Preparation method of aqueous polyurethane/fluorinated phosphazene nano fiber composite material

A fluorine-containing polyphosphazene and water-based polyurethane technology is applied in the field of nanomaterial preparation, which can solve the problems of nanoparticle structure and morphology damage, composite material comprehensive performance decline, inconvenient production process, etc., and achieves excellent thermal stability and improved thermal stability. The effect of stable performance and simple preparation method

Inactive Publication Date: 2017-08-18
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of physical filling modification, the agglomeration of nanoparticles is prone to occur, which leads to uneven dispersion of fillers and poor interfacial compatibility with the matrix resin, which leads to the disadvantages of a significant decline in the comprehensive performance of composite materials.
In addition, since the surface of most inorganic nanoparticles has no active sites, surface treatment must be carried out before filling modification, and this process requires complex multi-step chemical reactions, which brings inconvenience to the production process
The complex modification process will also damage the structure and morphology of nanoparticles, making them lose some of their functionality

Method used

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  • Preparation method of aqueous polyurethane/fluorinated phosphazene nano fiber composite material
  • Preparation method of aqueous polyurethane/fluorinated phosphazene nano fiber composite material
  • Preparation method of aqueous polyurethane/fluorinated phosphazene nano fiber composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1: Under magnetic stirring at 1200 r / min, add 0.1 g of hexachlorocyclotriphosphazene and 0.28 g of 4,4'-(hexafluoroisopropylidene ) bisphenol, slowly added 0.24 mL triethylamine, reacted at room temperature for 12 hours, washed three times with deionized water and ethanol, centrifuged at 4000 r / min, and dried in vacuum at 40°C for 24 hours to obtain fluorine-containing polyphosphazene nanoparticles Fiber, 80% yield.

[0027] Step 2: Put 30 g of PPG-2000 in a three-necked flask, and fill it with nitrogen (without fiber). Stir continuously in an oil bath at 100° C. for 0.5 hours, add 11.67 g of IPDI and 5 drops of dibutyltin dilaurate catalyst, and react at 95° C. for 2 hours. 2.01 g of DMPA, which had been vacuum-dried in advance, was added into the three-necked flask, and the reaction was continued for 3 hours. Lower the temperature of the system to 30°C, add TEA to neutralize to pH 7, and stir at constant temperature for 0.5 h to obtain a PU prepolymer. The pre...

Embodiment 2

[0029] Step 1: Under magnetic stirring at 1200 r / min, add 0.2 g of hexachlorocyclotriphosphazene and 0.38 g of 4,4'-(hexafluoroisopropylidene) into a single-necked flask containing 100 mL of toluene acetone solution Bisphenol, slowly add 0.48 mL triethylamine, react at room temperature for 12 hours, wash with deionized water and ethanol three times respectively, centrifuge at 4000 r / min, and vacuum dry at 40°C for 24 hours to obtain fluorine-containing polyphosphazene nanofibers , and the yield was 81%.

[0030] Step 2: Put 30 g of PPG-2000 in a three-necked flask, add 0.2552 g (0.5 wt.%) fluorine-containing polyphosphazene fiber at the same time, and fill it with nitrogen for protection. Stir continuously in an oil bath at 100° C. for 0.5 hours, add 11.67 g of IPDI and 5 drops of dibutyltin dilaurate catalyst, and react at 95° C. for 2 hours. 2.01 g of DMPA, which had been vacuum-dried in advance, was added into the three-necked flask, and the reaction was continued for 3 ho...

Embodiment 3

[0032]Step 1: Under magnetic stirring at 1200 r / min, add 0.4 g of hexachlorocyclotriphosphazene and 1.0 g of 4,4'-(hexafluoroisopropylidene ) bisphenol, slowly add 0.96mL triethylamine, react at room temperature for 12 hours, wash with deionized water and ethanol three times respectively, centrifuge at 4000 r / min, and vacuum dry at 40°C for 24 hours to obtain fluorine-containing polyphosphazene Nanofibers with a yield of 83%.

[0033] Step 2: Put 30 g of PPG-2000 in a three-necked flask, add 0.5104 g (1.0 wt.%) fluorine-containing polyphosphazene fiber at the same time, and fill it with nitrogen for protection. Stir continuously in an oil bath at 100° C. for 0.5 hours, add 11.67 g of IPDI and 5 drops of dibutyltin dilaurate catalyst, and react at 95° C. for 2 hours. 2.01 g of DMPA, which had been vacuum-dried in advance, was added into the three-necked flask, and the reaction was continued for 3 hours. Lower the temperature of the system to 30°C, add TEA to neutralize to pH ...

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Abstract

The invention discloses a preparation method of an aqueous polyurethane / fluorinated phosphazene nano fiber composite material. The method comprises the following steps: dissolving hexachlorocyclotriphosphazene and 4,4'-(hexafluoro isopropyl fork) bisphenol into a toluene / acetone composite solution; dropwise adding triethylamine and carrying out nucleophilic substitution reaction under a magnetic power stirring condition, and carrying out post-treatment to obtain fluorinated phosphazene nano fibers; adding the nano fibers into polypropylene glycol; then adding isophorone diisocyanate, a catalyst and 2,2-dimethylolpropionic acid until the reaction is completed; reducing the temperature and adding triethylamine to be neutralized; dispersing into the deionized water to obtain an aqueous polyurethane solution; and casting the aqueous polyurethane solution into an extensible sample strip mould to be naturally solidified to obtain the aqueous polyurethane / fluorinated phosphazene nano fiber composite material. According to the preparation method disclosed by the invention, by adopting a chemical in-situ polymerization method, the reaction is added into an aqueous polyurethane basal body, and the successfully obtained aqueous polyurethane composite material has excellent heat stability, extension performance and friction and abrasion performance.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, in particular to a method for preparing a waterborne polyurethane / polyphosphazene nanofiber composite material. Background technique [0002] Waterborne polyurethane (WPU) is a type of polymer that can be stably dissolved or dispersed in water after introducing hydrophilic groups into its molecular chain. WPU can be synthesized in two stages. The first is pre-stepwise polymerization, that is, the gradual polymerization of oligomer diols, diisocyanates, hydrophilic monomers and chain extenders into waterborne polyurethane prepolymers with relatively large molecular weights; secondly, neutralization and post-prepolymerization dispersion in water. The water-based polyurethane synthesized by this method has low organic volatiles and is relatively environmentally friendly. Through research in recent years, it has also been widely used, such as adhesives, surface treatment agents, fa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L75/08C08L85/02C08G18/66C08G18/48C08G18/34C08G79/025D01F6/78
CPCC08L75/08C08G18/348C08G18/4825C08G18/6692C08G79/025C08L2201/08C08L2205/16D01F6/78C08L85/02
Inventor 赵正平胡佳捷周泽平钟明强
Owner ZHEJIANG UNIV OF TECH
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