping warm for 2 hours after dropping. The molar ratio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/31
CPCC07C253/30C07C255/31
Inventor 张利雄陈超王重庆吴言富秦立华
Owner NANJING UNIV OF TECH
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