SU527453A1 - Method for preparing fluorinated polybenzimidazoles - Google Patents

Description

(54) METHOD FOR OBTAINING FLUORINATED POLY BENZYM AND DAZOLES The satisfactory solubility of the obtained polybenzimidaeols is achieved by using one fluorine-containing amine to obtain them. The use of both fluorine-containing components significantly increases the solubility of polymers. Fluorine-containing polybenzimidazoles are obtained in an inert gas flow under conditions of high-temperature polycondensation in a block in two stages. At first, at a temperature of 180220 ° C, a fluoropolymer is obtained, which, at a temperature of 300-32 ° C and evacuating for 0.5-3 hours, either in the same block, or after being removed from the block directly in the product, is converted into a high molecular weight product. Example 1. A mixture of 3.64 g of 0.01.-mol) 2,2-bis (m, p-diaminophenylene) -hexafluoropropane and 3.18 g (0.01 mol of isophthalic acid diphenyl ester are loaded into a condensation tube. Reaction inert gas is conducted in. The tube is placed in a block heated to 220 ° C and then the reaction is carried out according to the following mode: Temperature rise to 260 ° C, hour, 0, Exposure (per hour) at temperature, C: 260 0.5 270 2.5 . 290 2.0 300 0.5 (without vacuum) 300 0.5 (under vacuum) The reduced viscosity of a 0.5% aqueous solution of polybenzimidazole in formic acid is 20 C, 0.83 an / g. The polymer obtained is soluble on the ode in sulfuric and formic acids and dimethyl sulfoxide, and in amide solvents - when heated. Example 2. Mix 3.64 g (0.01 mol) 2,2-bis (AA, p-diaminophenylene) -hexafluoropropane and 3, 18 g (O, O1 mol of terephthalic acid diphenyl ester. The reaction is carried out as in Example 1. The expected viscosity of a 0.5% aqueous solution of the polymer in formic acid is 1.10 dL / g. The solubility of the polymer is similar to the solubility of the polymer in Example 1. Example 3. Mix 3.64 g (0.01 mol) of 2,2-bis (M, P - diaminophenylene) -hexafluoropropane and 5.44 g (0.01 mol) of 2.5-bis diphenyl ether (P -carboxyenyl) -hexafluoropropane. The reaction is carried out in accordance with Example 1 according to the following temperature regime: Loading into the unit at a temperature, C Exposure d (B hour) Poi temperature C: 270 (without vacuum) 27O (under vacuum) 29O (under vacuum) Reduced viscosity 0.5% a solution of polybenzimidazole in formic acid at 20 C is 0.5 dl / g. The polymer obtained is heated additionally under vacuum in the following mode:. Load into block at temperature, Ql-ZOO Exposure (per hour) at temperature, C: ZOO-1.0 310 1.0 32O1, O The reduced viscosity of 0.5% solution of the polymer in formic acid at 20 C is 0 , 89 dl / g. The paci polymer is cold in sulfuric and formic acids, dimethyl sulfoxide and, with slight heating, in amide solvents. Fluorine-containing polybenzimidazoles are high-molecular-weight heat-resistant polymers, which allows their use as a coating, binder, and glue in various sectors of the national economy. Fluorine-containing polybenzimidazoles obtained by the proposed method have high thermal characteristics and increased solubility. Thus, the data of thermogravimetric and differential thermal analyzes indicate the presence of weight loss only at a temperature of 500 ° C (for a prototype of 220 ° C). In addition, the obtained fluorine-containing polybenzimidazoles have high heat resistance (do not soften to a decomposition temperature of 49 ° -50 ° C). In tab. 1 and 2 and 2 shows the comparative data on the solubility of the proposed polymers and the prototype, in table. 2 - weight loss.

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Claims (3)

Prototype Decomposes with Prototype Formula 1. Investigation of the preparation of fluorinated polylbenimidazoles by melt polymerization of aromatic tetramine and diphenyl aromatic dicarboxylic ester in a melt, which is used in order to improve the heat resistance and solubility of polymers, E as an aromatic tetramine used, iro used in the aromatic tetramine is used as an aromatic tetramine. (m, l (-diaminophenylen) -hexaftopropan. 2 .., a guide to paragraph 1, about the t h and h and t and is with the fact that as dfenilovoyu aromatic dicarboxylic acid ester and completely at 70-80 ° C Also Completely at 50-60 ° С Partially at 120-140 С Table 2 Above 21O C temperature is 2,2-bis (p -carboxyphenyl) -hexafluoropropane diphenyl ether. Sources of information taken into account in the examination: 1. Dolgoplask B, D., Grussalimsky B.L., to others. Study of polybenzimidazoles. Reports of the Academy of Sciences of the USSR, 120, 783-788, 1958. 2. Korshak V.V. Synthesis and investigation of the properties of homogeneous and mixed polybenzimidazoles. High Molecular Compounds 6, No. 7, 1251, 1964. 3. Yakubovich A, Ya. Fluorinated polybenzimidazoles. High Molecular Compounds, 6, No. 5, 838. 1964 Prototype.