SU667553A1 - Tetraglycidyl of 3,3'-dichloro-4,4'-diaminotriphenyl methane for producing chemostable epoxide polymers - Google Patents

Description

Example 1. i chotyrekhorylnuyu bo, equipped with a stirrer, thermometer and reflux condenser, load SW weight, 3,3-dnhlor-4,4-diaminotriphenylmethane, 825 weight.h. epichlorohydrin, 3U ml of water, 0.6 weight.h. 2,4, b-gris- (limethylaminomethyl) -phenol. The reaction mixture is heated to 8590 ° C and maintained at vigorous stirring for 7-1O hours. The resulting terachlorohydrin Z. z-dichloro-4,4-diaminotriphenylmethane is washed with water and separated from the reaction mixture for the subsequent dehydrochloride {eovanie. Dehydrochlorination is carried out with a 40% aqueous solution of NaOH (72 g of NaOH 1 O8 g of NlO) with a constant supply of alkali solution and stirring for 3-3.5 hours at 55-6 O with. After addition of the alkali solution, the mixture is kept for 11 ~ 5 hours. Then the reaction mass is neutralized, defend, the organic layer is washed several times with water until there are no C ions and dried in a vacuum oven at 80-100 ° C for 3-4 hours. Obtain 144.2 g of product (yield per amine 140%). 25% epoxy groups were found, 30.3% epoxy groups were calculated. Found,%: C 59; H 2.83; N5,8. Calculated,%: C 6O, 2; H 2.8; CE, NC, d2,5; N4.9. Example 2. In chetyrehkorlyuyu; n bu, equipped with a stirrer, thermometer and reflux condenser, load 51.5 weight.h. 3,3-dichloro-4,4-diaminotriphenylmethane, 413 parts by weight epichlorohydri Indicator

Appearance

Epoxy content

found

calculated

Number of volatile,% Molecular weight

Table

Example 1 Example 2 | Example 3

Small product of dark brown hdata, 15 ml of water. Oh, l}} ec. 2,4, in-tris- (dnmethylaminomethyl) -feiol, the reaction mass is heated to 85 C and incubated for 10 hours. Next, proceed as indicated in example 1. Get 73.7 g of product (yield per amine 143%). Found epoxy groups 24.8%, calculated - DA, 3%. Found,%: C 59.2; H 2.76; C8. "13.6; N 5.1. Calculated,%: C 60.2; H 2.8; CE 12.5; N4.9. Example 3. in chetyrehosnuju flask equipped with a stirrer, thermometer and reflux condenser, load 154.5 parts by weight 3,3-dichloro-4,4-aiaminotriphenylmethane, 1238 parts by weight epichlorohydrin, 45 ml of water, 1 weight.h. 2,4,6-tris- (dimethylaminomethyl) -phenol. Massa is heated to 8 5 C and kept under stirring for 9 hours. Next come, as indicated in example 1; Obtain 211.6 g (yield per amine 137%). Found epoxy groups of 25.6%, calculated epoxy groups of 30.3%. Found, C 59.4; H 2.81; , 2; N 5.6. Calculated,%: C 60.2; H 2.8; All 12.5; N 4.9. The structure of the obtained substance of the above formula was established on the basis of data from the analysis of the elemental composition, molecular weight, IR spectra, characterizing the presence of two epoxy groups at each nitrogen atom. Physico-chemical properties of tetraglycidyl ether of 3,3-iichloro-4,4-diaminotriphenylmethane are given in table. one.

3,3-chichloro-4,4-diaminotriphenylmethane tetraglyl ether is dissolved in aiierone, epichlorohydrin, pyoxane, limegylformampe, chloroform, Properties

Indicator

The change in strength,%, with ti after exposure for 42 days. at;

38% hydrochloric acid 50% sulfuric acid acetone

4O% solution of caustic soda

Change Bieca,%, after 42 days. at:

38% hydrochloric acid sulfuric acid acetone

40% aqueous solution of caustic soda

Compressive strength, kg / cm 2

Hardness, kg / cm Heat resistance according to Martens,

based on the proposed epoxy polymer and izpest (gota liamina 1 ate rt -amnnoyeonilaniline cures in table 2.

table 2

Those traglyuhid sludge ester-3,3 -pichloro-4,4-o us inod ifen "methane (known compound)

Samples have collapsed

-sixteen

-23,19

-2.1 e changes

-16,46

-14,23

-2,6

Samples have collapsed

+ 7

-2.6

+3.46

+0.01 -O, O1

-OD

+0.01

2500

2400

2415 2762

168 170

Properties of epoxy material (cast samples) based on 3,3-dichloro-4,4-diaminotriphenylmethane tetraglycidyl ether, obtained by solidification of 5 P-aminobenyl amine and its comparison with

The change in compressive strength,%, after aging v. over 42 SUT. at:

 hydrochloric acid

5% sulfuric acetone

-32

-sixteen

-10,5

-2,1

-8,2

Table 3 lists the known epoxy material based on 3,3-DI.HLOR-3-nitro-4,4-diaminotriphenylmethane tetraglycidyl ether. 3, Table

667553

7,.:

Indicator

40% caustic soda solution. Weight change,%, after 42 sug. at:

Claims (2)

1. USSR author's certificate hfe 339562, c. 08 G 59 / 1O, 1974. 2. For: ka N8 2163512/04, cl. From 07 D 303 / Q8, 1975, according to which a decision was made to issue author certificates.