阅读说明：本技术 一种石墨烯改性金属的制备方法 (Preparation method of graphene modified metal ) 是由 许怒涛 许镇南 于 2021-08-20 设计创作，主要内容包括：本发明涉及金属制备领域的一种石墨烯改性金属的制备方法,该方法包括以下步骤：第一步,制备氧化石墨；将115mL浓硫酸置于带有机械搅拌和冰浴装置的四口烧瓶中充分冷却至4-5℃,将5.0g石墨和2.5g硝酸钠加入并搅15分钟,缓慢加入35.0g高猛酸钾,控温在10℃以下搅拌30分钟；升温至35℃中温反应60分钟后,再将230mL去离子水滴加进混合物中,使体系温度升至95-98℃,搅拌30分钟得到氧化石墨；将氧化石墨倒入1L去离子水中,加入双氧水并搅拌,直至变为黄色；氧化石墨依次用5％的稀盐酸和去离子水洗至pH为5。(The invention relates to a preparation method of graphene modified metal in the field of metal preparation, which comprises the following steps: firstly, preparing graphite oxide; placing 115mL of concentrated sulfuric acid into a four-neck flask with a mechanical stirring and ice bath device, fully cooling to 4-5 ℃, adding 5.0g of graphite and 2.5g of sodium nitrate, stirring for 15 minutes, slowly adding 35.0g of potassium permanganate, controlling the temperature below 10 ℃, and stirring for 30 minutes; heating to 35 ℃ and reacting at medium temperature for 60 minutes, then dropwise adding 230mL of deionized water into the mixture, heating the system to 95-98 ℃, and stirring for 30 minutes to obtain graphite oxide; pouring graphite oxide into 1L of deionized water, adding hydrogen peroxide and stirring until the graphite oxide becomes yellow; the graphite oxide was washed with 5% dilute hydrochloric acid and deionized water in that order to a pH of 5.)

1. A preparation method of graphene modified metal is characterized by comprising the following steps:

firstly, preparing graphite oxide; (1) placing 115mL of concentrated sulfuric acid into a four-neck flask with a mechanical stirring and ice bath device, fully cooling to 4-5 ℃, adding 5.0g of graphite and 2.5g of sodium nitrate, stirring for 15 minutes, slowly adding 35.0g of potassium permanganate, controlling the temperature below 10 ℃, and stirring for 30 minutes;

(2) heating to 35 ℃ and reacting at medium temperature for 60 minutes, then dropwise adding 230mL of deionized water into the mixture, heating the system to 95-98 ℃, and stirring for 30 minutes to obtain graphite oxide;

(3) pouring graphite oxide into 1L of deionized water, adding hydrogen peroxide and stirring until the graphite oxide becomes yellow;

(4) washing the graphite oxide with 5% dilute hydrochloric acid and deionized water in sequence until the pH value is 5;

secondly, intercalation treatment; mixing the graphite oxide obtained in the first step as a raw material, potassium ferrate, phosphorus pentoxide, concentrated sulfuric acid and concentrated nitric acid as an intercalation agent, potassium permanganate as a catalytic oxidant, and stirring at a high speed of 54-56 ℃ for 1.8-2.2 hours to obtain premixed graphite oxide;

thirdly, high-frequency ultrasonic oxidation; pouring concentrated sulfuric acid into a dry reaction kettle, cooling to a temperature lower than 4 ℃ by adopting an ultrasonic ice bath, uniformly mixing the obtained premixed graphite oxide, the intercalation agent and the oxidant, adding into the reaction kettle, and standing for 65-75 min;

fourthly, turning off the ultrasound; starting a stirring device, controlling the temperature of the reaction system not to exceed 20 ℃, and continuing stirring for 1.5 h;

fifthly, preparing a graphene oxide solution; heating the reaction temperature to 98 ℃, continuously stirring at constant temperature, carrying out suction filtration while the reaction is hot, and washing with 10% by mass of dilute hydrochloric acid; after washing, taking out the product, dispersing the product in deionized water, and performing ultrasonic oscillation for 3 hours to obtain a graphene oxide solution;

sixthly, preparing graphene; fully drying the graphene oxide solution at 78-82 ℃, and then grinding to obtain graphene oxide; and carrying out solid-liquid separation on the graphene solution, and collecting solids to obtain the graphene.

