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Preparation method of polycarboxylic acid and flame-retardant epoxy resin thereof

A polycarboxylic acid and epoxy resin technology is applied in the field of materials to achieve the effects of simple and easy synthesis process, mild reaction conditions and low production cost

Active Publication Date: 2019-07-09
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its synthesis cost is low, and no toxic gas is generated during the synthesis process, which meets the requirements of environmental protection. The synthesis and application of this kind of phosphorus and nitrogen elements and polycarboxylic acids have not been reported yet.

Method used

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  • Preparation method of polycarboxylic acid and flame-retardant epoxy resin thereof
  • Preparation method of polycarboxylic acid and flame-retardant epoxy resin thereof
  • Preparation method of polycarboxylic acid and flame-retardant epoxy resin thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 78.3g THEIC, 88.2g MAH and 80mL dioxane into a 500mL round bottom flask equipped with a stirrer, condenser and thermometer, raise the temperature to 95°C, and keep stirring for 2h. Then, 194.4 g of DOPO and 130 mL of dioxane were added to the reaction solution in 5 batches within half an hour, and the temperature was raised to reflux state (about 110° C.), and the stirring was continued for 8 h. The molar ratio of the reaction raw materials is THEIC:MAH:DOPO=1:3:3. After the reaction is completed, dioxane, deionized water and the polarity difference between the product are used for purification. The resulting solution was poured into deionized water and stirred, and filtered to obtain a white viscous liquid. Wash again with plenty of deionized water. Finally, the product was dried in a vacuum oven at 60°C for 24 hours to a constant weight, taken out and ground to obtain 325.2 g of light yellow powder, which was sealed in bags for later use. Get a small amount of ...

Embodiment 2

[0038]Weigh 100g of epoxy resin (E-51) and 84.7g of methyltetrahydrophthalic anhydride in a 250mL round bottom flask and stir at room temperature for 10min, then add 0.2wt% of 2,4,6-tri(di Methylaminomethyl) phenol was stirred for 10 minutes, degassed for 5 minutes, then poured into a preheated mold, and cured according to the curing system of 100°C / 4h+130°C / 2h+180°C / 2h+200°C / 2h. After the resin is cured, the sample is prepared according to the standard, and the obtained sample is recorded as EP, which is a reference sample without adding flame retardant.

Embodiment 3

[0040] Add 12.5g of flame retardant and 100g of epoxy resin (E-51) into a 250mL round bottom flask equipped with a stirrer and a thermometer, stir evenly at 130°C (about 1h), then add 79.5g of methyltetrahydrophthalate Diformic anhydride, stop heating, and then add 0.2wt% 2,4,6-tris(dimethylaminomethyl)phenol when the temperature drops to 75°C, stir for 10 minutes, degas for 5 minutes, and then pour into the preheated mold In the middle, the curing is carried out according to the curing system of 100°C / 4h+130°C / 2h+180°C / 2h+200°C / 2h. After the resin is cured, prepare a sample according to the standard, and the obtained sample is marked as EP-1, and the flame retardant content is 6.5%.

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Abstract

The invention discloses a preparation method of polycarboxylic acid and flame-retardant epoxy resin thereof. The preparation method comprises the following steps: (1) preparation of polycarboxylic acid: three steps of esterification, addition and purification are included; and (2) preparation of flame-retardant epoxy resin. The polycarboxylic acid of the invention is prepared from tris(2-hydroxyethyl) isocyanurate, maleic anhydride, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide. The preparation method is simple and environment-friendly, and the production cost is low. The polycarboxylic acid has flame retardancy and reactivity at the same time, the flame retardancy of common epoxy resin can be remarkably improved, and good process performance and excellent physical and mechanical properties of the epoxy resin can be kept. The technical problems that the manufacturability and stability of an epoxy resin additive type flame retardant are poor, and a reaction type halogen flame retardant is not environmentally friendly at present are solved. The prepared flame-retardant epoxy resin can be widely applied to the fields of electronic appliances, chemical environmental protection, house construction, transportation, aerospace and the like.

Description

technical field [0001] The invention relates to a polyvalent carboxylic acid containing phosphorus and nitrogen elements and a method for preparing the flame-retardant epoxy resin, which belongs to the field of materials. Background technique [0002] Because of its good bonding performance, electrical insulation performance, chemical corrosion resistance and high strength, epoxy resin can be used in the bonding of metal and non-metal, the manufacture of electrical and electronic insulating materials, fiber composite materials, etc. It is used in aerospace, shipping, electrical and electronic, machinery manufacturing and other fields. However, ordinary epoxy resin is easy to burn, which limits its application in some fields with high flame retardancy requirements. Therefore, it is of great significance to improve the flame retardancy of epoxy resin. [0003] The flame retardant method of epoxy resin is generally to improve the flame retardant performance of the resin by add...

Claims

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Application Information

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IPC IPC(8): C08G59/42C07F9/6574
CPCC07F9/657172C08G59/4238
Inventor 段华军陈勇胜王钧杨小利吉飒胡瑞
Owner WUHAN UNIV OF TECH
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