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A kind of phosphorus nitrogen synergistic high flame retardant polyester curing agent and its synthesis method

A technology of polyester curing agent and synthesis method, which is applied in the field of electronic packaging materials, can solve the problems of poor flame retardancy and synergy, and achieve the effects of being beneficial to environmental protection, ensuring the durability of flame retardancy, and simple synthesis process

Active Publication Date: 2015-08-26
天津凯华绝缘材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its flame retardancy is not very good, and it is often used in combination with other flame retardants, such as phosphorus and nitrogen, which have a synergistic effect. This is because the addition of nitrogen-based flame retardants can promote the carbonization of phosphorus-based, which has a synergistic effect

Method used

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  • A kind of phosphorus nitrogen synergistic high flame retardant polyester curing agent and its synthesis method
  • A kind of phosphorus nitrogen synergistic high flame retardant polyester curing agent and its synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A method for synthesizing a phosphorus-nitrogen synergistic highly flame-retardant polyester curing agent (A), the steps of which are as follows:

[0037] (1) Add 78.7g of ethylene glycol and 85g of neopentyl glycol to a 1L four-necked flask equipped with a heating mantle, agitator, thermometer, distillation column and condenser, heat up to about 120°C, heat and stir to melt;

[0038]⑵Add 283.99g tris-(4-hydroxymethylphenoxy)-triphenoxycyclotripolyphosphazene, 282.57g DOPOITA ([(6-oxo-(6H)-dibenzo-(c,e)( 1,2)-Oxaphosphorin-6-one)methyl]-succinic acid), 39.75g of adipic acid, 30.13g of isophthalic acid and 0.8g of monobutyltin oxide, nitrogen protection, to be After it dissolves, slowly raise the temperature to 150°C to start the esterification reaction and the by-product water flows out. During the reaction, control the temperature of the distillation column not higher than 100°C, and then carry out the segmented esterification reaction at 150-180°C for 2-4 hours , Rea...

Embodiment 2

[0043] A method for synthesizing a phosphorus-nitrogen synergistic highly flame-retardant polyester curing agent (B), the steps of which are as follows:

[0044] (1) Add 42.02g of ethylene glycol and 150g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, agitator, thermometer, distillation column and condenser, heat up to about 120°C, heat and stir to melt;

[0045] (2) Add 221.1g of tris-(4-hydroxymethylphenoxy)-triphenoxycyclotripolyphosphazene, 234.66g of DOPOITA, 49.52g of adipic acid, 42.22g of isophthalic acid and 0.74g of monobutyltin oxide , protected by nitrogen gas, after it dissolves, slowly raise the temperature to 150°C to start the esterification reaction and the by-product water flows out, control the temperature of the distillation column not higher than 100°C during the reaction, and then carry out the segmented esterification reaction, 150~ React at 180°C for 2-4 hours, at 180-220°C for 2-4 hours, at 220-240°C for 1-2 hours; when the...

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Abstract

The invention relates to a nitrogen-phosphorus synergistic high-flame retardant polyester curing agent and a synthesis method thereof. The synthesis method is characterized in that polyhydric alcohols, a reactive phosphonitrile compound, polyatomic acid, a reactive DOPO compound and a catalyst are prepared into the nitrogen-phosphorus synergistic high-flame retardant polyester curing agent through the sectional synthesis process by controlling the proportion of each component, the reaction temperature, the reaction time and other conditions; the prepared nitrogen-phosphorus synergistic high-flame retardant polyester curing agent has acid value of 60 to 130mg KOH / g, melt viscosity of 1,000 to 8,000 mPa.s / 180 DEG C and softening point of 75 to 130 DEG C and contains 5 to 8wt% of P and 1 to 2wt% of N. With the organic combination of phosphorus oxide, heterocyclic organic phosphorus and nitrogen-phosphorus synergism, the polyester curing agent synthesized by the synthesis method is relatively high in flame resistance, heat resistance and hydrolysis resistance, and can be applied to an electronic packaging material for realizing halogen-free flame retardant performance of the electronic packaging material as well as bringing the electronic packaging material with outstanding flame retardant persistence, heat resistance, hydrolysis resistance and electrical performance.

Description

technical field [0001] The invention belongs to the field of electronic packaging materials, in particular to a phosphorus-nitrogen synergistic high flame-retardant polyester curing agent and a synthesis method thereof. Background technique [0002] Epoxy resin is one of the most widely used matrix resins in polymer-based composite materials. It is a product obtained by polycondensation reaction of compounds with epoxy groups and polyhydric hydroxyl or polyol compounds. It has excellent adhesion, resistance Chemical corrosion, electrical insulation properties, mechanical properties, and easy processing, low shrinkage, small linear expansion coefficient, and low cost are widely used in the packaging of electronic components such as varistors, ceramic capacitors, diodes, and triodes. [0003] However, since the limiting oxygen index (LOI) of epoxy resin is low, only 19.5, it is a flammable substance, so it needs to be treated with flame retardancy. Usually, the method to impr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/692C08G59/40
Inventor 沈纪洋刘志轩
Owner 天津凯华绝缘材料股份有限公司