Phosphorus-nitrogen cooperative flame-retardant epoxy polymer and preparation method thereof

A technology of epoxy polymer and synergistic flame retardant, which is applied in the field of polymer flame retardant, can solve the problems of small migration, lack of effect of chemical bonds and resin matrix connection, etc., and achieve small impact on mechanical properties, high conversion rate, and reaction The effect of mild conditions

Active Publication Date: 2015-09-16
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because it is essentially an additive flame retardant, it is due to the physical cross-linking of the polymer chain and the resin matrix to achieve the purpose of less migration, or it cannot achieve the effect of connecting the resin matrix with chemical bonds.

Method used

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  • Phosphorus-nitrogen cooperative flame-retardant epoxy polymer and preparation method thereof
  • Phosphorus-nitrogen cooperative flame-retardant epoxy polymer and preparation method thereof
  • Phosphorus-nitrogen cooperative flame-retardant epoxy polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step 1, the synthesis of the first polymerized monomer (MAdiDOPO) described:

[0037] First, 43.2g (0.2mol) of DOPO, 10.9g (0.1mol) of p-aminophenol, 6.0g (0.1mol) of paraformaldehyde and 200mL of ethanol were added to a 500mL three-necked flask, and the reaction was stirred at 50°C for 5h , the product was washed with methanol to obtain a phenolic intermediate compound. Then, 33.2g (0.05mol) of the prepared phenolic intermediate 10.1g (0.10mol) of triethylamine and 100mL of dichloromethane were placed at 0°C and slowly dripped into 10.5g (0.10mol) Methacryloyl chloride, after the dropwise addition, continue to stir and react for 8 hours, filter to remove triethylamine hydrochloride, and purify the crude product by washing, rotary evaporation and drying to obtain the phosphorus nitrogen flame retardant MAdiDOPO containing active double bonds (References: CN104262398A).

[0038] Step 2, the synthesis of the second polymerized monomer (UPyMA) described:

[0039] Comple...

Embodiment 2～8

[0043] Experimental steps 1 and 2 are the same as in Example 1. The preparation method of step 3 is similar to that of Example 1, except that the ratio of different monomers is adjusted by adjusting the value of x:y:z, so that the ratio of phosphorus to nitrogen in the polymer is changed. The specific feeding ratio of UPyMA, GMA, and MAdiDOPO is shown in Table 1:

[0044] Table 1

[0045]

Example 2

Example 3

Example 4

Example 5

Example 6

Example 7

Example 8

UPyMA

20

30

40

50

60

70

0

GMA

30

30

30

30

30

30

30

MAdiDOPO

50

40

30

20

10

0

70

[0046] Those of ordinary skill in the art will know that when the technical parameters of the present invention vary within the following ranges, it can be expected to obtain the same or similar technical effects as those of the above-described embodiments:

[0047] A phosphorus-nitrogen syner...

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Abstract

The invention discloses a phosphorus-nitrogen cooperative flame-retardant epoxy polymer and a preparation method thereof. The molecular weight of the phosphorus-nitrogen cooperative flame-retardant epoxy polymer is within the range of 7000-100000g / mol, and the structural formula of the polymer is as shown in the specification, wherein R1, R2 and R3 can be H or methyl; X is a benzene ring or a C2-6 linear alkyl; x: y: z=(10-50): (10-30): (50-10). The polymer contains epoxy groups having extremely high reaction activity, and the epoxy groups can be well dispersed and connected in the epoxy resin by virtue of chemical bonds, and therefore, the defects of poor compatibility, easy migration and the like of a non-reactive flame-retardant polymer are avoided. The polymer simultaneously contains two flame-retardant elements P and N and therefore is good in flame-retardant effect; the polymer can be used as a flame retardant or an intrinsically flame-retardant polymer; the polymer hardly affects the mechanical properties of a material substrate; the preparation method of the polymer is simple, good in repeatability and suitable for expanded production.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polymers, and in particular relates to a phosphorus-nitrogen synergistic flame-retardant epoxy polymer and a preparation method thereof. Background technique [0002] Epoxy resin, as a thermosetting polymer material with excellent performance, is widely used in coatings, adhesives, composite materials and other fields, and has a history of more than 60 years. Recent research has focused on the diversification and high-performance applications of epoxy resins, but the lack of flame retardancy has limited the development of epoxy resins in high-end fields such as electronic appliances. Therefore, most epoxy resins must undergo flame retardant treatment in practical applications to make them reach the corresponding flame retardant level stipulated by the state. At present, the most commonly used method is to solve the flammability problem of polymer materials by adding halogenated flame reta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F230/02C08F220/36
Inventor 戴李宗刘诚陈国荣罗伟昂陈婷袁丛辉许一婷常迎
Owner XIAMEN UNIV
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