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Intermediate temperature latent thermal curing agents for epoxy resin

A heat curing agent and epoxy resin technology, applied in the preparation and application of medium temperature latent heat curing agent, can solve the problems of curing performance fluctuation, measurement error, cumbersome configuration process, etc.

Inactive Publication Date: 2010-01-13
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The commonly used epoxy curing system is a two-component system. The curing agent is usually acid anhydride and amine. The two-component system has the following disadvantages: the configuration process is cumbersome; the ingredients are not mixed uniformly, and the curing performance will fluctuate; the error in measurement is inevitable and many more
There are many types of epoxy resin latent curing agents that have been developed, mainly boron trifluoride complexes, melamine and its derivatives, imidazole derivatives and organic hydrazides, etc., but each type of curing agent has certain Advantages and disadvantages. Up to now, no latent curing agent with particularly good performance has been found.

Method used

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  • Intermediate temperature latent thermal curing agents for epoxy resin
  • Intermediate temperature latent thermal curing agents for epoxy resin
  • Intermediate temperature latent thermal curing agents for epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The present embodiment is carried out according to the following steps: take 0.038mol N-butylcarbazole, 0.025mol ferrocene, 0.075mol anhydrous AlCl 3 , 0.025mol Al powder and 50ml cyclohexane were put into a three-necked flask, stirred and dissolved, and passed N 2 Then slowly raise the temperature to 84°C and maintain the reflux state for 10h. After the reaction liquid is cooled, pour 10% methanol solution into it, stir and hydrolyze, filter, separate liquids, wash the organic phase with water, combine with the water phase, wash repeatedly with cyclohexane, and then add excess KPF 6 An orange-yellow precipitate appeared in the aqueous solution. The solid was dried and purified by column chromatography to obtain the product [cyclopentadiene-iron-N-butylcarbazole] hexafluorophosphate.

Embodiment 2

[0020] In this embodiment, N-alkyl substituted carbazole ferrocene salt is used as a latent thermal initiator to thermally initiate and cure epoxy compound ERL4221: take 0.01 g of N-alkyl substituted carbazole ferrocene salt and add it to 1 gram of epoxy compound ERL4221 , stir well to dissolve it, take 5-10 mg and put it into a DSC differential thermal analyzer for thermal curing analysis. The test conditions are: the heating rate is 10 degrees / min; N 2 Gas protection; temperature range is 50-250 degrees. The experimental data are shown in Table 1.

Embodiment 3

[0022] In this embodiment, N-alkyl substituted carbazole ferrocene salt is used as a latent thermal initiator to thermally initiate and cure epoxy compound TDE85: take 0.01 g of N-alkyl substituted carbazole ferrocene salt and add it to 1 gram of epoxy compound TDE85 , stir well to dissolve it, take 5-10 mg and put it into a DSC differential thermal analyzer for thermal curing analysis. The test conditions are: the heating rate is 10 degrees / min; N 2 Gas protection; temperature range is 50-250 degrees. The experimental data are shown in Table 2.

[0023] DSC data of the thermal curing system composed of 11% carbazole ferrocene salt and ERL4221

[0024]

[0025] DSC data of the thermal curing system composed of 21% carbazole ferrocene salt and TDE85

[0026]

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Abstract

The invention discloses intermediate temperature latent thermal curing agents and a preparation method thereof. The compounds are characterized by having a cyclopentadienyl-iron-N-alkyl carbazole ferrocenium salt structure. The compounds are prepared from raw materials, namely ferrocene and N-alkyl substituted carbazole through ligand exchange reaction under the catalysis of Lewis acid. As the latent curing agents, the compounds can initiate ring opening polymerization of epoxy compounds at mild temperature, and have good thermal initiating activity and latent thermal performance. The solubility of the compounds in nonpolar resin is obviously strengthened due to the introduction of alkyl, and the compounds have wide study potential and application prospect in the field of epoxy resin application.

Description

technical field [0001] The invention relates to the preparation and application of a class of medium-temperature latent thermal curing agents, in particular to the preparation and application of a class of thermal curing initiators for epoxy compounds. Background technique [0002] Epoxy resin is a kind of thermosetting polymer composite material with good bonding, corrosion resistance, insulation, high strength and other properties. It is widely used in the bonding of various metal and non-metal materials, corrosion-resistant coatings, electrical insulation materials, FRP / The manufacture of materials plays an important role in electronics, electricity, machinery manufacturing, chemical anticorrosion and many other industrial fields, and has become an indispensable basic material in various industrial fields. [0003] The commonly used epoxy curing system is a two-component system. The curing agent is usually acid anhydride and amine. The two-component system has the follo...

Claims

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Application Information

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IPC IPC(8): C08G59/40C08K5/56C08L63/00
Inventor 王涛李治全李蒙卢明宝
Owner BEIJING UNIV OF CHEM TECH