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System and method for synthesizing cyclohexanone-oxime by micro-reactor

A technology of microreactor and cyclohexanone oxime, which is applied in oxime preparation, organic chemistry, etc., can solve the problems of large material retention, local hot spots, and large volume, so as to improve controllability, safety, and material retention small effect

Active Publication Date: 2015-11-04
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still some problems in this reaction device: firstly, the volume of the slurry bed reactor is large, and the effect of mechanical stirring is poor, which easily leads to uneven distribution of reactant concentration and local hot spots; secondly, the stagnation of materials in the reactor is large, Once a large amount of hydrogen peroxide is decomposed, it will cause a safety accident

Method used

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  • System and method for synthesizing cyclohexanone-oxime by micro-reactor
  • System and method for synthesizing cyclohexanone-oxime by micro-reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Equipment parameters: the first micro-mixer 1 is a micro-mesh mixer, and the second micro-mixer 2 is a T-shaped micro-channel mixer. Among them, the micro-sieve mixer contains 20 micro-sieves with a diameter of 0.05 mm, and the hydraulic diameter of the T-shaped micro-channel is 0.1 mm.

[0027] Operating conditions: the concentration of titanium silicon molecular sieve in raw material A is 0.1wt%, the concentration of ammonia is 1wt%, and the molar ratio of ammonia to cyclohexanone is 2.5. The concentration of hydrogen peroxide in raw material B is 1 wt%, and the molar ratio of hydrogen peroxide to cyclohexanone is 1. The reaction temperature is 90° C., the reaction pressure is 0.2 MPa, and the reaction residence time is 20 minutes.

[0028] Reaction result: the conversion rate of cyclohexanone is 98.2%, and the selectivity of cyclohexanone oxime is 99.8%.

Embodiment 2

[0030] Equipment parameters: the first micro-mixer 1 is a micro-mesh mixer, and the second micro-mixer 2 is a Y-shaped micro-channel mixer. Among them, the micro-sieve mixer contains a micro-sieve with a diameter of 5mm, and the hydraulic diameter of the Y-shaped microchannel is 6mm.

[0031] Operating conditions: the concentration of titanium silicon molecular sieve in raw material A is 10wt%, the concentration of ammonia is 15wt%, and the molar ratio of ammonia and cyclohexanone is 1.5. The concentration of hydrogen peroxide in raw material B is 10wt%, and the molar ratio of hydrogen peroxide to cyclohexanone is 1.5. The reaction temperature is 60° C., the reaction pressure is 0.5 MPa, and the reaction residence time is 3 minutes.

[0032] Reaction result: the conversion rate of cyclohexanone is 99.8%, and the selectivity of cyclohexanone oxime is 99.0%.

Embodiment 3

[0034] Equipment parameters: the first micro-mixer 1 is a micro-mesh mixer, and the second micro-mixer 2 is a cross-shaped micro-channel mixer. Wherein, the micro-sieve mixer contains two micro-sieves with a diameter of 4mm, and the hydraulic diameter of the cross-shaped microchannel is 4mm.

[0035] Operating conditions: the concentration of titanium silicon molecular sieve in raw material A is 8wt%, the concentration of ammonia is 12wt%, and the molar ratio of ammonia and cyclohexanone is 2. The concentration of hydrogen peroxide in raw material B is 8wt%, and the molar ratio of hydrogen peroxide to cyclohexanone is 1.5. The reaction temperature is 70° C., the reaction pressure is 0.4 MPa, and the reaction residence time is 5 min.

[0036] Reaction result: the conversion rate of cyclohexanone is 99.6%, and the selectivity of cyclohexanone oxime is 99.5%.

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Abstract

The invention discloses a system and a method for synthesizing cyclohexanone-oxime by a micro-reactor and belongs to the field of chemical reaction engineering. The system is composed of a first micro-mixer, a second micro-mixer, a reaction pipeline provided with a heat exchange jacket and a counterbalance valve which are connected in series. The method comprises: firstly mixing slurry containing a titanium silicon molecular sieve and ammonia with a hydrogen peroxide solution by using the first micro-mixer; then dispersing cyclohexanone into the mixed slurry by using the second micro-mixer to initiate ammoximation reaction; and finally accomplishing the reaction process in the reaction pipeline. The system can achieve a high conversion rate (greater than 99%) and high selectivity (greater than 99%) within a reaction time of 0.5-20 minutes. The material stagnation amount of materials in the micro-reaction system is small, so that the controllability and the safety of ammoximation reaction are improved.

Description

technical field [0001] The invention belongs to the field of chemical reaction engineering, and in particular relates to a system and a method for synthesizing cyclohexanone oxime with a microreactor. Background technique [0002] Caprolactam is an important basic organic chemical used in the synthesis of nylon 6 fibers and nylon 6 engineering plastics. It is widely used in textiles, automobiles, electronics and other industries, and plays an important role in the development of the national economy. With the rapid development of my country's economy, the demand for caprolactam is increasing year by year. In 2013, the apparent consumption of caprolactam in my country has reached 1.5 million tons. The development and utilization of caprolactam in my country has a very broad prospect. Cyclohexanone oxime is a key intermediate for the production of caprolactam from cyclohexane. At present, about 80% of caprolactam in the world is obtained through Beckmann rearrangement of cy...

Claims

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Application Information

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IPC IPC(8): C07C251/44C07C249/04
Inventor 骆广生董晨王凯张吉松
Owner TSINGHUA UNIV
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