Preparation method of waterborne flame-retardant self-repairing polyurethane based on modified graphene

A self-healing and polyurethane technology, which is applied in the fields of leather finishing and fabric finishing, can solve the problems of affecting self-healing efficiency, modified graphene oxide cannot participate in self-healing, and mechanical properties cannot be guaranteed.

Active Publication Date: 2021-04-30
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method only uses a flame retardant to modify graphene oxide, which has a limited improvement in the flame retardant function of the material. Therefore, introducing multiple flame retardant components on graphene oxide to synergistically flame retardant has a better flame retardant effect on the material. promotion
[0010] For example, Chinese patent (CN109735094A) discloses a preparation method of nitrogen-phosphorus-silicon-modified graphene/self-healing polyurethane flame-retardant composite material, which is composed of polyethyleneimine, 9,10-dihydro-9-oxa-10- Phosphaphenanthrene-10-oxide and isocyanatosilane covalently modify graphene oxide and in-situ polymerize it with self-healing polyurethane containing diselenium, and obtain a good flame retardant effect, but the reaction system is The solvent system has not been water-based, and it is difficult to meet the growing environmental protection requirements
At the same time, the modified graphene oxide synthesized by this method is not grafted with polyurethane chains with self-healing function, so that the modified graphene oxide cannot participate in self-healing, and the content of self-healing components is reduced, which obviously affects the self-healing effic...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: 5 g of graphene oxide was prepared into a graphene oxide aqueous dispersion (1 mg / mL) and placed in a single-necked flask containing a magnetic stirrer, and 0.231 g of hexaaminocyclotriphosphazene and 0.01 g of 4-dimethylamino Pyridine, react at room temperature under nitrogen protection for 12 hours, centrifuge and dry to obtain nitrogen-phosphorus-modified graphene oxide; disperse 5.232g nitrogen-phosphorus-modified graphene oxide in 50g methyl ethyl ketone, add 0.205g isocyanate propyltrimethoxysilane, Under the protection of nitrogen, react at 70°C for 24 hours, ultrasonically pulverize with an ultrasonic cell pulverizer at room temperature for 6 hours, and centrifugally dry to obtain nitrogen-phosphorus-silicon-modified nano-graphene oxide with a particle size of less than 100 nm; After drying at ℃ for 2 hours, take it out and place it in a desiccator to fully cool; mix 5.437g of nitrogen-phosphorus-silicon-modified nano-graphene oxide, 1g of polytetrahyd...

Embodiment 2

[0043] Example 2: 5 g of graphene oxide was prepared into a graphene oxide aqueous dispersion (1 mg / mL) and placed in a single-necked flask containing a magnetic stirrer, and 0.231 g of hexaaminocyclotriphosphazene and 0.01 g of 4-dimethylamino Pyridine, react at room temperature for 12 hours under the protection of nitrogen, centrifuge and dry to obtain nitrogen-phosphorus-modified graphene oxide; disperse 5.232g nitrogen-phosphorus-modified graphene oxide in 50g methyl ethyl ketone, add 0.247g isocyanate propyltriethoxysilane , reacted at 70°C under nitrogen protection for 24h, ultrasonically pulverized with an ultrasonic cell pulverizer at room temperature for 6h, and centrifuged and dried to obtain nitrogen-phosphorus-silicon-modified nano-graphene oxide with a particle size of less than 100nm; After drying at 110°C for 2 hours, take it out and place it in a desiccator for sufficient cooling; mix 5.479g of nitrogen-phosphorus silicon-modified nano-graphene oxide, 1g of poly...

Embodiment 3

[0044]Example 3: 5 g of graphene oxide was prepared into a graphene oxide aqueous dispersion (1 mg / mL) and placed in a single-necked flask containing a magnetic stirrer, and 0.231 g of hexaaminocyclotriphosphazene and 0.01 g of 4-dimethylamino Pyridine, react at room temperature under nitrogen protection for 12 hours, centrifuge and dry to obtain nitrogen-phosphorus-modified graphene oxide; disperse 5.232g nitrogen-phosphorus-modified graphene oxide in 50g methyl ethyl ketone, add 0.205g isocyanate propyltrimethoxysilane, Under the protection of nitrogen, react at 70°C for 24 hours, ultrasonically pulverize with an ultrasonic cell pulverizer at room temperature for 6 hours, and centrifugally dry to obtain nitrogen-phosphorus-silicon-modified nano-graphene oxide with a particle size of less than 100 nm; After drying at ℃ for 2 hours, take it out and place it in a desiccator to fully cool; mix 5.437g of nitrogen-phosphorus-silicon-modified nano-graphene oxide, 1g of polytetrahydr...

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Abstract

The invention discloses a preparation method of waterborne flame-retardant self-repairing polyurethane based on modified graphene. The method comprises the following steps: firstly, ultrasonically crushing amino cyclotriphosphazene and isocyanate silane covalently modified graphene oxide, then reacting with macromolecular diol, a hydrophilic chain extender and diisocyanate, terminating with diselenide diol, neutralizing, emulsifying, and adding waterborne self-repairing polyurethane containing diselenide bonds so as to obtain the waterborne flame-retardant self-repairing polyurethane emulsion. According to the invention, by reducing the size of graphene oxide and modifying a waterborne polyurethane chain, the water dispersion stability and the dispersion uniformity and compatibility of the graphene oxide in the membrane are improved, so that the mechanical strength of the membrane is improved; due to nitrogen phosphorus silicon modification, the flame retardant property is further improved; the material is endowed with a good room-temperature illumination self-repairing function through double selenium bonds; and the method provided by the invention is environment-friendly, and the prepared material has high mechanical property and excellent flame-retardant self-repairing function, and can be applied to various fields of leather finishing, fabric finishing and the like.

Description

technical field [0001] The invention relates to a preparation method of water-based flame-retardant self-healing polyurethane, in particular to the preparation of water-based flame-retardant self-healing polyurethane based on nitrogen-phosphorus-silicon-modified nano-graphene oxide, and belongs to the fields of leather finishing and fabric finishing. Background technique [0002] Polyurethane is a polymer material with light weight, good mechanical properties, chemical stability, corrosion resistance, easy processing, and high resilience. Therefore, it has been widely concerned by researchers since it was developed by Bayer in 1937. After more than 80 years of development, it has been widely used in the fields of textile, leather, construction, automobile, aerospace and transportation. However, most polyurethanes are extremely flammable, which is determined by their chemical structure and elemental composition, which greatly restricts their practical applications in many fie...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/48C08G18/32C08G18/34C08K9/06C08K9/04C08K3/04D06M15/568C09D175/08C14C11/00
CPCC08G18/3234C08G18/348C08G18/3897C08G18/4854C08G18/6666C08G18/6692C08K9/04C08K9/06C08K2201/011C09D175/08C14C11/006C08K3/042D06M15/568D06M2200/30
Inventor 金勇商翔杜卫宁
Owner SICHUAN UNIV
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