SU550405A1 - The method of obtaining phenolamine resins - Google Patents

Description

Tablets 1

Strength of adhesion to calico vulcanized rubber compounds

table 2

Characteristics of carboxyl-containing

Feiolamine resins depending on the content

salicylic acid in the original mixture

10% salicylic acid; 25% salicylic acid was added to sample B-72. The use of a mixture of salicylic acid with an alkylphenol or arylalkylphenol as a phenolic component is recommended when it is necessary to obtain a phenol amine resin containing carboxyl groups, and at the same time, well soluble in organic solvents. In addition, the use of salicylic acid for the preparation of phenolamine resins in combination with alkylphenols in arylalkylphenols makes it possible to obtain a resin that can be dissolved in aqueous alkali. Due to such properties, the scope of application of resins is expanded, for example, for combination with rubbers in a latex stage. Below are the results of laboratory testing of the proposed method for the preparation of phenolamine resins containing carboxyl groups. P r and measures 1. In a flask with a stirrer, 23.6 g (0.17 mol) of salicylic acid, 4 g (0.29 mol) of hexamethylene tetramine are loaded and heated to 150 ° C. Ammonia emissions are observed. After 20 minutes, the contents are poured onto a baking sheet. The reaction mixture solidifies to amber mass. The dropping point of the obtained product is 129.5 ° C; it is insoluble in benzene and toluene. The resin is dissolved in an aqueous solution of caustic soda. Example 2. In the flask load 10 g (0,072 mol) of salicylic acid, 75 g (0.34 mol) of technical octylphenol and 15 g (0.07 mol) of hexamethylenetetramine. The reaction mass is heated and maintained at 145 ° C for 120 minutes. The resulting product is an amber-colored melt with a dropping point of 141 ° C. In tab. Figure 2 shows the characteristics of carboxylsoderyl phenolamine resins, depending on the content of salicylic acid in the initial mixture. The weight ratio of the mixture octylphenol and salicylic acid to hexamethylenetetramine in all cases is 6: 1. All resins are soluble in aqueous solution of caustic soda. Example 3. In the reaction flask equipped with a thermometer and a stirrer, load 60 g (0.4 mol) rt-tert.butylphenol, 10 g (0.0714 mol) of hexamethylenetetramine and 7.8 g (0.0565 MOTH, 10% of the total weight of the mixture) salicylic acid. The reaction mixture is heated to a temperature of 150 ° C. The reaction starts in the first 3 to 5 minutes and is accompanied by a vigorous release of ammonia. The mixture was kept at 150 ° C for one and a half hours, then, in a heated state, was poured into the pan and the resulting mass solidified as a solid, brittle amber resin. The drop point is 140 ° C. Example 4. Technical "-phenylethylphenol 90 g (0.454 mol) and hexamethylenetetramine 15 g (0.107 mol) in a weight ratio of 6: 1 were charged to a reaction flask equipped with a stirrer and a thermometer and added in a weight ratio of 6: 1 and 11.7 g (0.08 mol; 10% of the total weight of the reaction mixture) salicylic acid. The mixture is heated in an oil bath to 150 ° C. In the first 5 min of the reaction, the reaction mass is heated and ammonia is released. Table 3 The mixture was kept for one and a half hours with stirring, and then poured into a cellophane boat in a hot condition. The resulting product solidifies to a hard, brittle, dark amber resin with a dropping point of 121 ° C. The resin obtained by the proposed method, was tested as a stabilizer of rubbers, entering them in an amount of 1 weight. hours in styrene butadiene rubber.

The control sample is rubber with the addition of 1.2% neozone D.

Samples were tested for stability under heat aging conditions (140 ° C for 30 min with the control of Wallace plasticity).

Claims (1)

Invention Formula The method of obtaining phenolamine resins by condensation of the substituted phenol with hexamethylenetetramine at a temperature of 70-180 ° C, characterized in that salicylic acid or a mixture of salicylic acid with alkyl is taken as a substituted phenol to obtain resins that increase in adhesion of rubber and alkali-soluble -, aryl alkylphenols in the ratio I: 100-100: 1 with a molar ratio of substituted phenol and hexamethylenetetramine 1: 0.02-1.