SU572461A1 - Tetraglycidic ester(4,4,-aminophenoxyphenyl) of sulfone used for preparation of epoxy materials with higher chemical stability - Google Patents

Description

Example 1. In a four-necked flask, equipped with a stirrer, a thermometer and a reflux condenser, load 54 wt. including bis (4,4 aminophenoxyphenyl) sulfone, 585 weight. including epichlorohydrin, 30 ml of water and 0.3 weight. including 2,4,6tri (dimethylaminomethyl) phenol. The reaction mixture is heated to 85-90 ° C and maintained under vigorous stirring for 7 hours. The resulting tetrachlorohydrin benz (4,4-aminophenoxyfennl) sulfone is separated from the reaction mixture for dehydrochlorination. The dehydrochlorination is carried out with a 40% aqueous solution of caustic soda (30 g of caustic soda and 45 ml of water), by gradually feeding the solution of alkali and stirring for 3.5 hours at 57-63 ° C. The mixture is kept for 1 hour. Then the reaction mass is neutralized, settled, the organic layer is washed several times with water and dried in a vacuum oven at 70 ° C for 2 hours. 81 g are obtained (yield per amine is 150%). Found,%: enoxide groups 25.4. Calculated,%: epoxy groups of 26.2. Found,%; C 65.5; H 5.6; N 5.0; S 4,7. Calculated,%: C 65.8; H 5.5; N 4.3; S 4.87. Example 2. In chetyrehosnuju flask equipped with a stirrer, thermometer and reflux condenser, load 108 weight. including bis (4,4 monnofenoxnophenyl) sulfone, 1170 weight. h. epichlorohydrin, 60 ml of water and 0.6 wt. including 2,4,6trp (dimethylaminnomethyl) phenol. The reaction mass is heated to 90 ° C and incubated for 7 hours. Next, they proceed as indicated in procedure 1. 160 g are obtained (147% yield per amine). Found,%: enoxd groups 24. Calculated,%: epoxy groups 26.2. Found,%: C 65.2; H 5.76; N 5.2; S 4.76. Calculated,%: C 65.8; H 5.5; N 4.3; S 4.87. Example 3. In the chetyrehosnuju flask equipped with a stirrer, a thermometer and a reflux condenser, 81 weight is charged. including bis (4,4-aminophenoxyphenyl) sulfone, 877.5 weight. hours of zichlorohydrin, 45 ml of water and 0.45 wt. including 2,4,6-tri (dimethylaminnomethyl) phenol. The mass is heated to 85 ° C and kept under stirring for 8 hours. Next, they proceed as indicated in Example 1. 121 g are obtained (149% yield per amine). Found,%: epoxy groups 25. Calculated,%: epoxy groups 26.2. Found,%: C 65.62; H 5.43; N 5.0; S 4.8, Calculated,%: C 65.8; H 5.5; N 4.3; S 4.87. The structure of the obtained material; the above-indicated value, the formula for it was established on the basis of the data of the analysis of the elemental composition, molecular weight, IR spectra, which characterize the presence of two epoxy groups at each nitrogen atom. The physicochemical properties of tetraglycidic ester of bis (4,4-aminophenoxyfennl) sulfone, obtained from Examples 1-3, are listed in Table. 1. Table 1 The bis (4,4-aminophenoxennl) sulfone etheglucid ether is dissolved in acetone, diethylformamnde, chloroform, eichlorohydrin, dioxane, ethyl acetate. Receiving epoxy. Example 1. In the reactor load 100 weight. . tetraglycidic ether bie (4,4-aminophenosiphenyl) sulfone and heated to 120 ° C. After this, 33.2 wt. including molten 4,4-diamnnodiphenylsulfone. The mixture is stirred at a temperature of 120 ° C for 5 minutes, poured into metal molds and cured according to the mode: 120 ° C - 4 h, 160 ° C - 18 h, - 1 h. Example 2. Epoxy material was prepared as in example 1, but add 40 wt. including molten 4,4-diaminodipheny l sulfone and curing is carried out according to the mode: 120 ° C - 4 h, 160 ° C - 14 h, 180 ° C - 2 h. Properties of epoxy materal (cast samples) based on tetraglycidyl ether bis (4,4-amino table) Table 2 Change in compressive strength after exposure to hydrochloric acid (3896) for 42 days,% Change in compressive strength after exposure to sulfuric acid (50%) and for 42 days,% Change in weight after holding in hydrochloric acid (38%) after 42 days,% Weight change after aging in sulfuric acid (5096) after 42 days,% Compressive strength, kg / mTverdost kg / SMZ Heat resistance ye Martens, ° C

oxyphenyl) sulfone, obtained by curing 4,4-diamiodiopeshish1Lsulfoiom, and its comparison e, known epoxy material based on tetraglycidic ester 4,4-daysnnodiphenylsulfone are given in

. 2

From the data table. 2 shows that the epoxy material based on tetraglycidic ester of bis (4,4-aminophenoxyfengl) sulfone IIMOCT HSC, -CH-CHP

% / Aly / v

CHr (iH-CH2

about

For the preparation of epoxy materials with high chemical resistance.

removed chemical resistance in comparison with epoxy based on a known compound, tetraglycidic ether of 4,4-diaminophenyl / sulfone.

Claims (1)

Invention Formula Tetraglycidyl ester of bis (4,4-aminophenoxene) sulfone of the general formula SNGN-eNg / VA SO; CH 2 CH CrI 2 Sources of Information attributed to the examination during the examination 1. USSR Copyright Certificate No. 363719, cl. C 08G 30/08, 12.21.70.