Flame-retardant curing agent containing phosphazene/aromatic imine composite structure and preparation method thereof

A technology of aromatic imine and composite structure, which is applied in the field of flame retardant processing aids, can solve problems such as poor compatibility and decline in material comprehensive performance, and achieve excellent flame retardant performance, reduced dosage, and excellent intrinsic flame retardant performance Effect

Inactive Publication Date: 2020-05-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the compatibility between additive flame retardants and epoxy resins is generally poo...

Method used

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  • Flame-retardant curing agent containing phosphazene/aromatic imine composite structure and preparation method thereof
  • Flame-retardant curing agent containing phosphazene/aromatic imine composite structure and preparation method thereof
  • Flame-retardant curing agent containing phosphazene/aromatic imine composite structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation steps of the intermediate product: add 130g of p-hydroxybenzaldehyde, 100g of triethylamine, 54g of hexachlorocyclotriphosphazene, and 300mL of 1,4-dioxane into a magnetic stirring, condensing and reflux device, constant pressure drop Funnel and a nitrogen-protected 1L three-neck round-bottomed flask, after complete dissolution, the temperature was raised to 90°C, the reaction was continued for 12 hours, and cooled to room temperature. Then, it was filtered, concentrated by rotary evaporation, poured into 1 L of deionized water for precipitation, stirred at room temperature for 1 hour, filtered, washed with 300 ml of ethanol several times, and dried in vacuo to obtain a crude product. Purify by recrystallization with ethyl acetate to obtain 116.2 g of intermediate product with a yield of 90.3%.

[0032] Preparation steps of flame retardant curing agent: Add 75g of p-phenylenediamine and 100mL of 1,4-dioxane into a 500mL three-neck round bottom flask with...

Embodiment 2

[0036] Put 130g of salicylaldehyde, 41g of sodium hydroxide, 54g of hexachlorocyclotriphosphazene, and 300mL of tetrahydrofuran into a 1L three-necked round-bottomed flask with magnetic stirring, a condensation reflux device, a constant pressure dropping funnel, and nitrogen protection, and wait until completely After dissolving, the temperature was raised to 65°C, and the reaction was carried out for 48 hours, and then cooled to room temperature. Then concentrated by rotary evaporation, poured into 1L of deionized water for reverse phase precipitation, stirred at room temperature for 1 hour, filtered, washed with 300ml of ethanol for several times, and dried in vacuo to obtain a crude product. Recrystallization and purification with ethyl acetate gave 113.6 g of intermediate product with a yield of 85%.

[0037]Add 80g of 2,3-diaminopyridine and 200mL of tetrahydrofuran into a 500mL three-necked round-bottom flask equipped with magnetic stirring, condensing reflux device, and...

Embodiment 3

[0040] Add 100g of 3-ethoxy-4-hydroxybenzaldehyde (ethyl vanillin), 27g of sodium hydroxide, and 200mL of tetrahydrofuran into a 500mL three-neck tank with magnetic stirring, condensing reflux device, constant pressure dropping funnel and nitrogen protection. In the round-bottomed flask, heat up to 65°C, add 80ml of tetrahydrofuran solution containing 35g of hexachlorocyclotriphosphazene within 1 hour after complete dissolution, and cool to room temperature after reacting for 24 hours. Then concentrated by rotary evaporation, poured into 1L deionized water for precipitation, stirred at room temperature for 1 hour, filtered, washed with 300ml ethanol for several times, and dried in vacuo to obtain a crude product. Further recrystallization from ethyl acetate gave 102.3 g of intermediate product with a yield of 90.1%.

[0041] Add 70g of p-phenylenediamine into a 500mL three-necked round-bottomed flask equipped with magnetic stirring, condensing reflux device, and constant press...

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Abstract

The invention belongs to the field of flame-retardant auxiliaries of epoxy resin, and discloses a flame-retardant curing agent containing a phosphazene/aromatic imine composite structure and a preparation method thereof. The flame-retardant curing agent is composed of cyclotriphosphazene, aromatic imine and active amino groups, and the structural formula of the flame-retardant curing agent is shown in a formula I which is described in the specification. According to the invention, phosphonitrilic chloride trimer is subjected to substitution and condensation reactions with hydroxyl-containing aldehydes and aromatic diamines in sequence respectively so as to successfully prepare the phosphonitrile/aromatic imine composite structure-containing flame-retardant curing agent containing the polyfunctional active amino groups at the tail end. The whole preparation process has the characteristics of mild reaction conditions, controllable and adjustable reaction process, higher yield and the like, so the method is suitable for expanded production. According to the flame-retardant curing agent prepared by the invention, the contained active amino groups undergoes chemical reactions such as curing cross-linking with matrix epoxy resin and directly participates in forming of a polymer network three-dimensional structure to introduce a flame-retardant structure, so the prepared polymer material has excellent flame-retardant performance.

Description

technical field [0001] The invention relates to the field of flame retardant processing aids, in particular to a flame retardant curing agent with a composite structure containing phosphazene and aromatic imine and a preparation method thereof. Background technique [0002] Epoxy resin is a thermosetting material that is widely used. It has good adhesion, corrosion resistance, strength, stability, heat resistance, etc. It is widely used in coatings, adhesives, electronic packaging, aviation Aerospace, shipping and other fields. However, ordinary epoxy resin is a flammable material, and its limiting oxygen index is only about 20%. When it burns, it releases a large amount of black smoke and will continue to ignite other combustibles with the phenomenon of melting droplets, causing uncontrollable fire potential safety hazards. Therefore, actively developing and researching the flame retardant modification of epoxy resin materials has very important theoretical and practical s...

Claims

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Application Information

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IPC IPC(8): C07F9/659C08G59/50
CPCC07F9/65814C08G59/5046
Inventor 袁彦超陈瑜赵建青刘述梅
Owner SOUTH CHINA UNIV OF TECH
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