Epoxy curing agent, and preparation method and application thereof

An epoxy curing agent, epoxy resin technology, applied in epoxy resin coatings, titanium organic compounds, coatings, etc., can solve the problem of not meeting the requirements of large-scale casting construction, complicated reaction steps, and low temperature curing performance can not meet actual needs and other problems to achieve the effect of low reactivity and mixed viscosity

Active Publication Date: 2018-02-23
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the concrete repair paints on the market are slow-drying at room temperature. When the ambient temperature is lower than 10°C, the film-forming reaction speed is slow and cannot fully react, especially when the ambient temperature is below 0°C. Oxygen resin is difficult to cure and form a film. In winter in the north, the ambient temperature is often maintained at about -10°C. Due to the low ambient temperature, the construction period of the anti-corrosion project is delayed. It can be seen that the low-temperature curing performance of the existing epoxy resin coatings has been reduced. Can't meet actual needs
[0007] US4092293 is initiator with pentaerythritol, initiates the polymerization of propylene oxide, with allyl capping, and H 2 S reaction obtains a polythiol curing agent used under low temperature conditions, but the disadvantage of this preparation method is that the reaction steps are complicated, the conditions are harsh, the raw material price is relatively expensive, and the cost is high
[0008] CN102391476A adopts sorbitol / mercaptoacetic acid / p-toluenesulfonic acid / toluene to prepare a polythiol curing agent through esterification, and each molecule has 8 to 12 thiol groups after epoxy resin chain extension, and epoxy resin Good compatibility, but the mixing operation time of the curing agent and epoxy resin is relatively short, which does not meet the requirements of large-scale pouring construction
[0009] CN106318302A discloses 3-mercaptoacrylate (TMOMP) as the accelerator of dicyandiamide / epoxy curing system, which can significantly shorten the curing time of epoxy resin adhesive and reduce the curing temperature, but the amount of polymercaptan curing accelerator Must be appropriate, because when the amount is too high, it will not only lead to a longer curing time, but also will lead to a decrease in the performance of the epoxy resin adhesive
[0010] CN102604044A discloses a thiourea-modified low-temperature curing agent and its preparation method. It has high reactivity and can be completely cured in winter, but the cured product after complete curing with epoxy resin has poor toughness and cannot be used as a tensile material

Method used

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  • Epoxy curing agent, and preparation method and application thereof
  • Epoxy curing agent, and preparation method and application thereof
  • Epoxy curing agent, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] (1) Preparation of epoxy curing agent

[0069] ① Mix 1mol of m-hydroxybenzoic acid and 1.02mol of 2-mercaptoethanol evenly, heat to 165°C, react for 3 hours and remove water to obtain mercaptoethyl m-hydroxybenzoate;

[0070] ②Under the catalysis of 0.02mol% (the ratio of acid catalyst to amine compound, the same below) glacial acetic acid, mix 2mol WANALINK6200, 1mol mercaptoethyl m-hydroxybenzoate and 1mol 37% formaldehyde, heat up to 90°C, and react 9h, and then cooled to room temperature to obtain mercaptolated phenalkamine.

[0071] ③ Add 1 mol of titanium tetrachloride to 0.1 mol of benzene under stirring conditions, cool down to below 15°C after the addition, and pass in ammonia gas until the pH value of the reaction system reaches 9, slowly add 4 mol of sulfhydrylated phenalkamine prepared by ② , heated up to 55°C, reacted for 3.5h, and collected fractions with an absolute pressure of 0.09MPa and a temperature of 130°C after the reaction to obtain the epoxy cur...

Embodiment 2

[0077] (1) Preparation of epoxy curing agent

[0078] ①Mix 1mol of p-hydroxybenzoic acid and 1.04mol of 3-mercapto-1-propanol evenly, heat to 175°C, react for 3.5h and remove water to obtain mercaptopropyl m-hydroxybenzoate;

[0079] ②Under the catalysis of 0.1mol% 37% hydrochloric acid, mix 1mol UNLINK4100, 3mol mercaptopropyl m-hydroxybenzoate and 6mol paraformaldehyde evenly, heat up to 115°C, react for 14h, and then cool down to room temperature to obtain mercaptolated phenalkamine .

