SU1162808A1 - Method of obtaining mixture of ethyl-substituted silanes - Google Patents

Abstract

1. METHOD OF PREPARING A MIXTURE OF ETHYPICAL SILANES by the interaction of metal magnesium with ethnics and tetraethoxysilane in traditional solvents, including toluene and diethyldichlorosilane, at 50-100 ° C, characterized in that, with the aim of increasing the total content of these, this ethyl methane, is 50-100 ° C. In a mixture and simplification of the process, diztildichlorosilane is taken in an amount of 1.0-7.2% of the volume of the reaction mixture. 2. Method POP.1, characterized in that the process is carried out in the presence of silicon tetrachloride,

Description

HMCIIilO to UC) Ver11e 1STBog an OM OM CJiOC; Pu iii) j: y4eHHH r; THJKJaMciu Mini ,;

tni.I; i C Bj PRODUCT CHNPA.PUPH (; -: LA

:: o.-1ethylsiloxane; : zhd.ost it, iiiupoKo d named in kpchest) not heat carriers, working fluids d, h

hydraulic systems of J os priests IIEKPGTsMISR-

tour) oil oils,; and-mnfiruyp jnl, G i: pH6 (ipax and others,

IzEykugsn sposo () obtained} | I -rrnji amnescionic sillnosis ethn-lztoksisl-shannoe) mutual;: the action of magnesium with .y; o: -l; y-H) Go or brog-histy;) Tnd and t (.g lp; : and ssgly.1L1 ether I 1 „

Ned: 1STat method of lil stg i pi meenio ss 5 ether,

Also known is the preparation method for the preparation of elet ilo Io to c 11 s il ak a tov; t l e tl o r s ila yuw by means of a reciprocal process: neither with a mixture of ethyl chloride and tetra ethox: isilane or tetrachloride: 7h; go K;) emn1-1 (with the addition of cejinoro) ij-i a) and (or1ai (1 cellolyl, HaiiptiMe;) cc: ilola and .i toluene I, -j,

However, there was a kohversy 31 ilmagkyh, (ke, fkuiee 90; o lipolit to the loss of m: 1l lma lma1eme11; e ciijijjio; llc oolech 1.,) ; 1I) g /;. ;; hls - lrnoy dslp-; olig-oe {h lsilox oi. and imes; 1H; e ztlm and; -: X cnoiie-asa:

The closest to l: zobrege1 And about los tekhiicheski lol supikktnilllle SL) (lk: Is ;,: 1uchsli ;; c; ec; i;:, L1: chll -..ilde | 1-nb; x sl1lal; L (, Barely: chi metal: L5ches si} magnnl with chlorlet mill; ethyl, tetraltch5Ks 1Sila ;; (-, - l che -;: -. | rehhlorS111 /; cre: chil1: 1 e ext .-) - Lch (l; sulfuric flra is cpc:, .. e o: llllcho. e x oi-o) {) itite, h, (l.) (chgo; cs e; ..;,.: OJI {I Ch1tils1 loksanop and d: chlgll: 1x / 1Orsilan. 1 of those aloeo: -: s: io iiii-ai: t - TiHH (2 2--7b): (23- / o); h ii, l / iip; - ..Л --- Chlor-sill is 0.4–0.95% of l vol; rr h h lapichnruult iia composition

the volume of the reaction mixture (-brazuyuschas hgch.p adened with: silt; en

E single-piece method - helmetic co-composed of ell-chlienyeni ss.Ls; non. BUT

holding triple iJIXLop-, triethyl; ok with lll and ilhlore and h: r1 2., i; diethyl diets: siltanes and Hexaethyldisidoxanasiogl.lan 38, o: TeTiJar g1- {leylai, 4;

(up to 35%), as well as the need for triegilk.kollslan 8.8, three: yyr:) the current use of complex solvents (l-1lan 37, /, .1 h-h holding; -

