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Expansible fire retardant containing fluorine-phosphorus-nitrogen oligomer and preparation method thereof

An intumescent flame retardant and oligomer technology, applied in the field of flame retardants, can solve the problems of large addition, poor stability, and high moisture absorption, and achieve improved water resistance, good thermal stability, and char formation rate high effect

Active Publication Date: 2010-11-24
来安县亨通橡塑制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The intumescent flame retardant is mainly composed of three parts: carbon source (char-forming agent), acid source (dehydrating agent) and gas source (foaming agent). Due to the complex ratio of the three components, it is difficult to control the three components. The proportion between the flame retardant and the polymer matrix in the process of the overall addition is large, the stability is poor, and it is prone to problems such as migration, precipitation or volatilization. At the same time, the thermal stability of the flame retardant is poor and the moisture absorption is large.

Method used

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  • Expansible fire retardant containing fluorine-phosphorus-nitrogen oligomer and preparation method thereof
  • Expansible fire retardant containing fluorine-phosphorus-nitrogen oligomer and preparation method thereof
  • Expansible fire retardant containing fluorine-phosphorus-nitrogen oligomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] a. In a nitrogen atmosphere, first dissolve pentaerythritol diphosphate diphosphoryl chloride in acetonitrile solvent, and massage pentaerythritol diphosphate diphosphoryl chloride and 2-trifluoromethyl-4-4-diaminodiphenyl ether according to the The molar ratio is 1: 1 mixing, and it is 65 ℃ of reactions at temperature for 9 hours, and wherein the consumption of acetonitrile is 2 times of the total mass of pentaerythritol diphosphate diphosphoryl chloride and diamine; Wherein pentaerythritol diphosphate diphosphoryl chloride is made of Obtained by reacting pentaerythritol and phosphorus oxychloride at a molar ratio of 1:7 at 80°C for 24 hours;

[0027] b. Filter the above reaction product, wash the obtained filter residue twice with deionized water, then wash twice with absolute ethanol, and dry in a vacuum oven at 80°C for 24 hours to obtain the fluorine-phosphorus-nitrogen oligomer Intumescent flame retardant, its structural formula is:

[0028]

[0029] Flame ret...

Embodiment 2

[0034] a. In a nitrogen atmosphere, first dissolve pentaerythritol diphosphate diphosphoryl chloride in acetonitrile solvent, and mix pentaerythritol diphosphate diphosphoryl chloride with 2,2-bis[4-(4-amino-2-trifluoromethane Base phenoxy) phenyl] propane mixed according to the molar ratio of 1: 1.5, at a temperature of 70 ° C for 8 hours, wherein the amount of acetonitrile is 3 times the total mass of pentaerythritol diphosphate diphosphoryl chloride and diamine ; Wherein pentaerythritol diphosphate diphosphoryl chloride is obtained by reacting pentaerythritol and phosphorus oxychloride according to a molar ratio of 1:3 at 105° C. for 16 hours;

[0035] b. Filter the above reaction product, wash the obtained filter residue twice with deionized water, then wash twice with absolute ethanol, and dry in a vacuum oven at 80°C for 24 hours to obtain the fluorine-phosphorus-nitrogen oligomer Intumescent flame retardant, its structural formula is:

[0036]

[0037] Flame retarda...

Embodiment 3

[0042]a. In a nitrogen atmosphere, first dissolve pentaerythritol diphosphate diphosphoryl chloride in acetonitrile solvent, and mix pentaerythritol diphosphate diphosphoryl chloride with 1,4-bis(4-amino-2-trifluoromethylphenoxy Base) benzene was mixed according to the molar ratio of 1:1.5, and reacted at a temperature of 75°C for 7 hours, wherein the amount of acetonitrile was 4 times the total mass of pentaerythritol diphosphate diphosphoryl chloride and diamine; wherein pentaerythritol diphosphate Diphosphoryl chloride is obtained by reacting pentaerythritol and phosphorus oxychloride at a molar ratio of 1:5 at 100°C for 20 hours;

[0043] b. Filter the above reaction product, wash the obtained filter residue twice with deionized water, then wash twice with absolute ethanol, and dry in a vacuum oven at 80°C for 24 hours to obtain the fluorine-phosphorus-nitrogen oligomer Intumescent flame retardant, its structural formula is:

[0044]

[0045] Flame retardant applicatio...

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Abstract

The invention relates to the technical field of fire retardants, particularly relating to an expansible fire retardant containing a fluorine-phosphorus-nitrogen oligomer and a preparation method thereof. The fire retardant is prepared by mixing pentaerythritoldiphosphatediphosphoryl chloride and diamine based on a molar ratio of 1:1-1.5 for reaction, filtering the obtained substance, washing and drying the filter residue. The method is simple and convenient. Meanwhile, the expansible fire retardant containing the fluorine-phosphorus-nitrogen oligomer prepared by the invention is an oligomer type molecule and has large molecular weight and good stability, and solves the problems of shift, precipitation or volatilization and the like which occur in processing and molding the fire retardants and polymer substrates; at the same time, the introduced functional fluorine element greatly improves the water resistance of the substrates; and the fire retardant integrates a carbon source, an acid source and a gas source into a whole, the charcoal yield is high, the carbon residue amount is about 58% at air atmosphere under the temperature of 800 DEG C, and the thermostability is favorable.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a fluorine-phosphorus-nitrogen oligomer expansion type flame retardant and a preparation method thereof. Background technique [0002] The intumescent flame retardant is a composite flame retardant with nitrogen, phosphorus, and carbon as the main components. Antimony oxide is not used as a synergist, and the system itself has a synergistic effect. The intumescent flame retardant is a solid-phase flame retardant mechanism. When burning, the smoke is small and the gas released is harmless; in addition, the charcoal layer generated by the intumescent flame retardant can absorb molten and ignited polymers to prevent droplets from spreading fire. [0003] The intumescent flame retardant is mainly composed of three parts: carbon source (char-forming agent), acid source (dehydrating agent) and gas source (foaming agent). Due to the complex ratio of the three components, it is ...

Claims

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Application Information

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IPC IPC(8): C08G79/04C08L23/12C08L85/02
Inventor 徐文总陆波殷建国胡源
Owner 来安县亨通橡塑制品有限公司
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