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Metal phenyl phosphonate flame retardant material with controllable morphology, preparation method and application

A technology of phenylphosphonate and flame retardant material, applied in the field of polymer flame retardant, can solve the problems of low thermal stability and easy hydrolysis

Active Publication Date: 2020-12-22
XIAMEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphorus-based flame retardants have the advantages of high efficiency and environmental protection, but there are problems such as low thermal stability and easy hydrolysis

Method used

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  • Metal phenyl phosphonate flame retardant material with controllable morphology, preparation method and application
  • Metal phenyl phosphonate flame retardant material with controllable morphology, preparation method and application
  • Metal phenyl phosphonate flame retardant material with controllable morphology, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～4

[0032] Preparation of metal phenylphosphonate flame retardant materials:

[0033] (1) Add 1g of graphene oxide and 300mL of water to the reaction vessel, ultrasonicate for 1h at room temperature, stir for 2h, then add 2g of piperazine to the vessel, and 2 Condensate and reflux at 100°C for 6h under atmosphere, filter to obtain a black precipitate, and dry under vacuum at 60°C to obtain piperazine reduction-modified graphene oxide (Pip-GO).

[0034] (2) Add 0.632g of phenylphosphonic acid, 50mL of water and 0.632g of Pip-GO to four reaction vessels and stir for 30min, then add 0.868g of cerium nitrate, 0.75g of aluminum nitrate, 0.439g of Zinc acetate and 0.498g cobalt acetate were stirred for 30 minutes, and the reaction solutions were poured into four tetrafluoroethylene reactors, reacted at 100°C for 24h, washed with ethanol, and vacuum-dried at 60°C to obtain the four metal benzenes. Based phosphonate flame retardant materials (CeHPP-PG, AlHPP-PG, CoHPP-PG, ZnHPP-PG).

[...

Embodiment 5～8

[0038] Preparation of flame retardant epoxy resin:

[0039]Take by weighing four parts of epoxy resin prepolymer 20g respectively, heat up to 80 DEG C, add respectively 0.25g (1wt%) cerium phenylphosphonate, phenyl phosphonate in four parts of epoxy resin prepolymer Aluminum phosphonate, zinc phenylphosphonate and cobalt phenylphosphate flame retardant materials and 30mL chloroform were ultrasonically stirred until transparent, pumped until no bubbles were generated, and then 5g of curing agent 4,4-diaminodiphenylmethane ( DDM) until completely dissolved, then poured into a preheated mold, and cured at 120°C for 4h, 140°C for 3h, and 180°C for 2h to obtain four flame-retardant epoxy resins (CeHPP-PG / EP, AlHPP-PG / EP, CoHPP-PG / EP, ZnHPP-PG / EP).

[0040] Get the flame retardant epoxy resin obtained and do the oxygen index test. According to GB / T 2406-2009, the oxygen indices of CeHPP-PG / EP, AlHPP-PG / EP, CoHPP-PG / EP and ZnHPP-PG / EP are 26.9%, 26.5%, 25.2%, and 25.4%, respective...

Embodiment 9～12

[0042] Preparation of metal phenylphosphonate flame retardant materials:

[0043] (1) Add 1g of graphene oxide and 300mL of water to the reaction vessel, ultrasonicate for 1h at room temperature, stir for 2h, then add 2g of piperazine to the vessel, and 2 Condensate and reflux at 100°C for 6h under atmosphere, filter to obtain a black precipitate, and dry under vacuum at 60°C to obtain piperazine reduction-modified graphene oxide (Pip-GO).

[0044] (2) Add 0.632g of phenylphosphonic acid, 50mL of water and 1.264g of Pip-GO to four reaction vessels and stir for 30min, then add 0.868g of cerium nitrate, 0.75g of aluminum nitrate, 0.439g of Zinc acetate and 0.498g cobalt acetate, stirred for 30min, the reaction solution was poured into four tetrafluoroethylene reactors, reacted at 100°C for 24h, washed with ethanol, and vacuum-dried at 60°C to obtain the four kinds of metal phenyl Phosphonate flame retardant materials (CeHPP-PG, AlHPP-PG, CoHPP-PG, ZnHPP-PG).

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Abstract

The invention discloses a metal phenyl phosphonate flame-retardant material with controllable appearance, and a preparation method and application thereof. The flame-retardant material is obtained bycoordinating phenyl phosphonic acid with various metal ions and then carrying out reacting with piperazine-reduced graphene oxide. The graphene has a shielding and blocking effect, the metal phenyl phosphonate material has good catalytic carbon forming performance, and the synergistic effect of the graphene and the metal phenyl phosphonate material greatly improves flame retardant performance of the high polymer material. The flame retardant has good thermal stability and flame retardant performance, has a simple and feasible preparation method, and has a wide application prospect in the fieldof high molecular flame retardant.

Description

technical field [0001] The invention belongs to the field of flame retardant polymers, and in particular relates to a metal phenylphosphonate flame retardant material with adjustable shape, a preparation method and an application thereof. Background technique [0002] Polymer materials have good mechanical, physical and chemical properties and corrosion resistance, and are widely used, such as communications, electronics, medical, chemical, aerospace and other fields. However, most polymer materials are easy to burn, and there is a huge fire hazard, which greatly limits the practical application of polymer materials. Therefore, flame-retardant modification of polymer materials has become an important means to broaden its application fields. According to the flame retardant elements, flame retardants can be divided into halogen-based, organic phosphorus-based, nitrogen-based, silicon-based and nitrogen-phosphorus-silicon metal compounds. Phosphorus-based flame retardants hav...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/04C08K3/04C08K7/00C08K5/5399C08K5/00C08L63/00C08L77/00C07F9/6509C07F9/38
CPCC07F9/38C07F9/650952C08K5/0091C08K5/5399C08K7/00C08K9/04C08L2201/02C08K3/042C08L63/00C08L77/00
Inventor 戴李宗王秀杨杰陈婷洪静吴腾达鹿振武陈国荣曾碧榕罗伟昂
Owner XIAMEN UNIV
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