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Melamine-based nitrogen and phosphorus-containing compound, preparation method and application thereof, and flame-retardant epoxy resin composition of melamine-based nitrogen and phosphorus-containing compound

A melamine-based and melamine-based benzene technology is applied in the field of melamine-based nitrogen-containing phosphorus compounds and can solve the problems of flammability of epoxy resins and the like

Active Publication Date: 2021-04-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the flammability problem of existing epoxy resins, the present invention provides a melamine-based nitrogen-phosphorous compound and its preparation method and application

Method used

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  • Melamine-based nitrogen and phosphorus-containing compound, preparation method and application thereof, and flame-retardant epoxy resin composition of melamine-based nitrogen and phosphorus-containing compound
  • Melamine-based nitrogen and phosphorus-containing compound, preparation method and application thereof, and flame-retardant epoxy resin composition of melamine-based nitrogen and phosphorus-containing compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] R 1 is a hydrogen atom, R 2 The synthetic steps of the melamine-based nitrogen-containing phosphorus compound of hydrogen atom are as follows:

[0040] 7.77g melamine (commercially available), 12.21g paraformaldehyde (commercially available), and 17.39g phenol (commercially available) were added to a three-necked flask with a stirring device, and a certain amount of triethylamine (commercially available) was added dropwise to adjust pH to 9, under stirring and 100 ℃ temperature condition, carry out reaction 5h, after completion of reaction, vacuum drying obtains intermediate product; Then, 19.2g above-mentioned intermediate and 30.24g DOPO (commercially available) (the molar ratio of intermediate and DOPO 1:3) into a three-necked flask with a stirring device, and add solvent 250g THF, stir and react at a temperature of 40°C for 24h, after the reaction is complete, cool, filter and wash, and vacuum dry to obtain powdered melamine base Nitrogen-containing phosphorus com...

Embodiment 2

[0049] R1 is a hydrogen atom, and R2 is the synthesis steps of the melamine-based nitrogen-containing phosphorus compound of methyl as follows:

[0050] 7.77g melamine (commercially available), 12.21g paraformaldehyde (commercially available), 19.98g 4-methylphenol (commercially available) are added in the there-necked flask with stirring device, drop a certain amount of triethylamine ( Commercially available) adjust the pH to 9, react under stirring and 100°C temperature conditions for 6h, after the reaction is completed, vacuum dry to obtain the intermediate product; then, 20.88g of the above intermediate and 30.24g of DOPO (commercially available) (intermediate The molar ratio to DOPO is 1:3) into a three-necked flask with a stirring device, and a solvent of 250g THF (commercially available), stirred and reacted at a temperature of 40°C for 24h, after the reaction was complete, cooled, filtered and washed , to obtain powdery melamine-based nitrogen-containing phosphorus com...

Embodiment 3

[0059] R1 is a methyl group, and R2 is a melamine-based nitrogen-containing phosphorus compound synthetic step of a methyl group as follows:

[0060] 7.77g melamine (commercially available), 12.21g paraformaldehyde (commercially available), 22.57g 2,4-xylenol (commercially available) were added in a three-necked flask with a stirring device, and a certain amount of three Ethylamine (commercially available) was used to adjust the pH to 9, and the reaction was carried out under stirring and at a temperature of 100° C. for 8 h. After the reaction was completed, the intermediate product was obtained by vacuum drying; then, 22.56 g of the above intermediate and 30.24 g of DOPO (commercially available) (The molar ratio of the intermediate to DOPO is 1:3) into a three-necked flask with a stirring device, and add a solvent of 250g THF (commercially available), stir and react at a temperature of 40°C for 24h, after the reaction is complete, cool, Suction filtration, washing, and vacuum...

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Abstract

The invention discloses a melamine-based nitrogen and phosphorus-containing compound as well as a preparation method and application thereof. The method comprises the following steps: firstly, carrying out condensation reaction on raw materials including melamine, paraformaldehyde and aromatic phenol to prepare a melamine benzoxazine intermediate, and then reacting the intermediate with DOPO to obtain the compound. The compounds are useful as flame retardants for epoxy resins. The method is cheap in raw materials, wide in source, simple in process, efficient, safe, environmentally friendly and beneficial to batch production. The flame retardant overcomes the defects that a traditional flame retardant is large in combustion smoke, pollutes the environment, is poor in compatibility, is easy to separate out and the like. When the flame retardant is added into epoxy resin, the flame retardant property of an epoxy resin cured product can be remarkably improved, and when the addition amount of P in the epoxy resin reaches 1.0 wt%, the vertical combustion grade reaches UL94 V-0 grade, the limit oxygen index is 35-40, the charring rate at 800 DEG C reaches 23-27%, and the glass-transition temperature reaches 130-137 DEG C.

Description

technical field [0001] The present invention relates to the field of flame retardants, in particular to a melamine-based nitrogen-containing phosphorus compound, its preparation method and application. The compound can be used as a flame retardant and can be directly added to epoxy resin to participate in epoxy resin The curing reaction can effectively improve the flame retardancy and thermal properties of epoxy resin. Background technique [0002] Epoxy resin is an epoxy oligomer that can form a three-dimensional network of thermosetting plastics when it reacts with a curing agent. Because its cured product has excellent adhesion, heat resistance, chemical resistance, mechanical properties and electrical properties, it is a variety of thermosetting resins that are widely used in coatings, adhesives, Composite materials and other fields. [0003] However, epoxy resin is flammable and poses a great risk to human life and property. At present, research work on improving the...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C08K5/5313C08L63/00
Inventor 王鑫张藕生唐建华余荣禄王芳
Owner CHINA PETROLEUM & CHEM CORP
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