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Preparation method of single-layer graphene oxide modified waterborne polyurethane composite material

A water-based polyurethane and graphene modification technology is applied in the field of preparation of single-layer graphene oxide modified water-based polyurethane composite materials, which can solve the problems of thick GO layers, difficulty in exerting graphene oxide properties, and easy agglomeration. The effect of mechanical advantage

Active Publication Date: 2015-12-23
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Graphene oxide (GO), as a graphene derivative, has oxygen-containing groups on its surface so that it can be well dispersed in water, but the GO layer prepared in the laboratory by the general method is thick, unstable, and easy to agglomerate , can not be well dispersed in the polymer, so it is difficult to exert the superior performance of graphene oxide

Method used

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  • Preparation method of single-layer graphene oxide modified waterborne polyurethane composite material
  • Preparation method of single-layer graphene oxide modified waterborne polyurethane composite material

Examples

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Embodiment 1

[0027] (1) Preparation of single-layer graphene oxide: using a new type of iron-based strengthening agent, potassium ferrate, to oxidize and exfoliate flake graphite. Take flake graphite with a particle size of 40 μm and 98% concentrated sulfuric acid and stir, mix and infiltrate at -10°C for 0.5h , Potassium ferrate and periodic acid were added, and then the reaction solution was raised to 0° C. for 1 h. After the reaction, the reaction solution was centrifuged at 4000r / min to discard the strong acid. Slowly pour the sediment at the bottom into deionized water at 2°C to dilute, let it stand still for 0.5h, wash the sediment repeatedly with 1mol / L dilute hydrochloric acid and deionized water, wash each 15 times in turn, and centrifuge until the centrifuged supernatant The pH value was close to 7, and the final product was freeze-dried at -40°C for 48 hours to obtain a single-layer graphene oxide. During the reaction, the ratio of strong acid to graphite is 10mL: 1g, and the r...

Embodiment 2

[0034] (1) Preparation of single-layer graphene oxide: using a new type of iron-based strong oxidant, potassium ferrate, to oxidize and exfoliate flake graphite, take flake graphite with a particle size of 10 μm and 98% concentrated sulfuric acid and stir, mix and infiltrate at -10°C for 0.5h , Potassium ferrate and periodic acid were added, and then the reaction solution was raised to 0° C. for 1 h. After the reaction, the reaction solution was centrifuged at 4000r / min to discard the strong acid. Slowly pour the sediment at the bottom into deionized water at 5°C to dilute, let stand for 0.5h, wash the sediment repeatedly with 1mol / L dilute hydrochloric acid and deionized water, wash each 15 times in turn, and centrifuge until the centrifuged supernatant The pH value was close to 7, and the final product-50 was freeze-dried for 48 h to obtain a single-layer graphene oxide. During the reaction, the ratio of strong acid to graphite is 50mL: 1g, and the ratio of potassium ferrat...

Embodiment 3

[0039] (1) Preparation of single-layer graphene oxide: using a new type of iron-based strong oxidant, potassium ferrate, to oxidize and exfoliate flake graphite, take flake graphite with a particle size of 40 μm and 98% concentrated sulfuric acid and stir, mix and infiltrate at -10°C for 0.5h , Potassium ferrate and perchloric acid were added, and then the reaction solution was raised to 0° C. for 1 h. After the reaction, the reaction solution was centrifuged at 4000r / min to discard the strong acid. Slowly pour the sediment at the bottom into deionized water at 10°C to dilute, let stand for 0.5h, wash the sediment repeatedly with 1mol / L dilute hydrochloric acid and deionized water, wash each 15 times in turn, and centrifuge until the centrifuged supernatant The pH value was close to 7, and the final product was freeze-dried at -30°C for 48 hours to obtain a single-layer graphene oxide. During the reaction, the ratio of strong acid to graphite is 80mL: 1g, and the ratio of pot...

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Abstract

The invention provides a preparation method of a single-layer graphene oxide modified waterborne polyurethane composite material, belonging to the field of preparation of inorganic nano modified polyurethane materials. The method provided by the invention comprises the following steps: firstly carrying out oxidized stripping on crystalline flake graphite by utilizing a novel strong oxidizer, namely potassium ferrate, and centrifugally washing to obtain single-layer graphene oxide; and ultrasonically dispersing the single-layer graphene oxide into deionized water, adding in the waterborne polyurethane emulsion stage, and stirring at a high speed so as to obtain single-layer graphene oxide modified waterborne polyurethane composite emulsion. Compared with the existing inorganic substance modified high molecular material, the single-layer graphene oxide modified waterborne polyurethane composite material has the advantages that the single-layer graphene oxide can be stably dispersed in a polymer matrix after being subjected to ultrasonic treatment; and because the attributes, such as specific surface area, strength and hardness, of the graphene oxide are superior to those of other nano modified substances, the waterborne polyurethane has great advantages in the aspects of thermal stability, mechanical properties and the like.

Description

technical field [0001] The invention relates to a method for preparing a single-layer graphene oxide modified water-based polyurethane composite material, in particular, firstly using a new strong oxidant, potassium ferrate, to quickly and safely oxidize and peel flake graphite, and prepare a single-layer graphene oxide after centrifugal washing , and then the single-layer graphene oxide is ultrasonically dispersed in deionized water and added in the water-based polyurethane emulsification stage, and the single-layer graphene oxide-modified water-based polyurethane composite emulsion is prepared after high-speed stirring, which belongs to the preparation field of inorganic nano-modified polyurethane materials . Background technique [0002] Water-based polyurethane (WPU) is widely used in the fields of coatings, adhesives, plastics, rubber, fibers, and leather finishes because it uses water as the medium, is non-toxic, non-polluting, and inexpensive. Although water-based PU...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L75/06C08K3/04C08J5/18
Inventor 蒋平平胡令张萍波卞刚盛松松黄敏
Owner JIANGNAN UNIV
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