Imidazole sulfonate ionic liquid flame retardant containing DOPO and preparation method and application of imidazole sulfonate ionic liquid flame retardant

A technology of imidazole sulfonate and ionic liquid, which is applied in the field of flame retardancy, can solve the problems such as the decline in the mechanical properties of flame-retardant epoxy and poor compatibility, and achieve the effects of excellent thermal stability, wide source of raw materials, and avoiding pollution

Active Publication Date: 2018-02-02
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its large molecular weight and the poor compatibility between the compound of the triazine structure and epoxy, the mechanical properties of flame-retardant epoxy are significantly reduced.

Method used

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  • Imidazole sulfonate ionic liquid flame retardant containing DOPO and preparation method and application of imidazole sulfonate ionic liquid flame retardant
  • Imidazole sulfonate ionic liquid flame retardant containing DOPO and preparation method and application of imidazole sulfonate ionic liquid flame retardant
  • Imidazole sulfonate ionic liquid flame retardant containing DOPO and preparation method and application of imidazole sulfonate ionic liquid flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1) in N 2Under protection, add 1mol DOPO into 500ml solvent xylene, raise the temperature to 90°C, and mechanically stir for 30 minutes. After DOPO is completely dissolved in xylene, continue stirring for 10 minutes, and then slowly add 1mol~2mol of paraformaldehyde to maintain at React at 80°C for 5h to 8h. After the reaction, filter with suction and wash with deionized water for 3 to 5 times. A clean white sandy solid was obtained, irradiated by an infrared lamp for 4-6 hours, and then dried in a vacuum oven at 80° C. for 10 hours, with a yield of 96%. It was named DOPO-OH, and its structure was as follows:

[0043]

[0044] 2) in N 2 Under protection, dissolve 0.5mol DOPO-OH in 200ml dichloromethane, add 0.5mol triethylamine, stir mechanically at a rate of 400r / min for 10min, then slowly add 0.5mol methanesulfonyl chloride dropwise with a dropping funnel, drop The addition time was controlled within 1 hour, and after the dropwise addition, the reaction was carr...

Embodiment 2

[0050] 1) in N 2 Under protection, add 1mol DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) into 500ml solvent xylene, heat up to 90°C, stir mechanically for 30min, and wait until DOPO is completely Dissolve in toluene, continue to stir for 10 minutes, then slowly add 1 mol of paraformaldehyde, and maintain the reaction at 80°C for 5h to 8h. After the reaction, filter with suction and wash with ethanol for 3 to 5 times. A clean white sandy solid was obtained, which was dried under infrared light for 4-6 hours, and then dried in a vacuum oven at 80°C for 10 hours, with a yield of 96%. It was named DOPO-OH, and its structure was as follows:

[0051]

[0052] 2) in N 2 Under protection, dissolve 0.5mol DOPO-OH in 200ml acetonitrile, add 0.5mol triethylamine, stir mechanically at a rate of 400r / min for 10min, then slowly add 0.5mol p-toluenesulfonate dissolved in acetonitrile dropwise with a dropping funnel Acyl chloride, the dropwise addition time is controlled wi...

Embodiment 3

[0058] 1) in N 2 Under protection, add 1mol DOPO to 500ml solvent xylene, raise the temperature to 90°C, and stir mechanically for 30min. After DOPO is completely dissolved in xylene, continue stirring for 10min, then slowly add 1mol of paraformaldehyde, and maintain at 80°C Under the conditions of reaction 5h ~ 8h. After the reaction, filter with suction and wash with deionized water for 3 to 5 times to obtain a clean white sandy solid. Dry it with an infrared lamp for 4 to 6 hours, and then dry it in a vacuum oven at 80°C for 10 hours. The yield is 96%. It is named DOPO-OH. The structure is as follows:

[0059]

[0060] 2) in N 2 Under the condition of protective gas, dissolve 0.5mol DOPO-OH in 200ml ethanol, add 0.5mol pyridine, stir mechanically at a rate of 400r / min for 10min, then slowly add 0.5mol propylsulfonyl chloride dropwise with a dropping funnel, drop Adding time was controlled within 1 hour, and after the dropwise addition, the reaction was carried out at ...

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Abstract

The invention provides an imidazole sulfonate ionic liquid flame retardant containing a DOPO structure. The chemical structure of the flame retardant is as shown in formula , wherein X is alkyl, phenyl or DOPO group; Y is alkyl, vinyl, phenyl or p-methylphenyl. The invention further provides a preparation method of the flame retardant and application of the flame retardant in the preparation offlame-retardant materials. The ionic liquid flame retardant is simple in preparation method, free of halogen, wide in raw material source, low in cost, excellent in flame retardance to epoxy resin, low in adding amount, good in compatibility with the epoxy resin, low in influence on the mechanical performance of the epoxy resin, and the like.

Description

technical field [0001] The invention belongs to the technical field of flame retardancy, and in particular relates to an imidazole sulfonate ionic liquid flame retardant containing a DOPO structure and a preparation method and application thereof. Background technique [0002] As a new environment-friendly compound in the 21st century, ionic liquid has unique physical and chemical properties, such as good thermal stability, almost no vapor pressure, non-volatile, wide liquid range and non-flammability, etc., and is known as a substitute for traditional solvents. "Green Solvent". Ionic liquids can also adjust their physical and chemical properties by adjusting the types or structures of anions and cations to meet specific needs. [0003] At present, ionic liquids have been widely studied in organic synthesis, separation catalysis, electrochemistry, analytical chemistry and nanoscience, and they are used as functional plasticizers, antistatic agents, dispersants and flame ret...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C08L63/00C07F9/6574
CPCC07F9/657172C08K5/5313C08L2201/02C08L2201/22C08L63/00
Inventor 汪秀丽史月全李英奇贾蕴婉李德福赵禧王玉忠
Owner SICHUAN UNIV
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