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Imidazolium ionic liquid flame retardant containing cage phosphate structure and preparation method thereof

A technology of imidazole ionic liquid and caged phosphate, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of unsatisfactory effect when used alone and achieve good application prospects , Reduce the negative impact, the effect of simple process operation

Active Publication Date: 2017-10-03
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this patent, the synthesized ionic liquid flame retardant needs to use a certain amount of halogen to achieve the corresponding effect. With the expansion of the application field of polymer materials, people are more interested in flame retardants and flame retardant materials. The requirements are getting higher and higher, and the use of halogenated flame retardants has been gradually restricted due to the release of a large amount of smoke and corrosive and toxic gases such as dioxin and benzofuran during the combustion process.
Moreover, the flame retardant reported in this patent needs to be compounded with ammonium polyphosphate, pentaerythritol and melamine to form an intumescent flame retardant and added to the material to exert a good flame retardant effect. The effect of using it alone is not ideal, which makes It has certain limitations in application

Method used

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  • Imidazolium ionic liquid flame retardant containing cage phosphate structure and preparation method thereof
  • Imidazolium ionic liquid flame retardant containing cage phosphate structure and preparation method thereof
  • Imidazolium ionic liquid flame retardant containing cage phosphate structure and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) In N 2 Under protection, add 0.5mol PEPA and 0.5mol acid binding agent triethylamine to dichloromethane successively, stir for 10min at room temperature and 25℃, and then add 0.5mol methylsulfonyl chloride dropwise. The dropping time is controlled for 1.5h. After the addition, the reaction was carried out at 25°C for 6 hours. After the reaction, the dichloromethane was distilled off, and the intermediate was obtained after washing and drying. The yield was 85%. The structure is as follows:

[0040]

[0041] 2) Dissolve the obtained 0.5mol intermediate in the solvent 1-methylimidazole, then add 0.5mol 1-methylimidazole, and 2 Under protection, the temperature was raised to 85℃ and the reaction was stirred for 48h. The solvent 1-methylimidazole was distilled off, the residue was washed 3-4 times with acetone, and dried to obtain an imidazole ionic liquid flame retardant with methanesulfonate anion. The yield was 76%. Its structural formula is as follows:

[0042]

[0043] ...

Embodiment 2

[0045] 1) In N 2 Under the protection, add 0.5mol PEPA and 0.6mol acid binding agent triethylamine to acetone successively, stir at room temperature 25℃ for 20min, then add 0.75mol p-toluenesulfonyl chloride dropwise, the dropping time is controlled for 3h, after the dropping The reaction was carried out at 25°C for 8 hours. After the reaction, the acetone was distilled off, and the intermediate was obtained after washing and drying. The yield was 88%. The structure is as follows:

[0046]

[0047] 2) Dissolve 0.5 mol of the obtained intermediate in 1-methylimidazole, then add 0.6 mol of 1-methylimidazole, and add in N 2 Under protection, the temperature was raised to 83℃ and the reaction was stirred for 58 hours. The solvent 1-methylimidazole was distilled off. The residue was washed 3-4 times with acetone and dried to obtain an imidazole ionic liquid flame retardant with p-toluenesulfonate anion. The yield was 72%. Its structural formula is as follows:

[0048]

[0049] 3) The f...

Embodiment 3

[0051] 1) In N 2 Under protection, add 0.5mol PEPA and 0.5mol acid binding agent triethylamine to dichloromethane successively, stir at room temperature 25℃ for 10min, then add 0.52mol 1-butylsulfonyl chloride dropwise, and the dropping time is controlled for 1.5h. After the dropwise addition, the reaction was carried out at 26°C for 6 hours. After the reaction, the dichloromethane was distilled off, and the white intermediate was obtained after washing and drying. The yield was 78%, and the structure was as follows:

[0052]

[0053] 2) Dissolve the obtained 0.5mol intermediate in the solvent 1-methylimidazole, then add 0.5mol 1-methylimidazole, and 2 Under protection, the temperature was raised to 80℃ and the reaction was stirred for 50h. The solvent 1-methylimidazole was distilled off. The residue was washed 3-4 times with acetone and dried to obtain an imidazole ionic liquid flame retardant with butyl sulfonate anion. The yield was 75%. Its structural formula is as follows:

...

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Abstract

The general structural formula of an imidazolium liquid flame-retardant agent containing a caged phosphate structure disclosed in the invention is shown in the description, wherein X is an alkyl group, a phenyl group or a phosphate group of C=1-20, Y is an alkyl group, a phenyl group or a tolyl group of C=1-20, and the limit oxygen index of polycarbonate after the flame-retardant agent is used for polycarbonate can be increased by 4.5-6 units compared with pure polycarbonate.The invention further discloses a preparation method of the flame-retardant agent.The imidazolium liquid flame-retardant agent containing the caged phosphate structure does not contain halogen, is high in decomposition temperature, can be independently used, and is little in addition amount and good in flame-retardant effect.Oxidation decomposition occurring in the processing process of the flame-retardant agent can be effectively avoided, and adverse effects on mechanical properties of a material can be reduced.The preparation method is easy to operate, cost is low, a product obtained through reaction is high in yield, the reaction raw material substituted imidazole can be recycled and reused, and environmental protection and energy conservation are achieved.

Description

Technical field [0001] The invention belongs to an imidazole ionic liquid flame retardant and a preparation method thereof, and specifically relates to a preparation method of an imidazole ionic liquid flame retardant containing a cage-like phosphate structure. Background technique [0002] As a kind of environmentally friendly compound, ionic liquid has been developed rapidly and widely used in recent years due to its unique and excellent physical and chemical properties. For example, it has almost no vapor pressure, is not easy to volatilize, has a wide range of liquid range, and has good thermal stability. The characteristics of large heat capacity, wide electrochemical window, non-flammability, etc., are called "green solvents" that can replace traditional organic solvents. More importantly, the molecules of ionic liquids are highly designable. The physical and chemical properties of ionic liquids can be adjusted by adjusting the alkyl chain length of cations, changing the ty...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/521C08L69/00
CPCC07F9/65748C08K5/521C08L2201/02C08L69/00
Inventor 汪秀丽何秋霞史月全唐亮夏灵童王玉忠
Owner SICHUAN UNIV
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