RU1818329C - Process for manufacturing organopolysiloxanes - Google Patents

Abstract

Usage: a binder in the manufacture of fiberglass, for protective coatings, as additives to acrylate dispersants, waterproofing agents. SUBSTANCE: polymerization of a 10-45% solution in a non-polar solvent of the products of hydrolytic condensation of methyltrichlorosilane or its mixture with dimethyldichlorosilane in the presence of an alkaline catalyst. A linear dependence of the relative viscosity of a 10% solution of oligoorganosiloxanes on the polymerization time is provided. 2 ill.

Description

The invention relates to methods for producing organosilicon polymers, namely the polymerization of products of hydrolytic condensation of methyltrichlorosilane or a mixture thereof with dimethyldichlorosilane.

The aim of the invention is to provide the ability to control the polymerization process and organize it in a continuous mode.

This goal is achieved by the fact that in the process for preparing polyorganosiloxanes by polymerizing a solution of oligorganosiloxanes in a non-polar solvent in the presence of an alkaline catalyst, a 10-45% solution of the hydrolytic condensation products of methyltrichlorosilane or a mixture thereof with dimethyldichlorosilane is used as an oligoorganosiloxane solution.

With an increase in the concentration of oligomethylsiloxanes of more than 45 wt% in the reaction mass, the linear dependence of the relative viscosity on the polymerization time is not observed. At a concentration of less than 10 wt.%, It is not possible to determine the relative viscosity of a 10% solution.

Alkaline polymerization of a 10-45% toluene solution of oligomethylsiloxanes allows a linear dependence of the relative viscosity on the polymerization time to be obtained, which, in turn, allows one to predict the course of polymerization at the initial stage of the process. The absence of an increase in the polymerization rate while achieving a relative viscosity (1.9-2.0) prevents the formation of overpolymerized and crosslinked products.

PRI me R 1 (control). A reaction mixture consisting of 16% by weight of dimethyldichlorosilane and 37% by weight of phenyl trichlorosilane. 47 wt.% Toluene, hydrolysis00

s y

H)

They are removed by known methods, followed by distillation of the excess toluene. To 200 g of a toluene solution of oligomethylphenylsiloxanes (wt.% Oligomethylsiloxanes 61.6%) was added 6 g of a 10% alcohol solution of KOH. The change in the relative viscosity of a 10% solution of polymethylphenylsiloxanes in toluene is shown in FIG.

Example 2 A reaction mixture consisting of 18.1 wt.% Methyltrichlorosilane, 20.3 wt.% Dimethyldichlorosilane, 61.6 wt.% Toluene is hydrolyzed by known methods, followed by distillation of excess solvent. To 211 g of a toluene solution of oligomethylsiloxanes (May, 45% oligomethylsiloxanes), 4.7 g of a 10% alcohol solution of KOH are added. The change in the relative viscosity of a 10% solution of oligomethylsiloxanes in toluene is shown in Fig.2.

Example 3. The reaction mixture, consisting of 24.7 wt.% Methyltrichlorosilane, 9.1 wt.% Dimethyldichlorosilane, 66.2 wt.% Toluene, is hydrolyzed by known methods, followed by washing with clarification.

To 200 g of a toluene solution of oligomethylsiloxanes (wt% oligomethylsiloxanes 18.0%), 4.4 g of a 10% alcohol solution of KOH are added. The change in the relative viscosity of a 10% solution of oligomethylsiloxanes in toluene is shown in Fig.2.

Example 4. A reaction mixture consisting of 34.6 wt.% Methyltrichlorosilane, 65.4 wt.% Toluene is hydrolyzed by known methods, followed by washing with clarification.

To 102.6 g of a 19.0% toluene solution of oligomethylsiloxanes, 92.4 g of tolurl is added (May, the proportion of oligomethylsiloxanes in the reaction mass is 10.0%). After stirring for 15 minutes, 1 g of a 10% alcohol solution of KOH was added. The change in the relative viscosity of a 10% solution of oligomethylsiloxanes in toluene is shown in Fig.2.

PRI me R 5 (control). The reaction mixture, consisting of 18.1 wt.% Methyltrichlorosilane, 20.3 wt.%

dimethyldichlorosilane, 61.6 wt.% toluene, is hydrolyzed by known methods, followed by distillation of the excess solvent. To 193 g of a toluene solution of oligomethylsiloxanes (May 50% oligomethylsiloxanes), 4.75 g of a 10% alcohol solution of KOH was added. The change in the relative viscosity of a 10% solution of oligomethylsiloxanes in toluene is shown in Fig.2.

Claims (1)

The claims A method of producing polyorganosiloxanes by polymerization of a solution of oligoorganosiloxanes in a non-polar solvent in the presence of an alkaline catalyst, characterized in that, in order to provide the possibility of regulating the process and organizing it continuously from the time of polymerization, oligoorganosiloxanes are used 10-45% solution of hydrolytic condensation products of methyltrichlorosilane or its mixture with dimethyldichlorosilane. Figure 1 3 (L $ iPerch) 2 Editor (D j j b Compiled by N. Pr and P 1, h YU Prostorova Tehred M. Morgenthal Corrector L. Livrints Example 7 8 g, h and P 1, h ctor L. Livrints Figure 2