2. The method for preparing graphene-modified metal according to claim 1, wherein the method comprises the following steps: in the second step; the mass ratio of the obtained product, the potassium ferrate, the phosphorus pentoxide, the concentrated sulfuric acid, the concentrated nitric acid and the potassium permanganate is 1: 5: 0.6: 30: 0.09.

3. The method for preparing graphene-modified metal according to claim 1, wherein the method comprises the following steps: in the third step; the mass ratio of the product obtained in the high-frequency ultrasonic oxidation, the sodium boroxide, the hydrazine hydrate and the deionized high-purity water is 1: 25: 30.

Technical Field

The invention relates to the field of metal preparation, in particular to a preparation method of graphene modified metal.

Background

Graphene (Graphene) is a two-dimensional crystal consisting of carbon atoms only one layer atomic thick exfoliated from a graphitic material. In 2004, the physicists andrelim and consanguin norworth schloff, manchester university, uk, succeeded in isolating graphene from graphite, confirming that it can exist alone. Graphene is the thinnest material and the toughest material, and the breaking strength is 200 times higher than that of the best steel;

meanwhile, the elastic fabric has good elasticity, and the stretching amplitude can reach 20% of the size of the elastic fabric. It is the thinnest and highest-strength material in the natural world at present. Graphene is currently the most promising application as a silicon substitute for fabricating ultra-micro transistors for the production of future supercomputers. By replacing silicon with graphene, the operating speed of a computer processor will be hundreds of times faster. In addition, graphene is almost completely transparent, absorbing only 2.3% of light. On the other hand, it is very dense and impenetrable by even the smallest gas atoms. These characteristics make it well suited as a raw material for transparent electronic products such as transparent touch displays, light-emitting panels, and solar panels;

the synthesis method of graphene mainly includes two methods: mechanical methods and chemical methods. Mechanical methods include micro mechanical separation, epitaxy, and SiC heating; the chemical method is chemical reduction method and chemical dissociation method. However, in the prior art, the preparation process of the method for preparing graphene is slow, and the layering effect is not good, so that a novel preparation method needs to be developed.

Disclosure of Invention

The invention aims to solve the defects and provides a preparation method of graphene modified metal.

The purpose of the invention is realized by the following modes:

a preparation method of graphene modified metal comprises the following steps:

firstly, preparing graphite oxide; (1) placing 115mL of concentrated sulfuric acid into a four-neck flask with a mechanical stirring and ice bath device, fully cooling to 4-5 ℃, adding 5.0g of graphite and 2.5g of sodium nitrate, stirring for 15 minutes, slowly adding 35.0g of potassium permanganate, controlling the temperature below 10 ℃, and stirring for 30 minutes;

(2) heating to 35 ℃ and reacting at medium temperature for 60 minutes, then dropwise adding 230mL of deionized water into the mixture, heating the system to 95-98 ℃, and stirring for 30 minutes to obtain graphite oxide;

(3) pouring graphite oxide into 1L of deionized water, adding hydrogen peroxide and stirring until the graphite oxide becomes yellow;

(4) washing the graphite oxide with 5% dilute hydrochloric acid and deionized water in sequence until the pH value is 5;

secondly, intercalation treatment; mixing the graphite oxide obtained in the first step as a raw material, potassium ferrate, phosphorus pentoxide, concentrated sulfuric acid and concentrated nitric acid as an intercalation agent, potassium permanganate as a catalytic oxidant, and stirring at a high speed of 54-56 ℃ for 1.8-2.2 hours to obtain premixed graphite oxide;

thirdly, high-frequency ultrasonic oxidation; pouring concentrated sulfuric acid into a dry reaction kettle, cooling to a temperature lower than 4 ℃ by adopting an ultrasonic ice bath, uniformly mixing the obtained premixed graphite oxide, the intercalation agent and the oxidant, adding into the reaction kettle, and standing for 65-75 min;

fourthly, turning off the ultrasound; starting a stirring device, controlling the temperature of the reaction system not to exceed 20 ℃, and continuing stirring for 1.5 h;

fifthly, preparing a graphene oxide solution; heating the reaction temperature to 98 ℃, continuously stirring at constant temperature, carrying out suction filtration while the reaction is hot, and washing with 10% by mass of dilute hydrochloric acid; after washing, taking out the product, dispersing the product in deionized water, and performing ultrasonic oscillation for 3 hours to obtain a graphene oxide solution;

sixthly, preparing graphene; fully drying the graphene oxide solution at 78-82 ℃, and then grinding to obtain graphene oxide; and carrying out solid-liquid separation on the graphene solution, and collecting solids to obtain the graphene.

