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Reactive flame retardant containing double DOPO groups and nitrogen, and preparation method and application thereof

A reactive flame retardant and reaction technology, which is applied in the field of flame retardant materials, can solve problems such as failure to meet the performance requirements of flame retardants, poor flame retardant performance, and field limitations, and achieve improved condensed phase flame retardant effects and reduced carbon residues. The effect of reducing the rate and reducing the amount of addition

Active Publication Date: 2019-08-23
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The epoxy resin obtained by using this curing agent has an LOI of 28.1. Although it is still in the category of flame retardants, the LOI value is still low. Currently, flame retardant materials used in building materials and transportation have increasingly stringent requirements for flame retardant properties. In some cases, it may not be able to meet the performance requirements of flame retardants, and its reactive groups are phenolic hydroxyl groups and benzoic acid groups. Even after reacting with resins, they are extremely easy to hydrolyze and deteriorate the flame retardant performance, making it applicable field is restricted

Method used

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  • Reactive flame retardant containing double DOPO groups and nitrogen, and preparation method and application thereof
  • Reactive flame retardant containing double DOPO groups and nitrogen, and preparation method and application thereof
  • Reactive flame retardant containing double DOPO groups and nitrogen, and preparation method and application thereof

Examples

Experimental program
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Effect test

preparation example

[0037] Dissolve 1.39g (0.015mol) of aniline, 1.22g (0.01mol) of p-hydroxybenzaldehyde and 1.51g (0.05mol) of paraformaldehyde in 50mL of dioxane, and react at 80°C for 10 hours under stirring conditions. After the end, suction filtration under reduced pressure gave a light yellow solid 3-phenyl-6-aldehyde-3,4-dihydro-2H-1,3-benzoxazine PHB with a yield of 94%, and its H NMR spectrum was as follows: figure 1 As shown; 2.39g (0.01mol) of PHB and 6.48g (0.03mol) of DOPO were respectively added into a three-necked flask, and 20ml of anhydrous toluene was added, protected by nitrogen, heated to 130°C, and reacted for 5 hours under magnetic stirring. After the reaction was completed, the solvent was removed by filtration to obtain a light yellow solid, which was then poured into toluene for washing and filtered. Repeat 3 times, thereby remove excessive DOPO, obtain target flame retardant DB, the compound shown in formula (II), product is through proton nuclear magnetic resonance spe...

Embodiment 1

[0045] The preparation of the epoxy resin modified by embodiment 1 reactive flame retardant (DB)

[0046] First, the flame retardant DB synthesized in Preparation Example 1 was ground into powder. Weigh 100g of epoxy resin E-44, raise the temperature to 140°C, add 5g of flame retardant DB, then add 30g of curing agent 4,4'-diaminodiphenylsulfone (DDS), stir well and pour into preheated poly Tetrafluoroethylene mold was kept at 180°C for 4 hours to obtain a flame retardant-modified epoxy resin called PEa1.

[0047] Prepare flame retardant modified epoxy resin samples according to the same method, the difference is that the addition amount of flame retardant DB is different: the addition amount of DB is 10g, and the epoxy resin modified by flame retardant of gained is called PEa2; The addition amount is 15g, and the epoxy resin modified by the flame retardant is called PEa3; and the addition amount of DB is 20g, and the epoxy resin modified by the flame retardant is called PEa4...

Embodiment 2

[0051] Example 2 Preparation of reactive flame retardant (DB) and benzoxazine (PHB) compound system modified epoxy resin:

[0052] First, the flame retardant DB synthesized in Preparation Example 1 was ground into powder. Weigh 100g of epoxy resin E-44, heat up to 140°C, do not add flame retardant DB, then add 30g of curing agent 4,4'-diaminodiphenylsulfone (DDS), 5g of aldehyde benzoxazine ( PHB) is poured into the preheated polytetrafluoroethylene mold after stirring evenly, and is kept at 180 ℃ for 4 hours, and the epoxy resin obtained is called PEb1.

[0053] Prepare flame retardant modified epoxy resin samples according to the same method, the difference is that the addition amount of flame retardant DB is different: the addition amount of DB is 5g, and the epoxy resin modified by flame retardant of gained is called PEb2; The addition amount is 10g, and the epoxy resin modified by the flame retardant is called PEb3; the addition amount of DB is 15g, and the epoxy resin m...

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Abstract

The invention discloses a reactive flame retardant containing double DOPO groups and nitrogen, and a preparation method and an application thereof. The reactive flame retardant containing double DOPOgroups and nitrogen can be prepared in a high yield through a two-step reaction by the simple and efficient synthesis method. The reactive groups on the molecule of the reactive flame retardant are reacted with an epoxy resin to effectively improve the flame retardation property of the epoxy resin and improve the mechanical properties to a certain degree; the epoxy resin is modified with the reactive flame retardant to simultaneously improve the flame retardation effect and the mechanical strength of the epoxy resin, the synergistic flame-retardant effect of phosphorus and nitrogen greatly improves the flame retardation property of the modified epoxy resin at a very low dosage of the flame retardant, and results of limiting oxygen index and UL-94 vertical burning test show that the flame retardancy reaches V-0 level, and the limiting oxygen index (LOI) reaches 30.9. The preparation method of the reactive flame retardant containing double DOPO groups and nitrogen has the advantages of simplicity, and cheap and easily available raw materials, so the reactive flame retardant containing double DOPO groups and nitrogen is a reactive flame retardant hopeful to be industrialized.

Description

technical field [0001] The invention belongs to the technical field of flame retardant materials, in particular to a phosphorus-containing reactive macromolecular flame retardant and its preparation and application. Background technique [0002] Since epoxy resin was invented in 1936, it has been widely used in almost all fields such as transportation, infrastructure construction, ship and ocean, and aerospace because of its good physical and chemical properties. However, due to the flammability of general-purpose epoxy resin, it cannot be used in some specific occasions, or in daily life, once a fire occurs, it will threaten people's lives and safety. With the gradual refinement and functionalization of the epoxy resin industry, and the gradual enhancement of people's environmental awareness, some halogen flame retardants are gradually banned. Therefore, the development of new high-efficiency halogen-free flame retardants is currently a hot research topic for scientists. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08L63/00C09D5/18C07F9/6574
CPCC07F9/657172C08K5/5399C09D5/18C08L63/00
Inventor 李向梅刘奔奔杨荣杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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