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A kind of imidazole curing agent and preparation method thereof

A technology of imidazoles and curing agent, applied in the field of imidazoles curing agent and preparation thereof, can solve problems such as short storage time, and achieve the effects of easy popularization and simple and feasible preparation method

Active Publication Date: 2017-08-15
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved in the present invention is to provide a kind of imidazole curing agent, to solve the problem that the storage time existing in the prior art is shorter

Method used

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  • A kind of imidazole curing agent and preparation method thereof
  • A kind of imidazole curing agent and preparation method thereof
  • A kind of imidazole curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: the preparation of 7-methylcoumarin

[0035] Mix m-cresol (20ml, 0.19mol) with malic acid (25.4g, 0.19mol), add 98% mass fraction of concentrated sulfuric acid (20.9g) dropwise under an ice-water bath, stir at room temperature for 0.5h after addition, and then heat up to 120 ℃ for 3h until no gas escapes. Cool, pour into ice-water mixture, extract with 250ml ethyl acetate several times, combine organic layers, wash with water, anhydrous NaSO at room temperature 4 After drying for 18 hours, the solvent was distilled off at 80°C and recrystallized from 95% ethanol to obtain white needle-like crystals (12.5 g, yield 43%) with a melting point of 125-128°C.

Embodiment 2

[0036] Embodiment 2: the preparation of 7-bromomethyl coumarin

[0037] Mix 7-methylcoumarin 1b (1g, 6.25mmol), NBS (1g, 5.62mmol), benzoyl peroxide (0.01g), and dry benzene 20ml, reflux at 80°C for 6h, and evaporate to dryness at 80°C solvent, washed with hot water, and recrystallized from glacial acetic acid to obtain white needle-like crystals (0.6 g, yield 40%) with a melting point of 178-180°C.

Embodiment 3

[0038] Embodiment 3: the preparation of 1-(coumarin-7-methylene) imidazole

[0039] Imidazole (0.16g, 2.32mmol), NaH (0.18g, 7.5mmol), DMF10ml, stirred at room temperature, added 7-bromomethylcoumarin (0.5g, 2.10mol), heated to 70°C, reacted for 2h, cooled, Pour into water, extract with 50ml ethyl acetate, wash with saturated sodium chloride solution, dry over anhydrous magnesium sulfate, spin dry, recrystallize from methanol to obtain a light yellow solid (0.13g, yield 26%), melting point 226-228°C . IR(KBr)vcm-1: 2953, 2857, 1669, 1593, 1573, 1442, 819, ESI-MS: 290[M+Na]+, 1HNMR: 2.93(2H, s, -CH2), 6.10~6.13( 1H, d, -CH=C), 6.47~6.48(1H, d, ArH), 6.92~6.94(2H, d, ArH), 7.20~7.30(3H, m, -CH=C), 7.71(1H, S, -CH=N), 12.35 (1H, s, -NH)

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Abstract

The invention discloses an Iimidazole group curing agent, which is 1-(coumarin-7-methylene) imidazole. The invention further discloses a method for preparing the Iimidazole group curing agent. Coumarin which is replaced by methyl is firstly compounded, and is replaced through NBS bromine, and is condensed with Iimidazole at last. The Iimidazole group curing agent is better than curing performance of existing Iimidazole group curing agents. Simultaneously, the method for preparing the Iimidazole group curing agent is simple and practicable and easy to generalize.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to an imidazole curing agent and a preparation method thereof. Background technique [0002] Epoxy resins are widely used in adhesives, composite materials, coatings and other fields. Imidazole and its derivatives are an important class of epoxy resin curing agents with excellent properties. However, the existing imidazole curing agents cannot be stored for a long time as a one-component system due to their high curing activity. In order to overcome this shortcoming, it is necessary to modify simple imidazole compounds to synthesize new imidazole derivatives. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide an imidazole curing agent to solve the problem of short storage time in the prior art. [0004] The technical problem to be solved in the present invention is to provide a preparation method of the abov...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/40C07D405/06
Inventor 戴勇赵玲玲解明超祁刚
Owner YANCHENG INST OF TECH