SU897783A1 - Polymethilphenylphenethylsilazanes possesing increased hydrolytic stability - Google Patents

Description

The invention relates to the field of new chemical compounds, com. {RSiCNH),. FRSi where R-CsHy; R-SgN ,, SbNu; R-CH3; , which can be used to waterproof the various materials of anti-corrosion coatings. Polymethylphenylsilanes are known. obtained by ammonolysis of dimethyldichlorosilane and phenyltrichlorosilaneS. The compounds have good anti-corrosive and adhesive properties. However, they cannot be used for hydrophobization, since their hydrolytic stability is insufficient, retarding to polymethylphenylphenylethyl lasanes of the general formula, VflR SiNH3c} Polimetilfenilfonetilsilazany above formula were prepared ammonolysis metilfeniletildihlorsilana, fenetiltrihlorsilana or soammonolizom feniltrihlor- and metilfenetiltrihlorsilana and soammonolizom metilfenetildihlorsilanov sootnogaenii in 1: 1 or 1: 2 at a toluene medium. The compounds were identified by IR and NMR spectrometry, the elemental composition. Example 1. In a four-necked flask equipped with a stirrer, a thermometer, a bubbling tube for introducing ammonia and a reflux condenser, 83.8 g (0.38 mol) of 38 methylphenate dichloroside are charged:; .. q-Oz ml (1 gb) toluonl. After -unbui, the solution, while stirring, allows ammonia to flow at a rate of 0.5–0.6 l / min. With the contents of the flask, the temperature of the reaction mixture is kept within the limits. After the ammonolysis reaction is completed, ammonium chloride is filtered on a funnel After the distillation of toluene, first under vacuum of a water jet pump at 20–30 mm Hg, then at a residual pressure of 10 mm Hg, 51.3 g (82.7%) of product is obtained in the form of an oily liquid. Mol, weight 600. s..NtsZ (Nm.gjj sn. Calculated,%: C 66.25; Si 7.17; H 7.97; N 8.58. Found,%: C 66.33; Si 17 , 10; H 7.77; N 8.25.

{CC HjCjH Si (CH3) NH CC6H5SUNH) g3

Found,%: C 61.02; Si 18.80; H 6.73; N 11.14.

Calculated,%: C, 61.82; Si 19.24; H 7.1 1; N 12.03.

PRI me R 4. Analogously to examples 1-3 download 76,7 g (0.35 mol)

EHEN5SgNts5 SSNz), N5Sg.Nts% 1 (MN) ,,} Found,%: C 63.31; Si 1b; 4; H 7.33; N 9.91. Calculated,%: C 63.94; Si 17.55; H 7.52; N 10.96. In the IR spectra of the polymers obtained, there are absorption bands characteristic of SiNH-rpvnnH vibrations (935-940 cm, 1160-1170 cm) of methyl groups (785-790 cm, 1250 cm, 1425 cm), phenyl groups of 3050-3070 cm ethyl (1580 cm {CCfeH5Cj, H4Si (NH)

Found X: c 63.24; Si 17.75} H 7.22; N 11.79.

Calculated,%: C 64.00; Si 18.10; H 7.61; N 11.23.

EXAMPLE 6. A coating of chloroform-O solution is applied to the plate.

methylphenethyl dichlorosilane and 118.0 g (0.35 mol) of phenethyl trl chlorosilane (ratio of components 1: 1) and 1346 ml of toluene (: b). 101.8 g (30.07%) of polymer are obtained with a dry residue content of 99 3%. Mol. 2500

the polymer obtained in example 1 to another plate - the coating solution of the known polysil zana. After evaporation of the solvent, the films are dried under vacuum (for 2 hours at room temperature and Example 2). Example 1 load 1 1 I,; j g (0, D6 mol) phenethyltrichlorosilane and 773 ml ( 1: 6) toluene. 63.0 g (87.5%) of polyphenylsilazane are obtained, which, after solidification, is converted into a glassy mass with a solids content of 98.9%. Mol. Weight 1400. i: C, HsC,) Found %: C, 61.70; SI 18.2; H 6.74; N 13.12. Calculated,%: C, 61.66; Si 18.02; H 6.73; N 15.47. PRI me R 3. Analogously to examples 1,2 download 106,0 g:. (o, 48 mol) methylphenz1thyldichlorosilane and 0i, 5 g (o, 48 mol) of phenyltrichlorosilane (1: 1 ratio) and 1427 ml (i: b) of toluene. Obtain 92.1 g (70.3%) of a resinous mass with a cyxoi content of o residue of 99.1% Mol. weight. 1800. 2960 cm of g-CH., - CH-CHj (2870-29 —SNd-C groups of NH-groups of forces (3380 cm), as well as for SiCHj-rpynn (1260 cm). Example 5. Analogously to Example I, load 28 , 8 g (0.08 mol) of phenzethyltrichlorosilane, 7.6 g (0.04 mol) of methylfenzethyl dichlorosilane and 178 ml of toluene, 14.3 g (76.6%) of a glassy mass with a content of dry residue of 99.5% are obtained. 6000 (). CeH5t H ,, (CH5) 589 I mmHg (; imacIt IR spectra of the films obtained. The intensity of characteristic bonds of NH (3390 cm) and SiN (1180 cm) in spectra was measured to decrease in intensity, with an interval of 1 hour, they conclude that under the same conditions, 20 ° C, relative Airness 75% of the polymer is hydrolyzed 1.5 times slower than the known one according to Example 1. 3 The results of the luipiMiitic stability of pogimeron of Example 1-5 are similar.The hydrophobic properties of fabrics impregnated with the product of joint monolysis of methylfentyl dichlorosilane and phenethyltrichlorosilane are presented in the table.

Water resistance on penetrometer, mm of water column

to styr20s

170 ki.

100 C after

Washes

drying at 20 ° C

170 100 ° C 170 after

Wash

drying at 20 ° C

160

160

single absorption,% 1 hour before washing,

44,100

With streamer T ki

drying at 20 ° C

35 29 100 С

after washing II

with ear and pr 20 ° C

27 4 1 00 С 11 р и ме ч and and

160

205 185

187

190 194 190

206

201205 220

35

38 26

45 37

91 36

34 38

35 .1Z Washing is done in soap / soda solution for 30 minutes each.

7897783B

Thus, according to the invention can be used for

Claims (1)

Polymethylphenylphenethyl-hydrophobization was obtained. silazanes possessing the above formula of the invention hydrolytic stability, co-Polymethylphenylphenethylsilanes v {dSi (NHj gl CR-Sl (MH) gVBR 3lNHJc}, where R C5H5; 10bladanie increased hydrolytic R CjHuC (, Hjt-resistant. .1 CHj; a 0-1; .. Sources of information B from 8; taken into account in the examination С 0г4 ;, IS, 1, USSR Copyright Certificate , № 224803 ,, class. C 08 G 77/62, 1968 Another formula