SU506591A1 - Tris- / alkylimines / -1,3,5-triformylbenzene as rubber vulcanization accelerators - Google Patents

Description

- (0.066 mol) caustic soda in 10 ml of ethanol. Then the temperature of the reaction mixture is raised to 38–40 ° C and allowed to stand for 1 hour. After the end of the reaction, the contents of the flask are cooled, the precipitated sodium chloride is filtered off, the filtrate is dried with calcium oxide and subjected to fractional distillation. 3.24 g (66.8%) of tris-; ethyl imine) 1,3,5-triformylbeneol are obtained. PRI me R 2 Getting Tris- (about pilimina) 1,3,5-triformylbenzene. In a three-necked flask equipped with a reflux condenser, a thermometer, a dropping funnel and a stirrer, a solution of 1.62 g (0.01 mol) of 1,3,5-triformylbeneol is placed in 35 ml of ethanol and maintaining the temperature of the reaction mixture 20-t-25 ° C, a solution of 1.95 g (0.033 mol) of propylamine in 10 ml of ethanol is added dropwise. Then the temperature of the reaction mixture is raised to 38-40 ° C and stirred for 1 hour. At the end of the solution, the solution is dried with calcium oxide and subjected to fractional expansion. 1.79 g (62.7%) of tris (propylimine) 1,3,5-triformylbenzene are obtained. PRI me R 3. Obtaining Tris- (2-aminoethylenimine) 1,3,5-triformylbene ash. In a three-necked flask equipped with a reflux condenser, a thermometer, an addition funnel and a stirrer, 4.39 g (0.033 mol) of hydrochloric acid ethylene diamine, 50 ml of ethanol are placed and a solution of 2.64 g (0.33 mol) of caustic soda in 5 ml of ethanol. Then, keeping the temperature of the reaction mixture at 20-22 0, 1.62 g (0.01 mol) of 1,3,5-triformylbenzene are added in small portions, after which the reaction mixture is stirred for 1 hour at 38-40 ° C. After the end of the exposure, the precipitated sodium chloride precipitate is filtered off, the filtrate is dried with calcium oxide and the ethanol is removed under vacuum, the residue 2.13 g (73.9%) is tris (2-aminoethylenimine) 1,3,5-triformylbenzene . In tab. 1 shows the performance of the resulting azomethins of the general formula. , CH "N - R T. Tris- (alkylimino) 1,3,5-triformylbenzene tests as rubber vulcanization accelerators are carried out on samples of natural and SKI-3 rubbers under standard conditions. Rubber mixtures are prepared on laboratory rolls (type K-403, roll diameter 8, roll length 22 cm) at a roll temperature of 70-80 s for 13 minutes. The ingredients are introduced into rubber in the sequence: a) stearic acid, b) altax or azomethine, c) diphenylguanidine, d) zinc oxide, e) sulfur. The vulcanization process is carried out on a press in four-piece steel molds with a cell depth of 1 mm at 143 ° C for 30 minutes. The obtained rubber samples are tested on discontinuous machines RMI-60 according to GOST 270-64. In tab. 2 shows the composition of rubber mixtures 1-VI using the proposed vulcanization accelerators; in tab. 3 - mechanical properties of rubber. The results of the study are presented in table. 3 show that tris- (alkylimines) 1,3,5-triformylbenzene exhibit sufficient activity as rubber vulcanization accelerators. In terms of efficiency, they are close to an accelerator of a number of thiazoles (altaxus) (a razryu resistance at 20 ° G is 260-299 kgf / cm; the significant advantages of the proposed accelerators are that they are either liquids or low-melting substances, which makes it possible to improve the technological process and improve the quality of the rezingle, thanks to a more even distribution of the accelerator in the rubber compound, improved dosage of ingredients and improved production process as a whole.

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Claims (2)

Table 2. I. four . -bll j Formula of the Invention Tris- (alkylimines) 1,3,5-triformylbenzene of the general formula nn -CX CH-M506591 -12 where - alkyl or 2-aminoalkyl, as accelerators of vulcanization of rubbers,