Preferably, in the second step; the mass ratio of the obtained product, the potassium ferrate, the phosphorus pentoxide, the concentrated sulfuric acid, the concentrated nitric acid and the potassium permanganate is 1: 5: 0.6: 30: 0.09.

Preferably, in the third step; the mass ratio of the product obtained in the high-frequency ultrasonic oxidation, the sodium boroxide, the hydrazine hydrate and the deionized high-purity water is 1: 25: 30.

The beneficial effects produced by the invention are as follows: the expandable graphite is used as a raw material, so that the price is low, the cost is low, the graphene is easy to strip, and the yield can be greatly improved;

the adopted equipment is simple, the operation is convenient, the production steps are few, and the method is suitable for large-scale production;

by adopting intercalation and oxidation, the prepared graphene has good reduction effect and dispersion effect and few defects;

the method adopts a novel cheap nontoxic oxidant, so that the graphene preparation process is fast, the layering effect is fast, the layering distance is large, the oxygen-containing functional groups are sufficient, the cost is low, and no pollution is caused.

Drawings

FIG. 1 is a schematic flow chart of a method according to an embodiment of the present invention;

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.

In this embodiment, referring to fig. 1, a method for preparing a graphene-modified metal specifically implemented by the embodiment includes the following steps:

firstly, preparing graphite oxide; (1) placing 115mL of concentrated sulfuric acid into a four-neck flask with a mechanical stirring and ice bath device, fully cooling to 4-5 ℃, adding 5.0g of graphite and 2.5g of sodium nitrate, stirring for 15 minutes, slowly adding 35.0g of potassium permanganate, controlling the temperature below 10 ℃, and stirring for 30 minutes;

(2) heating to 35 ℃ and reacting at medium temperature for 60 minutes, then dropwise adding 230mL of deionized water into the mixture, heating the system to 95-98 ℃, and stirring for 30 minutes to obtain graphite oxide;

(3) pouring graphite oxide into 1L of deionized water, adding hydrogen peroxide and stirring until the graphite oxide becomes yellow;

(4) washing the graphite oxide with 5% dilute hydrochloric acid and deionized water in sequence until the pH value is 5;

secondly, intercalation treatment; mixing the graphite oxide obtained in the first step as a raw material, potassium ferrate, phosphorus pentoxide, concentrated sulfuric acid and concentrated nitric acid as an intercalation agent, potassium permanganate as a catalytic oxidant, and stirring at a high speed of 54-56 ℃ for 1.8-2.2 hours to obtain premixed graphite oxide;

thirdly, high-frequency ultrasonic oxidation; pouring concentrated sulfuric acid into a dry reaction kettle, cooling to a temperature lower than 4 ℃ by adopting an ultrasonic ice bath, uniformly mixing the obtained premixed graphite oxide, the intercalation agent and the oxidant, adding into the reaction kettle, and standing for 65-75 min;

fourthly, turning off the ultrasound; starting a stirring device, controlling the temperature of the reaction system not to exceed 20 ℃, and continuing stirring for 1.5 h;

fifthly, preparing a graphene oxide solution; heating the reaction temperature to 98 ℃, continuously stirring at constant temperature, carrying out suction filtration while the reaction is hot, and washing with 10% by mass of dilute hydrochloric acid; after washing, taking out the product, dispersing the product in deionized water, and performing ultrasonic oscillation for 3 hours to obtain a graphene oxide solution;

sixthly, preparing graphene; fully drying the graphene oxide solution at 78-82 ℃, and then grinding to obtain graphene oxide; and carrying out solid-liquid separation on the graphene solution, and collecting solids to obtain the graphene.

In the second step; the mass ratio of the obtained product, the potassium ferrate, the phosphorus pentoxide, the concentrated sulfuric acid, the concentrated nitric acid and the potassium permanganate is 1: 5: 0.6: 30: 0.09.

In the third step; the mass ratio of the product obtained in the high-frequency ultrasonic oxidation, the sodium boroxide, the hydrazine hydrate and the deionized high-purity water is 1: 25: 30.

The foregoing is a more detailed description of the invention, taken in conjunction with the specific preferred embodiments thereof, and is not intended to limit the invention to the particular forms disclosed. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as the protection scope of the invention.