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Three-dimensional porous graphite-coated nano zero-valent copper composite material and preparation method

A graphene-wrapped, nano-zero-valent technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of zero-valent material agglomeration, dissolution and deactivation, etc. Activity delay and prevention, high efficiency of the preparation process

Active Publication Date: 2018-06-26
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing graphene and nano-metal composite technology mainly focuses on the research of metal oxides, and its composite technology still cannot solve the problems of easy agglomeration and dissolution inactivation of zero-valent materials.

Method used

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  • Three-dimensional porous graphite-coated nano zero-valent copper composite material and preparation method
  • Three-dimensional porous graphite-coated nano zero-valent copper composite material and preparation method
  • Three-dimensional porous graphite-coated nano zero-valent copper composite material and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] First prepare graphene oxide (GO), the steps are as follows: add 106mL of concentrated sulfuric acid and 1.0g of expandable graphite into the reaction vessel, stir in an ice-water bath for 30min; slowly add 5g of potassium permanganate, and keep the system temperature not exceeding 15 ℃; after the reaction is completed, withdraw from the ice-water bath, and stir at a constant temperature of 35±1℃ for 3 days; then add ultrapure water three times, add 40mL for the first time, stir at 60±1℃ for 60min, and add 40mL for the second time , keep at 90±1°C for 30min, add 40mL ultrapure water directly for the third time; finally add 10mL 30wt% H 2 o 2 , centrifuged at 12000r / min for 30min while hot, after removing the supernatant, centrifuged and washed several times with hydrochloric acid and ultrapure water with a volume ratio of 1:10, and freeze-dried for later use, wherein the concentration of hydrochloric acid was 36-38%. (In other embodiments, conventional methods can also...

Embodiment 2

[0035] The preparation process of graphene oxide (GO) is the same as in Example 1. KBH 4 Under the condition that the stirring time of the reduced graphene is 1 h, the preparation steps of the three-dimensional porous graphene-wrapped nano-zero-valent copper composite material are as follows: first, 0.8 g of freeze-dried graphene oxide is ultrasonically dispersed in 100 ml of ultrapure water for 2 h; with 3g KBH 4 Mix, stir and react at room temperature for 1 h, pass argon to make the reaction vessel in an oxygen-free state; then drop 0.04 mol / L CuSO into the reaction vessel at a rate of 1 ml / min 4 ·5H 2 O solution 50ml, during the reaction process, argon gas was blown in to keep the reaction in the anaerobic state and prevent the agglomeration of nanoparticles, and kept stirring to keep the solution in a uniformly mixed state. After reacting for 1h, the synthesized composite material was naturally precipitated, discarded Supernatant liquid; adding the same amount of ultrap...

Embodiment 3

[0038] The preparation process of graphene oxide (GO) is the same as in Example 1. KBH 4 Under the condition that the stirring time of the reduced graphene is 25h, the preparation steps of the three-dimensional porous graphene-wrapped nano-zero-valent copper composite material are as follows: first, 0.8g of freeze-dried graphene oxide is ultrasonically dispersed in 100ml of ultrapure water for 2h; with 6.5g KBH 4 Mix, stir and react at room temperature for 25 hours, pass argon to make the reaction vessel in an oxygen-free state; then drop 0.04mol / L CuSO into the reaction vessel at a rate of 1ml / min 4 ·5H 2 O solution 50ml, during the reaction process, argon gas was blown in to keep the reaction in the anaerobic state and prevent the agglomeration of nanoparticles, and kept stirring to keep the solution in a uniformly mixed state. After reacting for 1h, the synthesized composite material was naturally precipitated, discarded Supernatant liquid; add the same amount of ultrapu...

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Abstract

The invention discloses a three-dimensional porous graphite-coated nano zero-valent copper composite material and a preparation method thereof, and belongs to the technical field of novel functional composite materials. The preparation method comprises the following steps that oxidized graphene and KBH4 are mixed at the indoor temperature; afterwards, a CuSO4.5H2O solution is dropped into mixed liquor of the oxidized graphene and the KBH4 under an oxygen-free atmosphere, after a reaction is completed, a synthesized composite material is naturally deposited, supernate is removed, and ultrapurewater or mixed liquor of hydrochloric acid and ultrapure water is added for washing; and a washed sample is refrigerated in vacuum and dried, so that the three-dimensional porous graphite-coated nanozero-valent copper composite material is obtained. According to the preparation method, the process is simple, operation is easy, the reaction is mild, special requirements for outside environment conditions are avoided, the raw materials are cheap and easy to obtain, and secondary pollution is avoided; and the composite material can prevent agglomeration to maintain the reaction activity of all components, dissolving-out inactivation of nano zero-valent copper is delayed and even prevented, and the preparation method has broad application prospects.

Description

technical field [0001] The invention belongs to the technical field of new functional composite materials, and more specifically relates to a three-dimensional porous graphene-wrapped nano-zero-valent copper composite material and a preparation method thereof. Background technique [0002] Nano-metal materials have small size effect, surface interface effect, high activation energy, more surface active sites and special chemical activity, and are widely used as catalysts. However, nano-metal materials, especially zero-valent materials, are prone to agglomeration and stripping inactivation. [0003] Graphene is a new type of two-dimensional carbon nanomaterial composed of a planar structure of six-membered rings of carbon atoms, and its theoretical specific surface area is very large (up to 2630m 2 / g); there are a large number of oxygen-containing groups such as epoxy groups, hydroxyl groups, and carboxyl groups on its surface, which has a unique nanostructure and excellent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/02B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00B22F9/24B22F1/054B22F1/16
Inventor 徐乐瑾陶渝杰杨雨佳杨军
Owner HUAZHONG UNIV OF SCI & TECH