SU952843A1 - Process for producing rubber stock stabilizer including polymeric 2,2,4-trimethyl-1,2-dihydroquinoline and 6-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline - Google Patents

Description

There is also known a method of obtaining santohin, consisting of the following operations;

liquid phase condensation of p-phenetidine with acetone in the presence of 20% hydrochloric acid at 130160 ° C and a molar ratio of p-phenetidine, acetone and hydrogen chloride 1: 2.3-3.6: 0.1-0.25, respectively ; with a process time of 5-6 hours, the conversion of p-phenetidine reaches 6065,

- Neutralization of the reaction mass, previously separated from excess acetone, with an aqueous solution of sodium alkali with simultaneous extraction with toluene / washing the extract with water from chlorine ions; distilling off the extractant, then, by vacuum rectification, the residual p-phenetidine to obtain the technical product in the vat residue and vacuum-distillation of the latter to obtain the product Santokhin in the distillate.

To obtain acetonanil PC stabilizer to acetonanil P, which is in the state of melt, at 100-180 ° C and stirring, the calculated amount of santochin is added, after which the melt is cooled and crystallized.

The disadvantages of this method of producing acetonanyl PC include the presence of separate productions of stabilizer ingredients, adding with acetonanil P to the blend stabilizer the following quantities (up to 15%) of p, n-diamino-2,2-diphenylpropane are compounds with primary amine groups, which are the processing of rubber compounds causes such an undesirable phenomenon as premature scorching (scorching), as well as a tendency to sticking the scales of the mixture stabilizer when the ambient temperature rises to 35-40 ° C.

The aim of the invention is to simplify the technology for obtaining the acetonanyl PC stabilizer and improve its quality.

The goal is achieved according to the method for producing a stabilizer of rubber mixtures, including polymer 2,2,4-trimethyl-1,2-Igidrohinolin and 6-ytoxy-2,2,4-trimethyl-1, 2-dihydroquinoline, namely, aniline and p-phenetidine together condense with acetone in the presence of 27-33% hydrochloric acid in the liquid phase under pressure at 130-160 ° C and the molar ratio of the starting aniline, p-phenetidia, hydrogen chloride and acetone 1: 0.09-0 , 20: 0.1-0.25-2.2-3, 6, respectively, followed by the distillation of excess acetone, polymerization of the obtained reaction th mass at 95-105 C in the presence of 20-25% hydrochloric acid relative content of 0.7-0.9 moles of hydrogen chloride to the total amine nitrogen and then isolation of the desired polymer product.

The proposed method allows not only eliminating the technological: thread (and the production costs associated with it) for obtaining 6-ETOXI-2,3,4-trimethyl-1,2-dihydroquinoline, but also to obtain the target product of higher quality for. by detecting a decrease in p, n-diamino-2,2-diphenylpropane (no more than 8%), and the lack of a tendency for sticking to scales.

In addition, the following favorable factors were identified in the combined process, which allow it to successfully implement in the existing hardware and technological design of acetonanil production P an increase in the rate of condensation of n-phenetidine with acetone, preservation of the necessary homogeneity of mixtures during the condensation and polymerization stages from An; Shna p-phenetidine is not homogenized with acetone in the presence of hydrochloric acid with a concentration of more than 20%, and 6-ethoxy-2, 2,4-trimethyl-1,2-dihydroquinoline, in contrast to 2,2,4- trimethyl-1,2-dihydro quinoline, gives a salt with hydrogen chloride, is practically insoluble in water).

Example 1. A pre-homogenized mixture of the following composition is loaded into a 150 ml titanium autoclave with a thermocouple, a pressure gauge and a stirrer:

Anilin44,65

p-Fenetidin7,88

Sol Na Acid

(28%) 9.81

Acetone71,72

wherein the molar ratio of aniline, p-phenetidine, hydrogen chloride and acetone is 1: 0.124 0.157: 2.584, respectively.

With stirring and a temperature of 150 ° C, the mixture is kept in an autoclave for 6 hours, the maximum developed pressure being about 10 atm. At the end of the completion, the autoclave is cooled and the contents transferred to a distillation flask, from which, then, excess acetone is distilled off. The remaining mass is transferred for polymerization into a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, placed in a glycerin bath with a temperature of 100-105 ° C, 61.4 g of 32% hydrochloric acid is added to the mixture, after which

Claims (1)

A method for producing a rubber compound stabilizer comprising polymer 2,2,4-trimethyl-1,2-dihydro35 quinoline and b-ethoxy-2,2,4-trimethyl-1,2-dihydroquinoline is distinguished. The reason is that, in order to simplify the technology and improve the quality of the target product, aniline and η-phen40 thidine are jointly condensed with acetone in the presence of hydrochloric acid with a concentration of 27-33% in the liquid phase under pressure at 130-160 ° C and the molar ratio of aniline, p-phenethidine, 45 hydrogen chloride and acetone 1: 0.090.20: 0.1-0.25: 2.2-3.6, respectively, then excess acetone is distilled off from the reaction mass and polymerized in the presence of hydrochloric 5θ acid with a concentration of 20-25% and a relative content of hydrogen chloride of 0.7-0.9 mol from wearing to total amine nitrogen at 90-105 ° C.