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Novel environmentally friendly phosphorus based flame retardant 2-(diphenylphosphine acyl)-1, 4-benzenediol as well as preparation method thereof and flame retardant epoxy resin composite

The technology of phosphorus-based flame retardant and diphenylphosphonyl, which is applied in the field of polymer materials, can solve the problems such as the decrease of heat resistance and mechanical properties of epoxy resin cured products, the limitation of addition amount for practical application, and the high price of DOPO. To achieve the effect of superior flame retardant performance, environmental protection and simple synthesis and purification process, and suitable for industrial production

Inactive Publication Date: 2013-12-04
BINHAI JINXIANG CHEM AUXILIARY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high price of DOPO, such a high amount of addition limits its practical application, and the addition of a large amount will also cause the heat resistance and mechanical properties of the epoxy resin cured product to decline

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Equipped with mechanical stirring, thermometer, reflux condenser, N 2 Into a 500ml dry four-neck flask in the catheter, pass dry nitrogen to remove the air in the flask, then add 0.3mol diphenylphosphine oxide and 140ml benzene, heat to 25°C, then slowly add 0.3mol p-benzoquinone, and control the reaction temperature At 25-35°C, continue to react for 2 hours after adding, filter to obtain a light yellow solid powder, recrystallize with ethylene glycol ether to obtain a white solid powder, which is a new environmentally friendly phosphorus flame retardant DPO-HQ, and the yield is 87%.

Embodiment 2

[0019] Equipped with mechanical stirring, thermometer, reflux condenser, N 2 Into a 500ml dry four-neck flask in the catheter, pass dry nitrogen to remove the air in the flask, then add 0.3mol diphenylphosphine oxide and 140ml benzene, heat to 160°C, then slowly add 0.3mol p-benzoquinone, and control the reaction temperature At 160-180°C, continue to react for 3 hours after adding, filter to obtain a light yellow solid powder, recrystallize with ethylene glycol ether to obtain a white solid powder, which is a new environmentally friendly phosphorus flame retardant DPO-HQ, the yield is 89%.

Embodiment 3

[0021] Equipped with mechanical stirring, thermometer, reflux condenser, N 2 Into a 500ml dry four-neck flask in the catheter, pass dry nitrogen to remove the air in the flask, then add 0.3mol diphenylphosphine oxide and 140ml benzene, heat to 110°C, then slowly add 0.3mol p-benzoquinone, and control the reaction temperature At 110-120°C, continue to react for 4 hours after adding, filter to obtain a light yellow solid powder, recrystallize with ethylene glycol ether to obtain a white solid powder, which is a new environmentally friendly phosphorus-based flame retardant DPO-HQ, and the yield is 90%.

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PUM

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Abstract

The invention discloses novel environmentally friendly phosphorus based flame retardant 2-(diphenylphosphine acyl)-1,4-benzenediol and a preparation method thereof. The flame retardant is reasonable in raw material price, less in additive amount and environmentally friendly and simple in preparation technology, and facilitates industrial production. A halogen-free flame retardant monocomponent epoxy resin composite containing the novel environmentally friendly phosphorus based flame retardant can be stored under room temperature, and is superior in flame retardant property after solidification; when the phosphorus content achieves 1.8%, the solidification flame retardant rating can achieve UL94 V-0; however, the DOPO flame retardant can achieve the same effect only when the phosphorus content thereof achieves 2.1%. The additive amount of the flame retardant is low, the cost is low, and the good mechanical property of the halogen-free flame retardant epoxy resin cured substance can be retained better.

Description

Technical field [0001] The present invention involves the field of polymer materials, which specifically involves the new type of environmentally friendly phosphorus flame retardant 2- (dihebenzyl galcol) -1,4-phenylphenol and its preparation method, which is suitable for epoxy resin compositions. Background technique [0002] Painting materials, stack products, variable semiconductor and insulation materials for electrical equipment.However, epoxy resin curing is flammable. With the increasing environmental requirements, its flame retardant, especially halogen-free flame retardant, is very urgent.(DOPO) is an important organic phosphorus flame retardant, which contains a linked phenyl -rigid structure. Compared with other flame retardants, the heat resistance and mechanical properties of epoxy resin have less influence and have received widespread attention in recent years.Introduce hydroxyl, carboxyl, amino groups, etc. in the DOPO molecular structure, which can obtain an epoxy...

Claims

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Application Information

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IPC IPC(8): C08K5/5397C08L63/02C07F9/53
Inventor 岳群王忠卫赵经纬
Owner BINHAI JINXIANG CHEM AUXILIARY
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