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A kind of halloysite nanotube halogen-free expansion flame retardant and its preparation method and application

A technology of halloysite nanotubes and intumescent flame retardants, which is applied in the field of flame retardants, can solve the problems of large damage to mechanical properties, high price, and large addition amount, and achieve high flame retardant efficiency, small impact on physical and mechanical properties, The effect of adding a small amount

Active Publication Date: 2019-09-27
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In PP intumescent flame retardants, the carbon source is the key. Traditional intumescent flame retardants use pentaerythritol, starch, etc. as charring agents, which have the disadvantages of large addition, easy precipitation, and large damage to mechanical properties.
[0003] Chinese patent application CN101225187A discloses a triazine char-forming-foaming agent, a polypropylene halogen-free flame retardant composed of ammonium polyphosphate and a synergist, and a flame retardant composed of a triazine char-forming-foaming agent Although the flame retardant effect is good, the mechanical properties of polypropylene composites are still damaged
[0004] Halogen-free intumescent flame retardants have poor compatibility with PP, which will reduce the mechanical properties (especially impact properties) of PP composites, thus limiting the application of PP in demanding occasions
It has been reported in the literature that flame retardant synergists such as montmorillonite, layered hydrotalcite, POSS, graphene, and carbon nanotubes can improve the flame retardant effect of IFR, but they are expensive and not suitable for industrial applications

Method used

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  • A kind of halloysite nanotube halogen-free expansion flame retardant and its preparation method and application
  • A kind of halloysite nanotube halogen-free expansion flame retardant and its preparation method and application
  • A kind of halloysite nanotube halogen-free expansion flame retardant and its preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) The synthetic steps of triazine series char-forming-foaming agent:

[0034] ①Add 350 grams of cyanuric chloride and 500 grams of acetone to the reaction kettle to disperse the cyanuric chloride evenly, and add 50 grams of ethanolamine and 30 grams of triethylamine dropwise at -5°C to 5°C until the pH of the solution is 5~7, react for 1~3 hours after the dropwise addition is completed;

[0035] ②Raise the temperature to room temperature, add 60 grams of ethylenediamine and 15 grams of triethylamine dropwise, keep the pH value of the solution at 5-7, raise the reaction temperature to 40°C-65°C after the dropwise addition, and react for 4-6 hours ;

[0036] ③Raise the reaction temperature, and add 60 grams of ethylenediamine and 15 grams of triethylamine dropwise into the reaction kettle at 80°C to 110°C, so that the pH of the solution is 5 to 7, and after 5 to 7 hours of reaction The acetone was distilled off, and the product was washed with water, suction filtered,...

Embodiment 2

[0039] (1) The synthetic steps of triazine series char-forming-foaming agent:

[0040] ①Add 50 grams of cyanuric chloride and 150 grams of acetone to the reaction kettle to disperse the cyanuric chloride evenly, and add 10 grams of aniline and 8 grams of triethylamine dropwise at -5°C to 5°C until the pH of the solution is 5~7, react for 1~3 hours after the dropwise addition is completed;

[0041] ②Raise the temperature to room temperature, add 20 grams of diethylenetriamine and 4 grams of triethylamine dropwise, and keep the pH value of the solution at 5-7. Hour;

[0042] ③Raise the reaction temperature, and add 20 grams of diethylenetriamine and 4 grams of triethylamine dropwise into the reaction kettle under the condition of 80℃~110℃, so that the pH value of the solution is 5~7, and react for 5~7 hours Afterwards, the acetone was evaporated, and the product was washed with water, suction filtered, and dried to obtain 60 grams of triazine-based char-forming-foaming agent. ...

Embodiment 3

[0047](1) The synthetic steps of triazine series char-forming-foaming agent:

[0048] ①Add 350 grams of cyanuric chloride and 500 grams of acetone to the reaction kettle to disperse the cyanuric chloride evenly, and add 50 grams of ethanolamine and 30 grams of triethylamine dropwise at -5°C to 5°C until the pH of the solution is 5~7, react for 1~3 hours after the dropwise addition is completed;

[0049] ②Raise the temperature to room temperature, add 60 grams of ethylenediamine and 15 grams of triethylamine dropwise, keep the pH value of the solution at 5-7, raise the reaction temperature to 40°C-65°C after the dropwise addition, and react for 4-6 hours ;

[0050] ③Raise the reaction temperature, and add 60 grams of ethylenediamine and 15 grams of triethylamine dropwise into the reaction kettle at 80°C to 110°C, so that the pH of the solution is 5 to 7, and after 5 to 7 hours of reaction The acetone was distilled off, and the product was washed with water, suction filtered, ...

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Abstract

The invention belongs to the technical field of flame retardants, and particularly relates to a halloysite-containing nanotube halogen-free intumescent flame retardant and a preparation method and application thereof. The halloysite-containing nanotube halogen-free intumescent flame retardant is prepared from a triazine charring-foaming agent, a phosphorus compound and a halloysite nanotube, wherein the halloysite nanotube accounts for 1 to 30 percent of the total weight of the halloysite-containing nanotube halogen-free intumescent flame retardant; the mass ratio of the triazine charring-foaming agent to the phosphorus compound is 1 to (1 to 5). The halloysite-containing nanotube halogen-free intumescent flame retardant has the characteristics of high flame retardance efficiency, small additive amount and small influence on the physical and mechanical performance of composite materials, and can be widely applied in the fields of automobiles, domestic appliances, building materials and the like.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a halogen-free expansion flame retardant containing halloysite nanotubes and a preparation method and application thereof. Background technique [0002] Intumescent flame retardant is one of the types of flame retardants widely used in recent years. This flame retardant overcomes the fact that halogenated flame retardants are easy to emit irritating and corrosive gases and smoke when burning, pollute the environment, and endanger human health. , while corroding equipment and other shortcomings, it is a very promising green and environmentally friendly flame retardant Intumescent flame retardant is composed of acid source, carbon source and gas source: (1) acid source: it can release inorganic acid under heating conditions The compound promotes the dehydration and carbonization of polyhydroxy compounds; (2) carbon source: polyhydroxy compounds rich in carbon a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L23/12C08L23/14C08L79/02C08K9/04C08K7/26C08K3/32C08K5/3492
Inventor 许家友黄思雯邓海铭
Owner GUANGZHOU UNIVERSITY