and sulfur ether, ethylchillac-h 46. (J4

The purpose of the invention H1 lgsgu; Unall-Raschitglgia about

The total l: sod / rye triethyl-chame-1 alkaline sigloch ethyl magnesium chloride is 98.9%. Example 2. A 243 kg (10-10 mol of magnesium and 1015 l (4.57-10 mol) of tetraethoxy silane are charged into a capacitive-type reactor with a volume of 6.3 m, equipped with a stirrer, reflux condenser, jacket, thermocouple, air). to 60-70 ° C, after the start of the reaction, transfer the reactor to cooling and for 8-10 hours at 50-70 ° C, the reaction mixture is introduced to 770 l (11-10 mol) ethyl chloride, 1000 l toluene and 50 diethyl dichlorosilane additive ( the amount of diethyl dichlorosilane added to the mixture, taking into account the tetraethoxy silane used, is 1.8% by volume.) The apparatus is heated to, for 3 hours, stirred at 100 ° C and discharged after cooling and analysis for hydrolysis. 3. The total content of trietrshsilanes (triethyl ethoxy-; silane and hexaethyl disiloxane) 10.7% Calculated by the composition of ethylsyl butyl ethylmagnesium chloride, constitutes 98.6%, Example 3, The synthesis of ethylsilane silanes is determined by example 2. The reaction is: t d bavku 150 l (5,4ob.% diethyldichlorosilane. The composition of the resulting ethyl-substituted silanes,%: ethyltriethoxysilane 5.0; triethyl ethoxy sisilane 13J5, diethyl ethoxysilane 76, hexaethyl disiloxane 3.6. The total content of triethylsilanes (triethoxyethylsilane and hexaethyldisiloxane is 17.1%. The composition of ethylsilane covers and ethylmagnesium chloride is 98.2%. Example 4. The synthesis of ethylsilane silanes is carried out as in Example 2. The difference: the reaction mixture is injected 200 L (7.2%. Diethyldichlorosilane. The composition of the ethylsilane silanes formed,%: Ethltryethras, 12.2, Triethyl ethoseisilane 19.1; Diethyldiethoxysilane 65.0; Hexaptildisiloxane 3.7. The total content of Triethylsilanes 65.0; Hexaptildisiloxane 3.7. The total content of triethylsilanes is 65.0; Hexaptildisiloxane is 3.7. The total content of Triethylsilanes is 65.0; Hexaptildisiloxane is 3.7. The total content of Triethylsilanes is 65.0; ana) 22.8 /. The ethylsilane conversion calculated for the composition of ethylsilane is 98.2%. Example 5. The synthesis of ethylsubstituted C1-shanes is carried out as in Example 2, Difference: 100 l (3.6 v .%) diethyldichlorosilane. Composition of the image of the ethylsilane substituted silane,%: ethyltriethoxysilane 6.2 triethyl ethoxycisilane 11.0; dethyltistociiCH. IdH 79.9, hexaethyl disiloxane 2.9) io content -3); eight%. The ethylanilane conversion calculated for this 1 mg magnesium chloride is 98.4%. Example 6. The apparatus with a capacity of 1.0 l, divided by height with heads with four reaction zones (numbering of zones from bottom to top), equipped with a stirrer and instruments for controlling temperature, mixture flow, speed, 500 g of magnesium with a granule size 1, 0-2.5 mm and a continuous flow of 1000 ml / h of a reaction mixture consisting of 210 ml (3,000 mol) of ethyl chloride, 304 ml (1.360 mol) of tetraethoxy-pan, 10 ml (0.067 mol) of diethyl orhsilane ( addition of diethyl dichlorosilane to the reaction mixture (sol. 1.0 vol.%) and 476 ml of toluene, to the bottom of the first zone and magnesium from the top of the reactor at a rate of 73g / h. The synthesis temperature is maintained in the first and fourth zones and the separator, BO second and third zones 50-52 0 by cooling the first zone and heating the fourth zone and the separator. The rotation speed of the stirrer is maintained within 120 -: -, .. 140 rpm. The product of the synthesis, which is a suspension of magnesium salts with ethyl ethoxysilanes and in a solution of toluene, is taken into a collection and analyzed for the composition of the formed etxethoxysilanes. The composition of the resulting ethylsilane issins,%: ethyltriethoxysilane 8.5 triethylethoxysilane 8.1-, diethyl ethoxysilane 83.4. The total content of triethylsilano is 8.1%. The ethyl silane conversion calculated for the composition of ethyl magnesium chloride is 95.3%.

3

and p and m with p 7. Lnaloichich (irnme;: y b}: the apparatus with the same parameters :: :) evaluation of the podigot mixture Toio same composition; .i. as in example 6, but with, 3ri; ; iH OM 25 ml (0.167 mol) di: 71ig (addition of diethyl dichlorosil ;;) the reaction mixture was compounded 2 ;;; about,%) and 461 ml of toluene.

Co g Cha p image uyushchs til za me: tse} ;; mx cvLianoB,%: etltriethoksisi.cha ;; l, 3; t | 1Eethylztoksisilan 1 O, A;,) G11..ppg. gszhg psi.ggan 83.3. The total amount of triiiylsilalovii 10.4%,

gaschey gaine on the composition of ethylsyl u: 4i ko ;;; -: e.rsi ethylmaginykhlori; G1 state,; plet 94, 6% „

And p 8 8 Lialo: 1chio lrime; The apparatus with the same process parameters serves the same mill as p 6, according to C isd1K) tildichlo x: 1: paw (dgcheagcha di:; n chlorosilag; an n; n aKiu; o; iyiii; / (. g 3, P cio./) and jjd:.; L then (; o (ggap oOrazkkiihgk ggi: 1 ;; x-.

N of silanes, L: oTiijn RI toxis: 13.0 triegi.aethoxysyl ;: 14; getildiethoxmsi.aan 72, 3, Sug-ma;) content of three 1 rinjcujiaiio; one (,

Dissociatingly comparing with -g; -, non-converting etl.lmag / craBJiHeT J4 chloride, h / l.

So ora ohm,) edlagag-: s

coG poses ;; ol er uni: lich amount: content -lNkLu.por-, trizt) toxisil 1O) | and tschatsaetildishi: on in the mixture of reaction products with article npoitecc due to

difficult races

Claims (2)

1. METHOD FOR PRODUCING A MIXTURE OF ETHYL SUBSTITUTED SILANES by reacting magnesium metal with ethyl chloride and tetraethoxysilane in an organic solvent, including toluene and diethyl dichlorosilane, at 50-100 ° С, characterized in that, in order to increase the total content of triethylchlorosilane tri in the mixture and simplify the process, diethyl dichlorosilane is taken in an amount of 1.0-7.2% of the volume of the reaction mixture. 2. The method of pop. 1, characterized in that the process is conducted in the presence of silicon tetrachloride.