Phosphorus-containing fluorine-containing synergic flame-retardant compound and preparation method thereof

A technology for synergistic flame retardant and compound, which is applied in the field of phosphorus-containing and fluorine-containing synergistic flame retardant compounds and their preparation to achieve the effects of reducing surface energy, mild reaction conditions and high conversion rate

Inactive Publication Date: 2016-07-06
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the shortcomings of existing flame retardant materials, and provide a phosphorus-containing and fluorine-containing synergistic flame retardant compound and its preparation method

Method used

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  • Phosphorus-containing fluorine-containing synergic flame-retardant compound and preparation method thereof
  • Phosphorus-containing fluorine-containing synergic flame-retardant compound and preparation method thereof
  • Phosphorus-containing fluorine-containing synergic flame-retardant compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1, the synthesis of the intermediate containing carbon-nitrogen double bond

[0030] First, 2g (3.86mmol) of 2,2-bis[4-(4-aminophenoxy)phenyl] 1,1,1,3,3,3-hexafluoropropane and 1.86g (7.68mmol) Add 3,5-bis(trifluoromethyl)benzaldehyde into a 100mL single-necked flask, dissolve it with 20mL methanol, stir and react at 55°C for 8h, spin the solvent to dryness with a rotary evaporator, and obtain a light yellow powder after vacuum drying solid, which is an intermediate containing a carbon-nitrogen double bond.

[0031] The characterization of the carbon-nitrogen-containing double bond intermediate is as follows figure 1 As shown, the chemical shifts from 8.8ppm to 9.0ppm are the characteristic peaks of C-H on the carbon-nitrogen double bond, and the six peaks from 7.0ppm to 8.7ppm are the characteristic peaks of C-H on the benzene ring.

[0032] Step 2, synthesis of phosphorus-containing and fluorine-containing synergistic flame-retardant compounds:

[0033] Add 2g...

Embodiment 2

[0036] Step 1, the synthesis of the intermediate containing carbon-nitrogen double bond:

[0037] First, 2g (3.86mmol) of 2,2-bis[4-(4-aminophenoxy)phenyl] 1,1,1,3,3,3-hexafluoropropane and 1.86g (7.68mmol) Add 3,5-bis(trifluoromethyl)benzaldehyde into a 100mL single-necked flask, dissolve in 20mL methanol, stir and react at 65°C for 6h, spin the solvent to dryness with a rotary evaporator, and obtain a light yellow powder after vacuum drying solid, which is an intermediate containing a carbon-nitrogen double bond.

[0038] Step 2, synthesis of phosphorus-containing and fluorine-containing synergistic flame-retardant compounds:

[0039]Add 2g (2.1mmol) of the carbon-nitrogen double bond intermediate obtained in step 1 and 0.91g (4.2mmol) of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into a 100mL single port In the flask, dissolve with 20mL N,N-dimethylformamide, react at 45°C for 8 hours, precipitate with methanol, wash repeatedly three times, and obtain a light yell...

Embodiment 3

[0041] Step 1, the synthesis of the intermediate containing carbon-nitrogen double bond:

[0042] First, 2g (10.08mmol) of 4,4'-diaminodiphenylmethane and 4.88g (20.16mol) of 3,5-bis(trifluoromethyl)benzaldehyde were added to a 100mL single-necked flask, and 20mL of methanol Dissolve, stir and react at 55° C. for 8 h, spin the solvent to dryness with a rotary evaporator, and obtain a light yellow powdery solid after vacuum drying, which is an intermediate containing a carbon-nitrogen double bond.

[0043] Step 2, synthesis of phosphorus-containing and fluorine-containing synergistic flame-retardant compounds:

[0044] Add 2g (3.10mmol) of the carbon-nitrogen double bond intermediate obtained in step 1 and 1.34g (6.19mmol) of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into a 100mL single port In the flask, dissolve with 20mL N,N-dimethylformamide, react at 55°C for 10h, precipitate with methanol, wash repeatedly three times, and obtain a light yellow powdery solid afte...

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Abstract

The invention provides a phosphorus-containing fluorine-containing synergic flame-retardant compound and a preparation method thereof, relating to flame-retardant compounds. The preparation method comprises the following steps: carrying out reaction on a diamido compound and 5-bis(trifluoromethyl)benzaldehyde in a first solvent, carrying out rotary evaporation, and drying to obtain an intermediate containing carbon-nitrogen double bond; and carrying out reaction on the intermediate containing carbon-nitrogen double bond and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a second solvent, precipitating the product with a precipitant, washing with the precipitant, and drying to obtain the phosphorus-containing fluorine-containing synergic flame-retardant compound. The compound simultaneously comprises the flame-retardant elements phosphorus and fluorine, and the phosphorus and fluorine have the synergic flame-retardant actions; and thus, the compound can be used as a flame retardant and has favorable flame-retardant effect. The introduced fluorine element can enhance the heat stability and chemical stability, lower the surface energy of the material and lower the dielectric constant and hydroscopic property of the material, thereby satisfying the required properties of the electronic packaging material. The compound contains two active groups, thereby being beneficial to enhancing the compatibility with the high-polymer material, improving the loss of the flame retardant and enhancing the flame retardancy.

Description

technical field [0001] The invention relates to a flame-retardant compound, in particular to a phosphorus-containing and fluorine-containing synergistic flame-retardant compound and a preparation method thereof. Background technique [0002] In recent years, with the development of electronic packaging technology, the performance requirements of epoxy resin are getting higher and higher. How to improve the thermal stability, mechanical properties and flame retardancy of epoxy resin while reducing its dielectric constant and moisture absorption Sex and expansion coefficient are problems to be solved urgently. Among them, the use of multi-element synergistic flame retardants to modify epoxy resins has become a promising direction for improving the performance of epoxy resins. [0003] GuL et al. (GuL, ChenG, YaoY.Twonovelphosphorus–nitrogen-containinghalogen-freeflameretardantsofhighperformanceforpoxyresin[J].PolymerDegradationandStability,2014,108:68-75.)Using 4,4'-diaminodi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/6574C07F9/657172
Inventor 戴李宗陈婷刘诚陈国荣袁丛辉陈显明曾碧榕许一婷罗伟昂
Owner XIAMEN UNIV
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