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Hyperbranched ionic liquid as well as preparation method and application

A technology of ionic liquids and hyperbranched polymers, applied in the field of hyperbranched polymers, can solve the problems of high water-resistant glass transition temperature, low curing volume shrinkage, and high curing temperature, so as to improve reactivity and compatibility, reduce The effects of curing temperature and easy availability of raw materials

Inactive Publication Date: 2018-05-18
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Benzoxazine resin is a new type of high-performance thermosetting resin, which has the characteristics of low curing volume shrinkage, good water resistance and high glass transition temperature. It is widely used in high temperature resistant electrical insulation materials, halogen-free flame-retardant printed circuit boards And electronic packaging materials, ablation-resistant materials and other fields, but benzoxazine resin still has disadvantages such as high curing temperature and high brittleness

Method used

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  • Hyperbranched ionic liquid as well as preparation method and application
  • Hyperbranched ionic liquid as well as preparation method and application
  • Hyperbranched ionic liquid as well as preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (a) Mix 13.42g of trimethylolpropane, 40.24g of dimethylolpropionic acid and 0.27g of p-toluenesulfonic acid, and stir and react at 170°C for 6h to obtain the first-generation hydroxyl-terminated hyperbranched polyester HBPM- 1. Each mole of HBPM-1 contains 6 moles of hydroxyl groups, and the number average molecular weight is 500 g / mol.

[0034] (b) Mix 48.26g HBPM-1, 76.42g mercaptopropionic acid MPA, 120mL dioxane and 2.49g p-toluenesulfonic acid, stir and react at 80°C for 12h, then wash with 150ml saturated aqueous sodium bicarbonate solution three times To neutrality, the organic layer was dried with anhydrous magnesium sulfate, filtered, and the organic solvent was distilled off under reduced pressure to obtain the first-generation mercapto-terminated hyperbranched polyester THBPM-1, with a number average molecular weight of 1100 g / mol.

[0035] (c) After mixing 50.57g THBPM-1, 80.44g 1-allyl-3-methylimidazolium hexafluorophosphate AMIMPF6 and 2.62g photoinitiato...

Embodiment 2

[0037] (a) Mix 13.42g trimethylolpropane, 120.72g dimethylolpropionic acid and 0.67g p-toluenesulfonic acid evenly, and carry out stirring reaction at 180°C for 5h to obtain the second generation hydroxyl-terminated hyperbranched polyester HBPM- 2. Each mole of HBPM-2 contains 12 moles of hydroxyl groups, and the number average molecular weight is 1100 g / mol.

[0038] (b) Mix 117.93g HBPM-2, 152.84g mercaptopropionic acid MPA, 250mL dioxane and 5.42g p-toluenesulfonic acid, stir and react at 90°C for 10h, then wash with 150ml saturated aqueous sodium bicarbonate solution three times To neutrality, the organic layer was dried with anhydrous magnesium sulfate, filtered, and the organic solvent was distilled off under reduced pressure to obtain the second-generation mercapto-terminated hyperbranched polyester THBPM-2, with a number average molecular weight of 2200 g / mol.

[0039](c) After mixing 55.93g THBPM-2, 80.44g 1-allyl-3-methylimidazolium hexafluorophosphate AMIMPF6 and 2....

Embodiment 3

[0041] (a) Mix 13.42g trimethylolpropane, 120.72g dimethylol propionic acid and 0.67g p-toluenesulfonic acid evenly, and carry out stirring reaction at 190°C for 4h to obtain the second generation hydroxyl-terminated hyperbranched polyester HBPM- 2. Each mole of HBPM-2 contains 12 moles of hydroxyl groups, and the number average molecular weight is 1100 g / mol.

[0042] (b) Mix 117.93g HBPM-2, 152.84g mercaptopropionic acid MPA, 250mL dioxane and 5.42g p-toluenesulfonic acid, stir and react at 100°C for 8h, then wash with 150ml saturated aqueous sodium bicarbonate solution three times To neutrality, the organic layer was dried with anhydrous magnesium sulfate, filtered, and the organic solvent was distilled off under reduced pressure to obtain the second-generation mercapto-terminated hyperbranched polyester THBPM-2, with a number average molecular weight of 2200 g / mol.

[0043] (c) After mixing 55.93g THBPM-2, 93.07g 1-allyl-3-butylimidazole hexafluorophosphate ABIMPF6 and 2.9...

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Abstract

The invention discloses hyperbranched ionic liquid. The hyperbranched ionic liquid is obtained by carrying out thiol-olefin click reaction on a mercapto-terminated hyperbranched polymer and allyl ionic liquid, wherein the mercapto-terminated hyperbranched polymer is obtained by taking a hydroxy-terminated hyperbranched polymer and mercaptopropanoic acid or mercaptoacetic acid to react. The invention further discloses a preparation method and application of the hyperbranched ionic liquid. According to the hyperbranched ionic liquid disclosed by the invention, the hyperbranched ionic liquid is prepared through conventional reaction; a synthesis technology is simple and raw materials are easy to obtain, so that the hyperbranched ionic liquid is suitable for industrial production. Compared with a traditional modifier with a linear structure, the prepared hyperbranched ionic liquid has a good enhancing and toughening effect on benzoxazine resin; an active end group can be used for improvingthe reaction activity and compatibility of the benzoxazine resin, so that the curing temperature is reduced; the hyperbranched ionic liquid is hopefully used for electronic and electrical, aeronauticand astronautic fields and the like.

Description

technical field [0001] The invention relates to the technical field of hyperbranched polymers, in particular to a hyperbranched ionic liquid and its preparation method and application. Background technique [0002] Hyperbranched polymers have a large number of cavity structures and a large number of end groups, so they have high reactivity. Due to the less entanglement between molecules of hyperbranched polymers, it is not easy to crystallize, and has good hydrodynamic properties, unique viscosity behavior, and easy film formation, making it a broad application prospect in many fields. Designing ionic liquids as hyperbranched ionic liquids can not only improve the performance of ionic liquids, but also expand the application fields of hyperbranched polymers, which has important theory and application. [0003] Benzoxazine resin is a new type of high-performance thermosetting resin, which has the characteristics of low curing volume shrinkage, good water resistance and high ...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08L61/34C08L67/04
CPCC08G63/912C08L61/34C08L67/04
Inventor 张俊珩张道洪张爱清
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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