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Hyperbranched expanded type flame retardant and preparation method thereof

An intumescent flame retardant and flame retardant technology, which is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem that the compatibility between flame retardants and substrates is not very good. , The flame retardant effect is not greatly improved, the synthesis steps of the flame retardant are cumbersome and other problems, to achieve the effects of high yield, reduced hygroscopicity, and short reaction time

Active Publication Date: 2017-09-05
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the one-component flame retardant uses imidazole as the gas source, which may cause harm to the environment and human health during use.
[0007] Chinese patent CN102634974A reports a flame retardant containing double-cage phosphate and its preparation method. The flame retardant is applied in the dyeing process, but the compatibility of the flame retardant with the matrix is ​​not very good, and the The combustion effect is not greatly improved
For example, Chinese patent CN102304222A reports a hyperbranched flame retardant with pentaerythritol as the center and polyphosphate as the "arm".

Method used

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  • Hyperbranched expanded type flame retardant and preparation method thereof
  • Hyperbranched expanded type flame retardant and preparation method thereof
  • Hyperbranched expanded type flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 22.14g (0.12mol) of cyanuric chloride and 250mL of dioxane into a 500mL three-necked round-bottomed flask equipped with a constant pressure dropping funnel, a serpentine condenser, and a thermometer, and stir the three with a magnetic force at 30°C. Polycyanide chloride is completely dissolved, and then 49.68g (0.276mol) of PEPA is slowly added to the flask. After half an hour of reaction, 24.24g (0.24mol) of triethylamine is slowly dropped into the round bottom flask with a constant pressure dropping funnel , The dropwise addition was completed within 1 hour, and then the reaction was continued for 1.5 hours to obtain a disubstituted product of cyanuric chloride. Continue to raise the temperature of the system to 70°C, add 3.72g (0.06mol) ethylene glycol to the round bottom flask, and then slowly drop 12.12g (0.12mol) triethylamine into the round bottom flask with a constant pressure dropping funnel In the flask, after reacting for 6 hours, cool the system to room ...

Embodiment 2

[0044]Add 22.14g (0.12mol) of cyanuric chloride and 250mL of dimethyl sulfoxide into a 500mL three-necked round-bottomed flask equipped with a constant pressure dropping funnel, a serpentine condenser, and a thermometer, and stir with magnetic force at 40°C. The cyanuric chloride is completely dissolved, and then 21.60g (0.12mol) of PEPA and 64.14g (0.12mol) of sodium lignosulfonate are slowly added to the flask, and after half an hour of reaction, 24.24g (0.24 mol) triethylamine is slowly added dropwise in the round-bottomed flask, and the dropwise addition is completed within 1.5 hours, and then the reaction is continued to obtain the disubstituted product of cyanuric chloride after 3 hours. Continue to raise the temperature of the system to 85°C, add 3.68g (0.04mol) glycerol to the round bottom flask, then slowly add 12.12g (0.12mol) triethylamine dropwise to the round bottom flask with a constant pressure dropping funnel In the flask, after reacting for 4 hours, the system...

Embodiment 3

[0046] Add 22.14g (0.12mol) of cyanuric chloride and 250mL of dimethylformamide into a 500mL three-necked round-bottomed flask equipped with a constant pressure dropping funnel, a serpentine condenser, and a thermometer, and stir with magnetic force at 50°C. Melamine chloride is completely dissolved, and then 21.60g (0.12mol) of PEPA and 13.44g (0.12mol) of trimethylsilanol are slowly added to the flask, and after half an hour of reaction, 24.24g (0.24 mol) triethylamine is slowly added dropwise in the round-bottomed flask, and the dropwise addition is completed within 1.5 hours, and then the reaction is continued to obtain the disubstituted product of cyanuric chloride after 4 hours. Continue to raise the temperature of the system to 95°C, add 3.944g (0.029mol) of pentaerythritol into the round bottom flask, then slowly drop 12.12g (0.12mol) of triethylamine into the round bottom flask with a constant pressure dropping funnel After reacting for 3 hours, the system was cooled ...

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Abstract

The invention discloses a hyperbranched expanded type flame retardant and a preparation method thereof. The method comprises the following steps: taking one or a mixture of any two of 1-oxo-4-hydroxymethyl-1-phospha-2,6,7-trioxabicyclo[2,2,2]-octane, trimethylsilanol and sodium lignosulphonate as a first monomer and taking cyanuric tricholoride as a second monomer; enabling the first monomer and the second monomer to react for 2.5h to 5.5h in an organic solvent at 30 DEG C to 50 DEG C in the presence of an acid binding agent A, so as to generate a di-substituted product; adding a third monomer polylol into the di-substituted product and reacting for 3h to 6h at 70 DEG C to 95 DEG C for in the presence of an acid binding agent B, so as to obtain the hyperbranched expanded type flame retardant. The adding amount of the hyperbranched flame retardant disclosed by the invention in a matrix is low and the branching degree of the flame retardant is increased so that the flame retardant is difficult to crystallize and has no chain entanglement; the dispersity of the flame retardant in the matrix and the compatibility of the flame retardant and the matrix are improved and the moisture absorption of the flame retardant is reduced; the water resistance and migration resistance of the flame retardant are improved.

Description

[0001] (1) Technical field [0002] The invention relates to the field of three-source integrated intumescent flame retardants, in particular to a hyperbranched intumescent flame retardant and its preparation method and application. [0003] (2) Background technology [0004] With the continuous development of science and technology, human life has become increasingly inseparable from polymer materials. However, polymer materials often encounter many problems during use, such as heat aging, light aging, combustion, static electricity, etc. Among them, the flammability of polymer materials is the biggest problem they face during use, so usually To add a flame retardant to the polymer to improve its flame retardant performance. At present, the most used in the world is still the halogen flame retardant, but the halogen flame retardant will generate a lot of smoke and toxic and corrosive gas when burning, which will cause great harm to the environment and the human body, so it is...

Claims

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Application Information

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IPC IPC(8): C08K5/521C08K5/523C08K5/544C08L69/00C07F9/6574
CPCC07F9/65748C08K5/521C08K5/523C08K5/5477C08L69/00
Inventor 陈思王旭林世超朱峰马猛施燕琴
Owner ZHEJIANG UNIV OF TECH
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