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Phosphor and nitrogen containing flame retardant curing agent, preparation method and application thereof

A curing agent, phosphorus-nitrogen technology, which is applied in the field of phosphorus-nitrogen-containing flame-retardant curing agent and its preparation, can solve the problems of glass transition temperature of only 72°C and 45°C, and large amount of smoke, and achieve low cost and high production efficiency. Simple, good flame retardant effect

Inactive Publication Date: 2012-05-02
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Chinese patent CN1916049A discloses a preparation method of a phosphorus-containing epoxy resin curing agent. After curing, the flame retardant oxygen index of epoxy can reach 29, but the glass transition temperature of epoxy after curing is less than 100°C. And the amount of smoke generated when burning is large
Jeng et al. (European Polymer Journal 2002, 38, 683-693 ) synthesized a variety of phosphorus-containing curing agents PPDCD230 and DCPD230, etc., and the flame retardancy of the cured product obtained after curing BE188 was greatly improved, but the glass transition temperature was only 72°C and 45°C
[0006] The purpose of the present invention is to provide a novel flame retardant curing agent preparation method, this kind of flame retardant can directly participate in the curing process of epoxy resin, solve the compatibility problem between epoxy resin and flame retardant, at the same time The phosphourea structure is introduced into the flame retardant structure. The phosphobenzene ring structure can promote char formation and stabilize the char layer. The urea group can release inert gas under heating conditions and dilute the concentration of combustible gas and oxygen, thereby improving the epoxy resin. Flame retardant

Method used

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  • Phosphor and nitrogen containing flame retardant curing agent, preparation method and application thereof
  • Phosphor and nitrogen containing flame retardant curing agent, preparation method and application thereof
  • Phosphor and nitrogen containing flame retardant curing agent, preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0026] Add 1 mol of 110 g of hydroquinone A to 2 mol of 180 mL of phosphorus oxychloride. React at 90°C for 5 hours, remove excess phosphorus oxychloride by rotary evaporation under reduced pressure at 85°C, then dissolve in a certain amount of anhydrous acetonitrile, add PEG-600, stir and mix well, add 3.5mol of 200g isocyanic acid in batches Methyl ester, reacted at room temperature for 2 hours, heated to 90-110°C under nitrogen gas, and refluxed for 4 hours. Suction filtration, take the filtrate, and rotary evaporation to obtain a yellow viscous substance intermediate with a yield of 70%.

[0027] The intermediate was added to a certain amount of toluene, and a mixed solution of 10 mol of diamine and toluene was added dropwise under ice-cooling. After 2 hours, the temperature was raised to 70° C., and the reaction was refluxed for 15 hours. A white solid was obtained, which was a phosphorus-nitrogen-containing flame retardant curing agent, and the yield was 90%.

[0028] ...

Embodiment 2

[0033] Add 5 mol of 47 mL of phosphorus oxychloride to 1 mol of 110 g of hydroquinone at 50°C. React at 90°C for 5 hours, remove excess phosphorus oxychloride by rotary evaporation under reduced pressure at 85°C, then dissolve in a certain amount of anhydrous acetonitrile, add PEG-400, stir and mix, add 5mol of 320g isocyanate in batches Ester, react at room temperature for 4h, heat to 70-90°C under nitrogen, and reflux for 6h. Suction filtration, take the filtrate, and rotary evaporation to obtain a yellow viscous substance intermediate with a yield of 75%.

[0034] The intermediate was added to a certain amount of toluene, and a mixed solution of 5 mol of diamine and toluene was added dropwise under ice-cooling. After 2 hours, the temperature was raised to 70° C., and the reaction was refluxed for 15 hours. A white solid was obtained, which was a phosphorus-nitrogen-containing flame retardant curing agent, and the yield was 90%.

[0035]Stir 100 parts by weight of ordinary...

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Abstract

The invention discloses a phosphor and nitrogen containing flame retardant curing agent, a preparation method and application thereof. The curing agent has a phosphorylurea structure, contains active ammonia and hydrogen atoms, has dual functions of both a flame retarding agent and a curing agent, and can be directly used for curing epoxy resin. In a curing progress, flame retardant elements are embedded into an epoxy structure, thus avoiding phase separation phenomenon due to introduction of additive type flame retarding agent. Phosphor elements mainly function in flame retarding of a condensed phase while a urea structure mainly functions in flame retarding of a gas phase. The curing agent can react with common epoxy resin to obtain uniform and transparent cured object; in addition, the curing agent has low phosphorus content, passes 1.6 mm UL 94 V0 level, reaches oxygen index as high as 29-34%, and has excellent flame retardance; in thermo-gravimetric analysis, the maximum thermal decomposition temperature is as high as 400 DEG C; the char yield of the curing agent at 700 DEG C is 35%; and glass transition temperature of the curing agent is as high as 150 DEG C. The curing agent can also realize co-curing together with common curing agents, such as, diaminodiphenyl sulfone and anhydride-type epoxy curing agents. The curing agent is low in cost, simple in production process, and available for industrial production.

Description

technical field [0001] The invention relates to the field of flame-retardant curing agents, in particular to a phosphorus-nitrogen-containing flame-retardant curing agent and its preparation method and application. Background technique [0002] Due to its good mechanical strength, electrical insulation, chemical corrosion resistance and other properties, epoxy resin cured products have been widely used in the bonding, packaging and manufacturing of printed circuit boards (PCBs) of electronic components, and have become a supporting industry for the electrical and electronic industries. important pillar. However, like most polymer materials, epoxy cured products are extremely flammable, and the most common in the industry is halogen-containing flame-retardant epoxy cured products. [0003] The European Union's "Waste Electrical and Electronic Equipment Law (WEEE)" and "Restriction of the Use of Certain Hazardous Substances in Electrical and Electronic Equipment (RoHS)" draft...

Claims

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Application Information

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IPC IPC(8): C08G59/40C08G59/50C07F9/24
Inventor 韦平赵小敏钱勇俞海州郭琪
Owner SHANGHAI JIAO TONG UNIV
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