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Flame-retardant epoxy resin curing agent and preparation method thereof

An epoxy resin curing and flame-retardant technology, which is applied in the field of preparation of flame-retardant epoxy resin curing agents and flame-retardant epoxy resin curing agents, can solve the problems of low flame retardancy and thermal stability of curing agents , to achieve improved flame retardancy and thermal stability, less smoke and toxic gases

Inactive Publication Date: 2020-04-28
NANJING ZHONGYING NEW NANOMATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the above-mentioned technical problems, the present invention provides a flame-retardant epoxy resin curing agent and its preparation method to solve the problem of low flame retardancy and thermal stability of existing curing agents. By introducing phosphorus-containing groups into amines In the structure of curing agent, the flame retardancy and thermal stability of epoxy resin can be significantly improved by using the phosphorus-nitrogen synergistic effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A flame-retardant epoxy resin curing agent, comprising the following raw materials in parts by mass: 20-40 parts of isophorone diamine, 10-20 parts of diaminodiphenylmethane, and 10-15 parts of n-butanol hydroglyceryl ether , 5-8 parts of oxalic acid, 3-7 parts of phthalic anhydride, 2-4 parts of bis(3-aminobenzyl)methylphosphine oxide.

[0017] The present invention also provides a preparation method for the above-mentioned flame-retardant epoxy resin curing agent, comprising the following steps: successively adding isophorone diamine, diaminodiphenylmethane, diluent, oxalic acid, phthalic anhydride , Bis(3-aminobenzyl)methylphosphine oxide gradually mixed slowly, reacted at 0.1-0.2MPa, 50-70℃ for 3-6 hours. After the reaction is finished, the solvent is distilled off under reduced pressure, and then deionized water 2-3 times the amount of the solid content is added to the solid content to disperse to obtain a curing agent.

Embodiment 2

[0019] A flame-retardant epoxy resin curing agent, comprising the following raw materials in parts by mass: 20-40 parts of isophorone diamine, 10-20 parts of diaminodiphenylmethane, and 10-15 parts of n-butanol hydroglyceryl ether , 5-8 parts of oxalic acid, 3-7 parts of phthalic anhydride, 2-4 parts of bis(3-aminobenzyl)methylphosphine oxide, bis(4-aminophenyl)-bis(9,10 -1-3 parts of dihydro-9-oxa-10-phosphaphenanthrene-10-oxide)methane.

[0020] The present invention also provides a preparation method for the above-mentioned flame-retardant epoxy resin curing agent, comprising the following steps: successively adding isophorone diamine, diaminodiphenylmethane, diluent, oxalic acid, phthalic anhydride , Bis(3-aminobenzyl)methylphosphine oxide gradually mixed slowly, reacted at 0.1-0.2MPa, 50-70℃ for 3-6 hours. After the reaction is finished, the solvent is distilled off under reduced pressure, and then deionized water 2-3 times the amount of the solid content is added to the...

Embodiment 3

[0022] A flame-retardant epoxy resin curing agent, comprising the following raw materials in parts by mass: 20-40 parts of isophorone diamine, 10-20 parts of diaminodiphenylmethane, and 10-15 parts of n-butanol hydroglyceryl ether , 5-8 parts of oxalic acid, 3-7 parts of phthalic anhydride, 2-4 parts of bis(3-aminobenzyl)methylphosphine oxide, and 1-2 parts of maleimide tungoleic anhydride.

[0023] The present invention also provides a preparation method for the above-mentioned flame-retardant epoxy resin curing agent, comprising the following steps: successively adding isophorone diamine, diaminodiphenylmethane, diluent, oxalic acid, phthalic anhydride , Bis(3-aminobenzyl)methylphosphine oxide gradually mixed slowly, reacted at 0.1-0.2MPa, 50-70℃ for 3-6 hours. After the reaction is finished, the solvent is distilled off under reduced pressure, and then deionized water 2-3 times the amount of the solid content is added to the solid content to disperse to obtain a curing agen...

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Abstract

The invention provides a flame-retardant epoxy resin curing agent, which is prepared from the following raw materials in parts by mass: 20 to 40 parts of isophorone diamine, 10 to 20 parts of diaminodiphenyl methane, 10 to 15 parts of a diluent, 5 to 8 parts of oxalic acid, 3 to 7 parts of phthalic anhydride and 2 to 4 parts of bis(3-aminobenzyl)methyl phosphine oxide. The invention also providesa preparation method of the flame-retardant epoxy resin curing agent, wherein the preparation method comprises the following steps: gradually and slowly mixing isophorone diamine, diaminodiphenyl methane, a diluent, oxalic acid, phthalic anhydride and bis(3-aminobenzyl)methyl phosphine oxide, and controlling the temperature at 50-70 DEG C to react for 3-6 hours. The flame-retardant epoxy resin curing agent has the following beneficial effect: the phosphorus-containing group is introduced into the structure of the amine curing agent, so that the flame retardancy and the thermal stability of theepoxy resin are improved; and no halogen is contained, and little smoke and toxic gas are generated.

Description

technical field [0001] The invention relates to a flame-retardant epoxy resin curing agent and a preparation method of the flame-retardant epoxy resin curing agent, belonging to the field of epoxy resin curing agents. Background technique [0002] Epoxy resins generally refer to polymer oligomers containing two or more epoxy groups, with alicyclic or aromatic organic compounds as the backbone and capable of forming thermosetting products through the reaction of epoxy groups. Due to the good performance of the epoxy resin system, it is widely used in various industries. However, due to its flammability, it cannot be used in occasions with special requirements for flame retardancy. The curing agent is an indispensable part of the epoxy resin system, so the epoxy resin system can be made flame retardant by developing a halogen-free flame retardant curing agent. The flame retardant curing agent overcomes the easy leakage of the additive flame retardant shortcoming. Halogen-fr...

Claims

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Application Information

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IPC IPC(8): C08G59/58C08G59/50C08G59/42
CPCC08G59/4223C08G59/504C08G59/58
Inventor 苏杨王奇
Owner NANJING ZHONGYING NEW NANOMATERIALS
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