[0080] ③Add 1 mol of titanium trichloride to 0.5 mol of benzene under stirring conditions, cool down to below 15°C after the addition, and pass in ammonia gas until the pH value of the reaction system reaches 10, slowly add 3 mol of thiolated phenalkamine prepared by ② , raised the temperature to 85°C, reacted for 6h, and collected fractions with an absolute pressure of 0.1MPa and a temperature of 140°C after the reaction to obtain the epoxy curing agent of the present invention.

[0081] ...

Embodiment 3

[0086] (1) Preparation of epoxy curing agent

[0087] ①Mix 1mol of p-hydroxybenzoic acid and 1.03mol of 2-mercaptoethanol evenly, heat to 170°C, react for 3.2 hours and remove water to obtain mercaptoethyl p-hydroxybenzoate;

[0088] ②Under the catalysis of 0.05mol% 37% hydrochloric acid, mix 1mol UNLINK4102, 2mol mercaptoethyl p-hydroxybenzoate and 3mol paraformaldehyde evenly, heat up to 100°C, react for 12h, and then cool down to room temperature to obtain mercaptolated phenalkamine .

[0089] ③Add 1 mol of titanium tetrachloride to 0.25 mol of benzene under stirring conditions, cool down to below 15°C after the addition, and pass in ammonia gas until the pH value of the reaction system reaches 10, slowly add 4 mol of mercaptolated phenalkamine prepared by ② , raised the temperature to 70°C, reacted for 5h, collected the distillate with an absolute pressure of 0.1MPa and a temperature of 135°C after the reaction, to obtain the epoxy curing agent of the present invention. ...

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Abstract

The invention discloses an epoxy curing agent for concrete refinishing paint, and a preparation method and application of the epoxy curing agent. The preparation method of the epoxy curing agent includes 1), allowing a carboxylic phenolic compound to react with a mercaptan compound to obtain a sulfhydryl phenolic compound; 2), under the action of an acid catalyst, evenly mixing an amine compound,the sulfhydryl phenolic compound and an aldehyde compound to react to obtain sulfhydryl-terminated phenolic aldehyde amine; 3), injecting nitrogen into a mixture of a titanium dichloride compound andbenzene, slowly adding the sulfhydryl-terminated phenolic aldehyde amine after the pH value of a reaction system reaches 9-10, and performing distillation after reaction to obtain the epoxy curing agent. The epoxy curing agent has the advantages that the epoxy curing agent can be mixed with epoxy resin to prepare an epoxy resin composition for the concrete refinishing paint; sulfydryl, tertiary amine and phenolic hydroxyl in the molecular structure of the curing agent have synergistic promotion effect, and accordingly, the epoxy curing agent can cure the epoxy resin below minus 25 DEG C and has high adhesion to concrete materials.

Description

technical field [0001] The invention belongs to the field of epoxy resins, and in particular relates to a low-temperature, high-humidity epoxy curing agent for concrete repair paint and a preparation method thereof, and its use for preparing an epoxy resin composition for concrete repair paint. Background technique [0002] Epoxy resin has excellent mechanical properties, aging resistance, water resistance, chemical medium resistance and good acid resistance. Due to the above performance advantages of epoxy resin, it occupies an important position in synthetic adhesives. It is now used both at home and abroad. Among the adhesive products, more than 90% are epoxy adhesives, and even some reinforcement specifications require the use of epoxy adhesives. [0003] Civil construction is a complex system engineering, which will be affected by various effects such as poor construction, rain and snow erosion, and ambient temperature. If it is not repaired in time, under the action of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/62C07F7/28C09D163/00
Inventor 周萌刘赵兴杜秀才陈杰张春
Owner WANHUA CHEM GRP CO LTD
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