Industrial method for producing iminodibenzyl from 2,2'-ethylenedianiline by catalytic deamination

Abstract

The invention discloses an industrial method for producing iminodibenzyl from 2,2'-ethylenedianiline by catalytic deamination. The industrial method comprises the following steps that 1, reaction materials are heated until the reaction materials are melted; 2, the reaction material melt is mixed with high-temperature steam and then the mixture enters into a deamination reactor and undergoes a deamination reaction in the deamination reactor which is an axial or radial fixed bed reactor with thin bed layers; 3, the high-temperature products discharged from the deamination reactor pass through a waste heat boiler so that heat is recovered and the high-temperature products are subjected to condensation to form liquid; 4, the liquid is fed into a gas-liquid separation tank and crystallizes in water in a lower part of the gas-liquid separation tank; and 5, iminodibenzyl crystals and the like are obtained by crystal-water separation in a liquid-solid separation tank, wherein the most of steam discharged from an upper part of the gas-liquid separation tank orderly passes through a filter, a superheater and a compressor and then returns back to a heating furnace for recycle and the rest of the steam is discharged. The industrial method provided by the invention has the characteristics of good reaction performances, and low raw material consumption and energy consumption.

Description

technical field [0001] The invention belongs to the technical field of chemical reaction engineering, and specifically relates to an industrial production method for catalytic deamination of iminodibenzyl, a pharmaceutical intermediate. Background technique [0002] Iminodibenzyl (10,11-dihydro-5H-dibenzo[b,f]azepine, referred to as IDB) is an important drug synthesis intermediate, mainly used in carbamazepine and oxcarbazepine drugs Synthesis. [0003] Using 2,2'-diaminobibenzyl (DADB for short) to synthesize iminodibenzyl is a method widely used in industry, mainly including thermal deamination of 2,2'-diaminobibenzyl dioate, 2,2' -Diaminobibenzyl liquid phase catalytic deamination, 2,2'-diaminobibenzyl concentrated phosphoric acid deamination and 2,2'-diaminobibenzyl gas phase catalytic deamination method. The pyrolytic deamination method of 2,2′-diaminobibenzoate is the earliest method for synthesizing iminodibenzyl. The process of this method is simple, but the decomp...

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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

The above-mentioned method for producing iminodibenzyl by catalytic deamination of 2,2'-diaminobibenzyl is a laboratory preparation method, and the production process during industrial scale production is not proposed. The reaction device is an experimental device, and the catalyst has a short service life. Seriously insufficient

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