Integrated industrial production method for producing iminostilbene by continuous catalytic deamination and catalytic dehydrogenation of 2,2'-diamino-bibenzyl

A diaminobibenzyl catalytic deamination and catalytic dehydrogenation technology, which is applied in the chemical industry, sustainable manufacturing/processing, organic chemistry, etc., can solve the problems of severe decomposition of raw materials and products, low utilization rate, and poor product quality , to achieve the effect of increasing life, improving utilization rate and reducing energy consumption

Inactive Publication Date: 2012-05-02
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

The pyrolytic deamination method of 2,2′-diaminobibenzoate is the earliest method for synthesizing iminodibenzyl. The process of this method is simple, but the decomposition of raw materials and products in the reaction engineering is serious, resulting in low yield and product poor quality
The product quality of 2,2′-diaminobibenzyl liquid-phase catalytic deamination method is good, but the yield is low
The concentrated phosphoric acid deamination method of 2,2′-diaminobibenzyl has better quality and higher yield, but requires higher equipment
[0010] In summary, in the above-mentioned method for producing iminostilbene, no continuous integrated industrial production method for producing iminostilbene by continuous catalytic deamination and catalytic dehydrogenation of 2,2'-diaminobibenzyl has been found yet; Both the preparation of iminostilbene from aminodibenzyl and the preparation of iminodibenzyl from 2,2'-diaminobibenzyl use steam with a high molar ratio as diluent and heat carrier. In the step-by-step reaction preparation method, water vapor only participates One reaction, the utilization rate is not high, resulting in high energy consumption, and insufficient auxiliary equipment

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  • Integrated industrial production method for producing iminostilbene by continuous catalytic deamination and catalytic dehydrogenation of 2,2'-diamino-bibenzyl
  • Integrated industrial production method for producing iminostilbene by continuous catalytic deamination and catalytic dehydrogenation of 2,2'-diamino-bibenzyl
  • Integrated industrial production method for producing iminostilbene by continuous catalytic deamination and catalytic dehydrogenation of 2,2'-diamino-bibenzyl

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Embodiment 1

[0036] 2,2′-Diaminobibenzyl gas-phase catalytic deamination and catalytic dehydrogenation to produce iminostilbene and figure 1 The process flow is carried out, the molar ratio of water vapor to 2,2'-diaminobibenzyl is 300, 2,2'-diaminobibenzyl is sent into DADB raw material tank 1, melted under the heating of water vapor, and then passed through DADB The metering pump 2 sends it to the DADB mixer 3; the water is heated to 580°C in the heating furnace 4, sent to the intermediate heat exchanger 6 to heat the product of the deamination reaction, and sent to the DADB mixer 3 after heat exchange. In DADB mixer 3, 2,2'-diaminobibenzyl is mixed with high-temperature steam to reach a deamination reaction temperature of 420°C, and then enters deamination reactor 5 for catalytic deamination reaction, deamination reactor 5 The inlet pressure is 250kPa, and the reaction product enters the intermediate heat exchanger 6 and is heated to a dehydrogenation reaction temperature of 550°C by hi...

Embodiment 2

[0038] 2,2′-Diaminobibenzyl gas-phase catalytic deamination and catalytic dehydrogenation to produce iminostilbene and figure 2 The process flow is carried out, the molar ratio of water vapor to 2,2'-diaminobibenzyl is 400, 2,2'-diaminobibenzyl is sent into DADB raw material tank 1, melted under the heating of water vapor, and then passed through DADB The metering pump 2 transports it to the DADB mixer 3; the water vapor is heated to 540°C in the heating furnace 4, sent to the intermediate heat exchanger 6 to heat the product of the deamination reaction, and sent to the DADB mixer 3 after heat exchange. In the DADB mixer 3, 2,2'-diaminobibenzyl is mixed with high-temperature steam to reach a deamination reaction temperature of 400°C, and then enters the deamination reactor 5 for catalytic deamination reaction, and the deamination reactor 5 The inlet pressure is 90kPa, the reaction product is mixed with the recovered intermediate product iminostilbene, then enters the intermed...

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Abstract

The invention provides a continuous integrated industrial production method for producing iminostilbene by the catalytic deamination and catalytic dehydrogenation reaction of 2,2'-diamino-bibenzyl. The method comprises the following process flows of: mixing the 2,2'-diamino-bibenzyl with high-temperature water vapor; adding the mixture into a catalytic deamination reactor; after reaction, performing heat exchange on a reaction material through an intermediate heat exchanger; adding the reaction material into a catalytic dehydrogenation reactor; and treating the material which is taken out of the reactor to obtain the iminostilbene. The method is a continuous integrated process of the catalytic deamination and catalytic dehydrogenation reaction, and has the characteristics of simple reaction process, low energy consumption, small equipment investment and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical reaction engineering, and specifically relates to a continuous industrial production method of catalytic deamination and catalytic dehydrogenation for preparing a pharmaceutical intermediate iminostilbene. Background technique [0002] Iminostilbene (5H-dibenzo[b,f]azepine, referred to as IS) is an important drug synthesis intermediate, mainly used in the synthesis of carbamazepine and oxcarbazepine. [0003] Synthesis of iminostilbenes with iminodibenzyl (10,11-dihydro-5H-dibenzo[b,f]azepine, referred to as IDB) is a method widely used in industry, mainly bromination method, liquid phase catalysis Dehydrogenation method and gas phase catalytic dehydrogenation method. The bromination method is the earliest industrial method for the production of iminostilbene. The iminodibenzyl is prepared by acylation, bromination, dehydrobromination, deacylation and other multi-step methods. This method has lo...

Claims

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Application Information

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IPC IPC(8): C07D223/22
CPCY02P20/10
Inventor 李瑞江朱子彬吴勇强张琪黄震尧刘时贤倪燕慧陶国忠
Owner EAST CHINA UNIV OF SCI & TECH
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