Flexible flame-retardant polyester curing agent with star-like branched structure, and synthesis method thereof

Abstract

The invention relates to a flexible flame-retardant polyester curing agent with a star-like branched structure, and a synthesis method thereof. The flexible flame-retardant polyester curing agent with the star-like branched structure is prepared by controlling the conditions such as proportion of polyalcohols, polyprotic acid, hexa(4-carboxyl phenoxyl)cyclotriphosphazene and catalyst, reaction temperature, reaction time and the like through adopting segmental synthesis technology, the acid value ranges from 120mgKOH / G to 260mgKOH / G, the melt viscosity ranges from 1500mPa.s / 150DEG C to 6000mPa.s / 150DEG C, and the softening point ranges from 60 DEG C to 110 DEG C. the synthesis method is simple in steps and stable to produce, the prepared polyester resin has the characteristics of being low in viscosity, high in functionality, free from chain winding, good in solubility, excellent in flame retardance and the like, not only can realize the non-halogenation of an electronic packaging material, but also can endow the electronic packaging material with excellent flexibility when being used for the electronic packaging materials, so that the cold and heat impact resistance of the electronic packaging material can be greatly improved.

Description

technical field

[0001] The invention belongs to the field of electronic packaging materials, in particular to a flexible flame-retardant polyester curing agent with a star-shaped branch structure 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. Due to the requirem...

Examples

Embodiment 1

[0036] A method for synthesizing a flexible flame-retardant polyester curing agent (A) with a star-shaped branched structure, the steps are as follows:

[0037] (1) Add 22.49g of ethylene glycol and 170g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column and condenser, heat to about 120°C and stir to melt, then add 13.25g of hexyl Diacid, 15.06g of isophthalic acid and 0.22g of monobutyltin oxide are protected by nitrogen gas. After they are dissolved, the temperature is slowly raised to 150°C to start the esterification reaction, and by-product water flows out. During the reaction, the distillation column is controlled The temperature is not higher than 100°C, and then carry out segmented esterification reaction, heating reaction at 150-180°C for 2-4 hours, heating at 180-220°C for 1-3 hours, when no by-product water flows out, cool down to 100-120°C between.

[0038] (2) Add 289.25g of hexa(4-carboxyphenoxy)...

Embodiment 2

[0043] A method for synthesizing a flexible flame-retardant polyester curing agent (B) with a star-shaped branched structure, the steps are as follows:

[0044](1) Add 48.47g of ethylene glycol and 190g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column and condenser, heat to about 120°C and stir to melt, then add 114.25g of hexyl Diacid, 86.59g of isophthalic acid and 0.44g of monobutyltin oxide are protected by nitrogen gas. After they are dissolved, the temperature is slowly raised to 150°C to start the esterification reaction, and by-product water flows out. During the reaction, the distillation column is controlled The temperature is not higher than 100°C, and then carry out segmented esterification reaction, heating reaction at 150-180°C for 2-4 hours, heating at 180-220°C for 1-3 hours, when no by-product water flows out, cool down to 100-120°C between.

[0045] ⑵Add 207.82g of hexa(4-carboxyphenoxy)cyc...

technical field

[0001] The invention belongs to the field of electronic packaging materials, in particular to a flexible flame-retardant polyester curing agent with a star-shaped branch structure 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. Due to the requirem...

Examples

Embodiment 1

[0036] A method for synthesizing a flexible flame-retardant polyester curing agent (A) with a star-shaped branched structure, the steps are as follows:

[0037] (1) Add 22.49g of ethylene glycol and 170g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column and condenser, heat to about 120°C and stir to melt, then add 13.25g of hexyl Diacid, 15.06g of isophthalic acid and 0.22g of monobutyltin oxide are protected by nitrogen gas. After they are dissolved, the temperature is slowly raised to 150°C to start the esterification reaction, and by-product water flows out. During the reaction, the distillation column is controlled The temperature is not higher than 100°C, and then carry out segmented esterification reaction, heating reaction at 150-180°C for 2-4 hours, heating at 180-220°C for 1-3 hours, when no by-product water flows out, cool down to 100-120°C between.

[0038] (2) Add 289.25g of hexa(4-carboxyphenoxy)...

Embodiment 2

[0043] A method for synthesizing a flexible flame-retardant polyester curing agent (B) with a star-shaped branched structure, the steps are as follows:

[0044](1) Add 48.47g of ethylene glycol and 190g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column and condenser, heat to about 120°C and stir to melt, then add 114.25g of hexyl Diacid, 86.59g of isophthalic acid and 0.44g of monobutyltin oxide are protected by nitrogen gas. After they are dissolved, the temperature is slowly raised to 150°C to start the esterification reaction, and by-product water flows out. During the reaction, the distillation column is controlled The temperature is not higher than 100°C, and then carry out segmented esterification reaction, heating reaction at 150-180°C for 2-4 hours, heating at 180-220°C for 1-3 hours, when no by-product water flows out, cool down to 100-120°C between.

[0045] ⑵Add 207.82g of hexa(4-carboxyphenoxy)cyc...

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