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Phosphorus-nitrogen-containing liquid acrylate monomer and flame-retardant vinyl ester resin and preparation method thereof

A technology of vinyl ester resin and acrylate, which is applied in the field of preparation of liquid acrylate monomer and its flame-retardant vinyl ester resin, to achieve controllable process conditions, improve flame-retardant efficiency and smoke suppression performance, and simple preparation method Effect

Active Publication Date: 2020-10-16
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a liquid acrylate monomer containing phosphorus and nitrogen elements and a preparation method of the flame-retardant vinyl ester resin for the above-mentioned deficiencies in the prior art. Additive flame retardants modified by ester resins have low flame retardant efficiency, poor compatibility with resins, deterioration of physical and mechanical properties and process performance of flame retardant resins, and environmental protection.

Method used

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  • Phosphorus-nitrogen-containing liquid acrylate monomer and flame-retardant vinyl ester resin and preparation method thereof
  • Phosphorus-nitrogen-containing liquid acrylate monomer and flame-retardant vinyl ester resin and preparation method thereof
  • Phosphorus-nitrogen-containing liquid acrylate monomer and flame-retardant vinyl ester resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Synthesis of liquid acrylate monomers containing phosphorus and nitrogen elements.

[0042] Add PDCP (22.79g, 0.108mol) and acetonitrile (350ml) in a 500ml four-neck flask equipped with a stirrer, dropping funnel, condenser and nitrogen inlet, then HEMA (14.04g, 0.108mol) , a mixed solution of triethylamine (21.86g, 0.216mol) and acetonitrile (30ml) was slowly added dropwise into a four-necked flask within 2h, and the stirring reaction was continued at this temperature for 4h. Then, catalysts 4-dimethylaminopyridine (0.63g, 2mol%) and THEIC (9.44g, 0.036mol) were added into the four-necked flask, and after stirring for 2h under ice bath, the temperature was raised to 85°C and kept for 12h. After the above system is cooled to room temperature, remove the triethylamine salt by suction filtration, pour the filtrate into a large amount of deionized water, obtain the crude product by extraction, wash it several times with deionized water, and then dissolve it in dichloro...

Embodiment 2

[0049] (1) See Example 1 for the synthesis method of the liquid acrylate monomer containing phosphorus and nitrogen elements.

[0050] (2) Preparation of flame retardant vinyl ester resin cast body.

[0051] Add 90g of common vinyl ester resin (901-VER) and 10g of acrylate monomer flame retardant into a 100ml round bottom flask, stir vigorously at room temperature for 5min, then add 2g of benzoyl peroxide as an initiator in the flask, After stirring until the benzoyl peroxide is completely dissolved, take an appropriate amount of the mixture for process performance testing. Then degas the above mixture in a vacuum defoamer for 5 minutes, then pour it into a metal mold preheated in an oven at 80°C, and follow the curing system of 80°C / 2h+100°C / 2h+140°C / 2h The mixture is thermally cured. After the mold is naturally cooled to room temperature, it is demoulded, and an engraving machine is used to prepare the standard pattern required for the flame retardant performance test. The...

Embodiment 3

[0053] (1) See Example 1 for the synthesis method of the liquid acrylate monomer containing phosphorus and nitrogen elements.

[0054] (2) Preparation of flame retardant vinyl ester resin cast body.

[0055] Add 85g of common vinyl ester resin (901-VER) and 15g of acrylate monomer flame retardant into a 100ml round bottom flask, stir vigorously at room temperature for 5min, then add 2g of benzoyl peroxide as an initiator in the flask, After stirring until the benzoyl peroxide is completely dissolved, take an appropriate amount of the mixture for process performance testing. Then degas the above mixture in a vacuum defoamer for 5 minutes, then pour it into a metal mold preheated in an oven at 80°C, and follow the curing system of 80°C / 2h+100°C / 2h+140°C / 2h The mixture is thermally cured. After the mold is naturally cooled to room temperature, it is demoulded, and an engraving machine is used to prepare the standard pattern required for the flame retardant performance test. The...

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Abstract

The invention discloses a phosphorus-nitrogen-containing liquid acrylate monomer and flame-retardant vinyl ester resin and a preparation method thereof. The liquid acrylate monomer containing three phosphorus, three nitrogen and three carbon-carbon double bonds in the molecular structure is synthesized through a substitution reaction among phenyl dichloro-phosphate, partially methacrylated or acrylated alcohol and tris(2-hydroxyethyl) isocyanurate; and can be used as a reactive flame retardant and added into common vinyl ester resin to prepare halogen-free flame retardant vinyl ester resin. The liquid acrylate monomer has the advantages of environmental friendliness, simple preparation method, and controllable process conditions; the problems that the physical and mechanical properties ofthe matrix are reduced due to poor compatibility of an additive flame retardant and a matrix, and the viscosity of the resin is increased and the processing property is poor due to the fact that a solid flame retardant is insoluble in resin are solved, and the flame retardant property and the smoke suppression property of vinyl ester resin can be greatly improved.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a liquid acrylate monomer containing phosphorus and nitrogen elements and a method for preparing the flame-retardant vinyl ester resin thereof. Background technique [0002] Vinyl ester resin (VER) is a kind of thermosetting resin obtained by addition polymerization of bisphenol type or novolac type epoxy resin (EP) and unsaturated monocarboxylic acid containing double bonds such as methacrylic acid. unsaturated polyester resin (UPR). It combines the advantages of EP and UPR, such as excellent heat resistance and corrosion resistance, good toughness and physical and mechanical properties, outstanding wettability and adhesion. Due to their very good comprehensive properties, they are widely used in composite pipes, printed circuit board coatings, flocculants, adhesives and many other industrial fields. However, like most common polymer materials, VER is mainly composed of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6521C08F283/10C08F230/02
CPCC07F9/6521C08F283/105C08F230/02Y02P20/52
Inventor 段华军吉飒陈勇胜杨小利王钧王翔
Owner WUHAN UNIV OF TECH
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