CS199162B1 - Continuous process for preparing n,n'-bisphenyldicarboxybenzendiamides - Google Patents

Description

Author of the invention HORYNA JAROSLAV ing., PARDUBICE ( ⁵⁴ ) A continuous process for the production of N, N * -bisphenyldicarboxybenzenediamides

SUMMARY OF THE INVENTION The present invention relates to a continuous process for the preparation of N, N * -bisphenyldicarboxybenzihdiamides from aromatic amines and diesters of benzenedicarboxylic acids.

The preparation of N, N * -hindered Idicarboxybene from endiamides in a batch process from aromatic amines and diesters of benzene dicarboxylic acids by gentle action at temperatures of 210 to 380 ° C is protected by Se. As a number of these diameters are attractive intermediates for the preparation of man-made fibers or large-scale tar dyes, the technical problem of their more rational production has arisen.

According to the present invention, Κ, Ν'-bisphenyldicarboxybenzenedlamides can be produced continuously from aromatic amines and diesters of benzenedicarboxylic acids by mixing said components in a selected ratio, homogenizing by heating and mixing, while introducing the liquid mixture into the flow reactor space wherein the temperature is maintained between 210-380 ° C and the residence time in the reaction zone is 10 minutes to 4 hours.

Virtually all aromatic amines processed by the novel process are either liquids or low melting solids. Of the diesters of benzenedicarboxylic acids has the highest

199 162 melting point of methyl terephthalate at 140 ° C; Thus, by heating mixtures of amines and esters, melt solutions of Si can easily be prepared. _x

Thus, at a predetermined molar ratio, the emission of the component, the mixture by heating is transferred to a liquid state, and the homogenized melt of the components is discharged into the reaction zone of the approved reactor. The choice of temperature and reaction time is interdependent, so that considerably longer time to achieve high conversion is required at about 210 ° C, while about 380% of time in some cases is 1 minute 10 minutes. In the course of the reaction ae, they release the volatile fumes which leave the reactors in the form of feathers. When operating in closed apparatuses, the volatile products increase the operating pressure, but by relieving the resulting overpressure, a relatively low pressure can be maintained above the system at the beginning of the reaction and the end product pressure.

In the new process, it is desirable to select a temperature mode in the reaction zone where both the starting components and products are in the molten state, or the melt is miscible and the liquid products - without mechanical inconvenience - leave the reactor. In order to ensure a smooth reaction, it is advantageous to select lower temperatures at the beginning of the reaction zone and higher temperatures at the end of the reaction zone; at the same time, the removal of volatile fumes is easy to operate.

Practically all types of horizontal and vertical flow reactors or cascade arrangement are suitable for the new production process.

In cases where an excess of amine is used, the excess amine can be removed from the final reaction mixture by distillation or directly from the flow reactor space.

He did

194.2 g of tarephthalic acid dimethyl ether (1 mol) are mixed and 372.5 g of aniline (4 mol) are heated to 145 ° C, mixed, and the resulting melt is sent by pump to a vertical pressurized stirred reactor to maintain the temperature. 350 ° C The melt of the reaction mixture is continuously discharged through the valve installed in the bottom of the apparatus and the exhaust gas is discharged through the valve located in the lid so that the overpressure in the working space does not exceed 1 MPa. >

Example 2

194.2 g of isophthalic acid dimethyl ether (1 mol) are mixed with 321.4 g of p-toluidine (3 mol), the mixture is heated to 170 and the melt is formed and further processed as in Example 1.

AND

SUBJECT. OF THE INVENTION

Claims (4)

SUBJECT. OF THE INVENTION A continuous process for the preparation of N, N * -bisphenyldlcarboxybenzenediamides of the general formula I Ar - NHCO - [- θ '- CONH-Ar (I) wherein Ar represents a benzene residue optionally substituted by one to two substituents such as methyl, chlorine, -OCH R 2, -OC 4 H 4, from the aromatic amines of formula II Ar NH _second r (II), wherein Ar is as hereinbefore defined, and benzene dicarboxylic acid diesters at temperatures of 210 to 380 ° C, characterized in that said components are mixed in a ratio of 2 to 1: 20: 1, homogenized by heating and mixing, whereupon the liquid mixture It introduces into the space of the flow zone, in which the reaction overpressure is maintained at 0.1 to 1 MPa, by the removal of volatile products. 2. A process according to claim 1, wherein the components pass through a zone and a variable temperature. 3. The process according to claim 1, wherein the temperatures in the reaction zone are selected to be higher than the melting points of the reaction mixture passing through and the melt is removed from the zone. 4. Process according to claim 1, characterized in that it is carried out in a closed reaction system from which the feathers of the more volatile reaction products are discharged.