The method of obtaining the hardeners of epoxy resins cold curing

 

The invention relates to the production of hardeners used in the epoxy compounds intended for corrosion protection and other Hardeners of epoxy resins of cold hardening receive a mixture of aromatic and aliphatic di - or polyamines and the introduction of salicylic acid. Previously obtained by interaction of aromatic di - or polyamine (And) salicylic acid (B), dissolved in the product of esterification of orthophthalic acid with a hydroxyl-containing compound (C) selected from the group comprising butyl, icononly, benzyl alcohol, by mixing the components in the reactor at a temperature of 5090oWith over 640 min in the ratio a:B:wt.h. from 98:1:1 to 10:20:70. In another reactor pre-gain product of the interaction of aliphatic di - or polyamine (G) with the same components by mixing them at a temperature of 3055oC for 325 min in the ratio of G:B:wt.h. from 96:2:2 to 4:16:80, after which the resulting interaction products based on aromatic and aliphatic di - or polyamines are mixed at a temperature of 15

The invention relates to a method for production of hardeners epoxy cold cured with aromatic amines and can be used in the production of hardeners used in the epoxy compounds intended for corrosion protection, as self-leveling floors in the building, for impregnation of reinforcing fillers in contact molding and other purposes.

A method of obtaining hardeners epoxy cold cured by mixing an aromatic amine with cresol and salicylic acid or a liquid mixture of 3 aromatic amines with salicylic acid (see C. A. lapitskiy, A. A. Kritsuk, "Physico-mechanical properties of epoxy polymers and plastics, Kiev: "Naukova Dumka", 1986, S. 26-27).

This method allows to obtain hardeners, providing for cold curing higher strength properties and deformation resistant epoxy polymers compared with those obtained using as hardeners �chr/247.gif">2 h at 20o(C) that it is not possible to prepare them in advance and set as a commodity product, that is in the works with the use of such hardeners they need to cook small portions and immediately used. In addition, the known method involves the use of toxic components - cresol and meta-phenylenediamine, causing toxic effects on the workers and pollute the environment. Caulk same polymers although greater than those on structural performance and heat resistance, cured aliphatic amines, but have insufficient wear resistance and vibration resistance. The disadvantage of these hardeners is also a dark color hardened their epoxy polymers.

Also described is a method of obtaining hardeners, as the stage of preparation of epoxy compositions of cold hardening, which consists in mixing an aromatic amine, aliphatic amine, cresol and salicylic acid (see USSR Author's certificate 807622 priority on February 27, 1978, at the request 2583142 - prototype).

Obtained by a specified method hardeners provide improved wear resistance and vibration hardened in the cold of polymers, Nala epoxy cold cured, stable during prolonged storage, providing curing, starting with -10oWith, and obtain high-strength polymer with high heat resistance capable - with the introduction of dyes and pigments - staining them in almost any color.

This objective is achieved in that the pre-gain product of the interaction of aromatic di - or polyamine (And) salicylic acid (B), dissolved in the product of esterification of orthophthalic acid with a hydroxyl-containing compound (C) selected from the group comprising methyl, ethyl, oktilovom, butyl, icononly, benzyl alcohol by mixing the components in the reactor at a temperature of 5090oWith over 640 min in the ratio a: B:wt.h 98:1:1 to 10:20:70, in another reactor pre-gain product of the interaction of aliphatic di - or polyamine (G) with the same components by mixing them at a temperature of 3055oC for 325 min in the ratio of G:B:wt.h. from 96:2:2 to 4:16:80, after which the resulting interaction products based on aromatic and aliphatic di - or polyamines mix 5:5 to 5:95.

Specified is confirmed by the examples.

Example 1.

In a reactor equipped with a heating-cooling mixer, load 54 wt. including aromatic diamine -4,4 diaminodiphenylmethane (A), 10 wt.h salicylic acid (B), dissolved in 36 wt.h. the product of esterification of orthophthalic acid, a mixture of n-butyl and benzyl alcohols butylbenzylphthalate (B), when the ratio of components a:B:=54:10:36, the temperature in the reactor is raised at a constant operating the mixer, and after reaching a temperature of 70oThe mixture was kept under stirring for 12 min at this temperature, due to ekzotermicheskie reaction begins to rise and therefore include cooling and maintain the temperature of the 70oWith 11 minutes (i.e. the total time 23 min). The resulting product is cooled to 36oC. In another reactor similar conduct a mixture of Ethylenediamine - 50 wt.h. with 9 wt.h. salicylic acid, also dissolved in 42 wt.h. benzylbutylphthalate. The process of obtaining the product of the interaction of ectothermic, so after reaching the temperature of the 36oWith over 2 min include cooling and maintaining the temperature of the 42oC, stirred for further 12 minutes After that, the product is cooled to 20oC.

Next, both products were who live in the ratio of 50: 50 for 12 min at a temperature of 38oC. the thus Obtained compound then is loaded into a metal container and stored in warehouse conditions.

Examples 2-14 carried out analogously to example 1. The parameters of their implementation are given in table. 1. The properties of the hardeners according to examples 1-14 in comparison with analogue and prototype, and the most common hardeners of epoxy resins cold-curing - polyethylenepolyamine (PEPA), ethylenediaminetetra-formaldehyde condensate AF are given in table. 1 and 2.

Hardeners obtained by the present method, have indisputable advantages in comparison with known and has received good reviews both from foreign and domestic consumers. They are stable during storage and transportation, nelituji, non-toxic, utverjdayut epoxy resin even at moderate frosts, providing higher strength properties and heat resistance.

Claims

The method of obtaining hardeners epoxy cold cured, which includes operations of the mixture of aromatic and aliphatic di - or polyamines, and the introduction of salicylic acid, wherein the pre-gain product of the interaction of aromatic di-roxanadenadan connection (In), the selected groups include butyl, icononly, benzyl alcohol, by mixing the components in the reactor at a temperature of 5090oWith over 640 min in the ratio a:B:wt. hours from 98: 1: 1 to 10:20:70, in another reactor pre-gain product of the interaction of aliphatic di - or polyamine (G) with the same components by mixing them at a temperature of 3055oC for 325 min in the ratio of G: B: wt.h. from 96:2:2 to 4:16:80, after which the resulting interaction products based on aromatic and aliphatic di - or polyamines are mixed at a temperature of 1560oC for 320 min in a ratio of from 95:5 to 5:95.

 

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2 tbl, 8 ex

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