SU388591A1 - Method for preparing carborane-containing polyamides - Google Patents

Description

The invention relates to the production of heterochain, barrister-containing polymers, which are promising for the use in the manufacture of heat-resistant and peitron-capturing materials.

One type of boron-containing polymers are polyamides with carborane drami. They are synthesized by the polycondensation of diamines with 1,2-bis {pcarboxyphenyl) -o-carboran, 7-bis (n-car6oxyfepyl) -uI-carboran, and dichlorides of m- and -carborane dicarboxylic acids.

(j BioHiD with

fiNHj,

in order to expand the range of aromatic boron-containing polyamides, but the proposed method is 1.7-byc (g-aminofeni.h) - Ucarborane is subjected to solution polycondensation with dicarboxylic acid dichlorides. To obtain an iolmnd, a solid powdered dichlorohydride is added at room temperature to a solution of the abovementioned diamine in a polar solvent inert to the dichlorohydrin hydride, and the mixture is stirred until the polycondensation proceeds according to the following scheme:

NHj + g, ClGOArCOC

С-BioH-io С С

where Ar is a bivalent aromatic radical.

Depending on the basicity of the solvent, the polycondensation is carried out in the presence of acceptors of hydrogen chloride released during the reaction.

The obtained boron-containing polyamides are white fibrous substances, well soluble in organic

MNSOAGSO-1 l

solvents, heat resistant up to -250 ° C. From the solution in tetrahydrofuran, they form colorless transparent films.

Example 1. To a solution of 1.7-bms (/ g-aminophenyl) -zh-: carborate mixed in an inert gas stream with the addition of 0.26 ml of triethylamine in 5 ml of tetrahydrofuran, 0.19 g of teraphthalic acid dichloride is added at room temperature. Reak3

This mass is stirred for 1 hour and mixed with water. The colorless fibrous polymer is filtered off, washed with water, acetone and dried in vacuum ppn 70-80 ° C.

-Exit and full-grams 0.4 g (95%). The reduced viscosity of a 0.5% aqueous solution of a polymer in dimethylformamide at 25 ° С is 0.47 d.iiz. The softening temperature of the thermo-chemical curve is 300 ° C. When heated in air up to 450 ° C, the polymer loses 11% in weight. Elementary analysis of the polymer: Found,%: C 57.05; 56.96; H 5.46; 5.66; B 22.31; 22.14; N 5.82; 4.42.

C22H24BioN202.

Calculated, o / o: C 57.86; H 5.29; B 23.63; N 6.13.

EXAMPLE 2 Polyamide is prepared under the conditions of the previous example, with the difference that dichlorohydroxyd4,4-dicarboxylic acid dichlorohydride is used as the dichloride.

four

Polymer yield -100%. Its reduced viscosity is 0.28 for 1 g, the softening temperature is 250 ° C, and the weight loss during heating is 400 ° C –7%.

Example 3. Polyamide is prepared under the conditions of Example 1 with the difference that dichlorohydride ((-carboranicarboxylic acid) is used.

The output of the polymer is -100%. Its reduced viscosity is 0.34, softening temperature is 240 ° C.

Claims (1)

Invention Formula The method of obtaining carborane-containing polyamides, distinguished by the fact that, in order to expand the range of aromatic boron-containing polyamides, 1-bis (pomnophenyl) -zh-carborane is subjected to solution polycondensation with aromatic dicarbopic acid dichlorides.