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Phosphorus-silicon-nitrogen-containing metal ion complex flame retardant, and preparation method and application thereof

A metal ion and complex technology, applied in the field of organic-inorganic hybrid materials, can solve the problems of loss of matrix mechanical properties, poor resin compatibility, and high curing temperature, and achieve improved mechanical properties, flame retardant properties, and reduced Effect of curing temperature

Active Publication Date: 2019-04-19
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the metal elements currently introduced into epoxy resins are usually inorganic fillers such as inorganic salts and metal oxides, which have poor compatibility with resins. Although they are introduced into the matrix by mechanical blending, the agglomeration phenomenon is still obvious and will loss of mechanical properties of the matrix
In addition, some high-temperature epoxy curing agents have high curing temperature and long time when used alone, and often need to add accelerators to catalyze the curing of epoxy resin.
At present, there are few reports in the literature that the combination of metal ions, POSS, and DOPO can be used as flame retardants for epoxy resins through coordination.

Method used

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  • Phosphorus-silicon-nitrogen-containing metal ion complex flame retardant, and preparation method and application thereof
  • Phosphorus-silicon-nitrogen-containing metal ion complex flame retardant, and preparation method and application thereof
  • Phosphorus-silicon-nitrogen-containing metal ion complex flame retardant, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: When preparing R is isobutyl, metal ion M is Fe 3+ , the selected metal salt is Fe(NO 3 ) 3 .9H 2 O, the curing agent is methyltetrahydrophthalic anhydride, the accelerator is imidazole, and the synthesis conditions are as follows, at this time m=3, n=3:

[0033] (1) Synthesis of iron ion complex flame retardant containing phosphorus, silicon and nitrogen

[0034] 8.75g of NH 2 -POSS, 2.60g of DOPO and 1.66g of 3,4-dihydroxybenzaldehyde were added to a 250mL three-necked flask connected with a condenser tube, dissolved in a mixed solution of 100mL of chloroform and 50mL of anhydrous methanol, and were 2For protection, stir at 55°C for 12h. After the reaction, the reaction solution was concentrated by rotary evaporation to about 25 mL, slowly added dropwise into ice methanol, precipitated, and filtered under reduced pressure. Precipitation with ice methanol was repeated three times, and finally vacuum-dried for 24 hours to obtain the ligand PDC. 10.9...

Embodiment 2

[0048] Embodiment 2: when preparing R is isobutyl, metal ion M is Cu 2+ , the selected metal salt Cu(CH 3 CH 2 COO) 2 , the synthesis conditions are as follows, at this time, m=2, n=2:

[0049] (1) Synthesis of copper ion complex flame retardant containing phosphorus, silicon and nitrogen

[0050] 8.75g of NH 2 -POSS, 2.60g of DOPO and 1.66g of 3,4-dihydroxybenzaldehyde were added to a 250mL three-neck flask connected with a condenser tube, dissolved in a mixed solution of 100mL of chloroform and 50mL of absolute ethanol, and then used N 2 For protection, stir at 55°C for 12h. After the reaction, the reaction solution was concentrated by rotary evaporation to about 25ml, slowly added dropwise into ice methanol, precipitated, and filtered under reduced pressure. Precipitation with ice methanol was repeated three times, and finally vacuum-dried for 24 hours to obtain the ligand PDC. 9.69g of the above ligand PDC and 0.73g of Cu(CH 3 CH 2 COO) 2 Dissolved in chloroform ...

Embodiment 3～8

[0060] With embodiment 1,2 technology, change the kind of metal salt in (2), calculate the charging ratio, when metal salt is Fe(CH 3 CH 2 COO) 3 , Al(CH 3 CH 2 COO) 3 , Al(NO 3 ) 3 , m=3, n=3; when the metal salt is Zn(CH 3 CH 2 COO) 2 , Cu(NO 3 ) 2 When, m=2, n=2.

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Abstract

The invention discloses a phosphorus-silicon-nitrogen-containing metal ion complex flame retardant, and a preparation method and an application thereof. The phosphorus-silicon-nitrogen-containing metal ion complex flame retardant (M(PDC)1-3) is synthesized through successfully preparing a ligand containing DOPO, POSS and catechol by a one-step process and coordinating the ligand with metal ions. The metal ion complex flame retardant has a high thermal stability, a good compatibility with epoxy resin and a strong catalysis effect, and can accelerate the generation of a large amount of residualcarbon during burning of materials to generate a dense carbon layer playing a role in thermal insulation and oxygen isolation, so the flame retardation property of a matrix is improved. The phosphorus-silicon-nitrogen-containing metal ion complex (M(PDC)1-3) can reduce the curing temperature during curing of the epoxy resin and a curing agent, so the phosphorus-silicon-nitrogen-containing metal ion complex also can be used as a promoter during curing when used as a flame retardant. The phosphorus-silicon-nitrogen-containing metal ion complex (M(PDC)1-3) greatly improves the mechanical properties of the epoxy resin when introduced into the epoxy resin.

Description

technical field [0001] The invention relates to a phosphorus-silicon-nitrogen-containing metal ion complex flame retardant and a preparation method and application thereof, belonging to the field of organic-inorganic hybrid materials. Background technique [0002] As one of many thermosetting polymer materials, epoxy resin has the advantages of high mechanical strength, good adhesion, high dimensional stability, acid and alkali resistance, etc., so it is used in various fields. However, the oxygen index of epoxy resin is only about 19.8, which is a flammable material and cannot meet the requirements of many fields. Therefore, the development of new and effective flame-retardant epoxy resins has attracted much attention. [0003] In order to improve the flame retardant properties of materials, a widely used method is to add flame retardants to epoxy resins. Phosphorus-based, silicon-based, and nitrogen-based flame retardants have been gradually developed because they meet e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/08C08L63/00C08G77/30
CPCC08G77/045C08L63/00C08L83/08C08L2201/02
Inventor 曾碧榕陈锦梅戴李宗陈国荣
Owner XIAMEN UNIV
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