CS240593B1 - Organo-silicon esters and method of their preparation - Google Patents

Description

CZECHOSLOVAK SOCIALISTIC B 0 n 1 1 / A DESCRIPTION FOUND TO COPYRIGHT CERTIFICATE 240593 (11) (Bl) (51) Int. Cl.4 C 07 F 7/08 C 07 F 7/18 (W) (22) Logged in 21 03 84 (21) (PV 2030-84) OftAD FOR VYNA LEZY (40) Posted on 18 07 85 (45) Published 15 08 87 AND DISCOVERIES (75)

Author of the Invention SASÍN MIROSLAV ing; CSERM, JIŘÍ, CSc., PARDUBICE (54) Organosilicon esters and their preparation (1

The invention relates to organosilicon esters and a process for their preparation from phenyltrichlorosilane, 1,4-butanediol and monovalent alcohols. It is a new type of ester for use as a component of synthetic oils and hydraulic fluids.

The novel organosilicon esters of the formula (6 ') 5-SiO 2 5 - (3) where x = 1, 3, 10 are prepared according to the invention by gradual esterification of phenyltrichlorosilane with 1,4-butanediol and 2-ethylhexanol at 70 to 120 ° C, with hydrogen chloride through a stream of nitrogen and by distilling off the sodium hydroxide solution in 2-ethylhexanol followed by distillation of the volatiles. 1,4-Butanediol is a promising raw material that can be prepared from ethylene by electrolytic waste technology. The new esters obtained have excellent viscosity dependencies and very low freezing points and are therefore suitable as components for said oils and hydraulic fluids. The examples below illustrate the preparation method of the invention. Example 1

780 g of phenyltrichlorosilane (3.67 moles) were introduced into a 2.5 L Keller flask equipped with a stirrer, thermometer, reflux condenser, flask, heating bath and drain line with pressure gauge, and heated to 70 ° C with stirring. , initiated at 240593 240393 by dropping 300 g of 1,4-butanediol (3.33 moles) and continuing to heat the flask. 1,4-Butanediol was added dropwise over 30 minutes and the flask temperature was raised to 120 ° C to which it was maintained. Thereafter, 565 grams of 2-ethylhexanol (4.3mol) were begun to be admitted, and the admission was terminated in 30 minutes. The admission was controlled by the pressure-shifting hydrogen chloride. Nitrogen was then passed through the tube and the hydrogen chloride content of the flask was reduced to 1.9% KH / g under nitrogen for 1 hour while stirring.

Then, the calculated amount of saturated sodium hydroxide solution in 2-ethylhexanol was added to the flask with stirring. The flask was transferred to a distillation vacuum flask and the volatiles were distilled off by boiling point 226 ° C at 2.6 kPa. After cooling, the 904 g distillation residue was filtered through a filter paper. A clear-colored ester was obtained with the physical constants shown in Table II and characterized in Table I below x = 10.

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Claims (2)

240593 The ratios given in Table I of the ester prepared with the physical constants given in the same procedure as in Example 1 were in Table II, characterized in Table 1 using the same starting compounds in the value x = 1. 1. Organosilicon esters of formula HgCgO -Si οκη2> ¥ oCgHj where x = 1, 3, 10. 2. A process for the preparation of organosilicon esters according to claim 1, characterized in that the phenyltrichlorosilane is reacted with 1,4-butanediol and 2-ethylhexanol at a temperature of 70-120 [deg.] C., then the hydrogen chloride is expelled with a stream of nitrogen. neutralizes with sodium hydroxide in 2-ethylhexanol and volatiles are distilled off. Severografia, n. P., Závod 7, Most Price 2,40 Kcs