SU418065A1 - Method of preparing organosiliconic urethan oligomers - Google Patents

Description

t

Known silicone urethane oligomers based on silicone diisocyanates type

T J OCM- (tH2V5i-0-5i- (CH., - NCO,

R R. Where

R, R-C ,,

and organosilicon carbofunctional glycols of the following structure R

nomn ,, - (si, won,

R R where, 2,3,4;

4 "" -CH.-CgHy.-CgH,;,

A method for the preparation of silicone oligomers of the following structure is proposed.

OC tH-C-C-L-0-C-t; lYP-C-0-L-K-t-OH, A);

but about n-m 6 OCN4P-N-C-0-L-K, -L-o e th, -p-ms, about 6);

MO (E and

Where

(p - (CH) .. 0-Si- (C-HaV,

- R

R --- CH ,, -, R --- OH ,,, - C2.Hs ,, h-.,

“R R R R

(-l-Si-; -S-i-0-Si-I-Si4D-Si-i Yai "," .. ",", ,,

T- --- 4Vi-CHH4-o-CbH4-, K ° - cHj, -CfeHs;

--0-CH, -CH, j-CH, -CH2 -, - tH, i-0-CH ,, -, -IN

In order to increase the frost resistance, heat resistance, hydrophobicity and weather resistance of the final reactive product, silarylene ether alcohols of the general formula HO-L-K-L-OH are used as the initial hydroxyl-containing compounds, and the diisocyanate bisisocyanate alkyl disiloxanes of the total

formulas

Claims (3)

OCN-P-NtO Reaction of the interaction of the organosilicon diisocyanates with silarylene ether alcohols easily proceeds at an elevated temperature, preferably at 50-100 seconds, in the presence of a catalyst, preferably octoate, in a solvent, in an atmosphere of thoroughly dried argon. The yield of products in all cases is close to the theoretical. Depending on the ratio of the starting diisocyanates and silarylene esters (from 0.5 to 2), oligomers with terminal isocyanate, hydroxyl or isocyanet and hydroxyl groups can be obtained. The structure of the obtained oligomers is confirmed by elemental analysis by IR spectra, analysis of isodianate groups. The proposed organosilicon oligomers with urethane units in the chain and reactive isocyanate and hydroxyl end CHI CHj. IO-CH2-OH2-0-CH2- & 1-0- $ 1-CH, CH, and 2.95 g 1,3-bisisocyanate propyldimetyl disisylsilane. , then tin catalyst, with the calculation of its concentration in the reaction mixture, equal to 0.0001 mol / L. The reaction mass is maintained at 80 ° C for 8 hours under an atmosphere of dry argon. Then the solvent is distilled off and the resulting oligourethanes are brought to constant weight in vacuum (10 mm Hg). 9.4 g (95.0%) of a light amber-colored oligourethane-resinous product () is obtained. %: C 57.50; H 7.37; Si 16.15; NCO 0.4; OH 0.19. Calculated,%: C 51, AO; E 7.35; Si 16.80. The molecular weight (ebulioscopically) is 8790. EXAMPLE 2. 4.85 g of silicon ether ether alcohol (I) and 2.98 1,3-bis-isocyanate propyl dimethyldisiloxane in the presence of 0.0001 mol / l tin octoate in chlorobenzene are kept for 8 hours at. After distilling off the solvent and charging it, 7.50 g (96.0% of type A oligourethane is obtained (). Found: C, 61.0; H, 7.6; 14.38; NCO, 0.6; OH, 0.26. Calculated ,%: C 60.5; H 7.3; Si 14.10, I Mole, be 6361. Example 3. 6.05 Silicon ether ether (1) and 3.0 g 1.3 bis bisocyanate propyl dimethyldisilane in chlorobenzene in in the presence of 0.0001 mol / l tin octoate is kept for 8 hours at 70 C. After the solvent is distilled off and evacuated, 8.4 g (94%) of type A oligourethane is obtained (). Found: C 55.1; H 7; 70; S i 19.0; NCO 1.35; OH 0.55. Calculated,%: C 54.8; H 7.65; Si 18.7. Mol. Weight 3080. in groups can be used in the synthesis of p Various classes of polymers, moreover, the introduction of silicon into such compounds contributes to an increase in frost resistance, hydrophobicity, and weather resistance, the introduction of silphenylene bridges into the polymer chain significantly increases the temperature resistance of polymers. Synthesis of type A oligomers In a three-necked reactor equipped with a stirrer, a thermometer and a tube for argon supply blown with argon for 0.5 h, load 100 ml of chlorobenzene, 6.9 g of organosilicon ether alcohol (1) iO-Si-CH-O-CHj-CHj-OH CeHj CHj Example 4. 5.92 g of organosilicon ether alcohol (I) 3.0 g of 1,3-bisizotsianatpropildimetildisiloksana chlorobenzene in solution in the presence of 0.0001 mol / l of tin octoate kept for 8 hours at. After distilling off the solvent and evacuating, 8.5S g (96.0%) type A oligourethane () is obtained. : C 62.8; H 7.52; Found, 1 Si 12., 6; NCO 0.7; OH 0.3, C 62.2; H 7.44; Calculated Si 12.5. Mol. Weight 5340. Synthesis of type B oligomer. Example 5. 2.1 g of organosilicon ether alcohol (T) and 2.3 g of 1,3-bisisocyanate propyl dimethyldisiloxane in chlorobenzene solution in the presence of 0.0001 mol / l tin octoate are incubated for 5 h at 80 ° C. After distilling off the solvent and evacuating, 4.75 g (95.0%) of type B oligourethane is obtained. Found: C 55.2; H 18.0; NCO 5.8. Calculated,%: C 55.0; H Si 17.3. Mol. Weight 1500. Example 6. 5.2 g of an organosilicon ether alcohol (T) and 1.2 g of 1,3-bisisocyanate propyl dimethyldisiloxane in a solution of chlorobenzene in the presence of 0.0001 mol / l tin octate are incubated for 8 hours at 80 ° C, After distilling off the solvent and evacuating, 6.2 g (97.0%) of type B oligourethane are obtained. Found: C 58.7; H Si 16.5. Calculated,%: C 58.5; Si 16.4. Claims 1. A process for preparing organosilicon urethane oligomers reak9 418,065 tion organosilicon diieotsianatov with organosilicon glycols, characterized in that, in order to increase heat resistance, mo OZOSTOYKOSTI, hydrophobicity and BTMO-j sferostoykosti reactive end capable product as cream niyorganicheskih glycols use silarylene ether alcohols of the general formula .uch OH) "I -. flfCHnb (K} --1D goe -L- Ul, v / n2) 4.-) .2 and (liilZ in d 6} RR 1. R, R. K - 5i-l-5i -, - 5-io-Si-u-Si-o-Si-, R fi. R fiH4.0-CsIl. D “, 2. The method according to claim 1, differing from the goys and the fact that the reaction is conducted in a solvent. 3. The method according to claim 1, characterized by the fact that the reaction is carried out in the presence of catalysts.