阅读说明：本技术 一种石墨烯插层材料的制备方法 (Preparation method of graphene intercalation material ) 是由 衷田妹 于 2021-08-17 设计创作，主要内容包括：本发明公开了一种石墨烯插层材料的制备方法,包括如下步骤：S1、称取一定量的天然石墨通过化学试剂以及氧化剂进行氧化还原反应制得石墨溶剂；S2、然后向石墨溶剂内分多次添加氧化钒并充分搅拌混合制得氧化石墨混合液；S3、将所得氧化石墨混合液放入搅拌机内进行加热搅拌烘干,制得固体反应物；S4、将固定体反应物进行水洗,并对洗净后的固体进行低温干燥,制得氧化石墨粉体；S5、对氧化石墨粉体进行高温加热剥离,制得氧化石墨烯。本发明方法操作简单,产量高,使所制得的石墨烯含有较丰富的氧化钒,且石墨烯通过氧化钒插层,有效的提高了石墨烯的导电性,进而提高了成品材料的电磁屏蔽性能。(The invention discloses a preparation method of a graphene intercalation material, which comprises the following steps: s1, weighing a certain amount of natural graphite, and carrying out oxidation-reduction reaction on the natural graphite through a chemical reagent and an oxidant to prepare a graphite solvent; s2, adding vanadium oxide into the graphite solvent for multiple times, and fully stirring and mixing to obtain a graphite oxide mixed solution; s3, putting the obtained graphite oxide mixed solution into a stirrer, heating, stirring and drying to obtain a solid reactant; s4, washing the reactant of the immobilized body with water, and drying the washed solid at low temperature to obtain graphite oxide powder; and S5, heating and stripping the graphite oxide powder at high temperature to obtain the graphene oxide. The method is simple to operate and high in yield, the prepared graphene contains abundant vanadium oxide, and the graphene is intercalated by the vanadium oxide, so that the conductivity of the graphene is effectively improved, and the electromagnetic shielding performance of a finished material is further improved.)

1. A preparation method of a graphene intercalation material is characterized by comprising the following steps:

s1, weighing a certain amount of natural graphite, and carrying out oxidation-reduction reaction on the natural graphite through a chemical reagent and an oxidant to prepare a graphite solvent;

s2, adding vanadium oxide into the graphite solvent for multiple times, and fully stirring and mixing to obtain a graphite oxide mixed solution;

s3, putting the obtained graphite oxide mixed solution into a stirrer, heating, stirring and drying to obtain a solid reactant;

s4, washing the reactant of the immobilized body with water, and drying the washed solid at low temperature to obtain graphite oxide powder;

s5, heating and stripping the graphite oxide powder at high temperature to obtain graphene oxide;

s6, putting graphite oxide into water for mixing, and then dispersing through ultrasonic oscillation to form a uniformly dispersed graphene oxide solution;

s7, dropwise adding ammonia water into the graphene oxide solution, and dissolving a reducing agent in water to form a mixed aqueous solution;

s8, uniformly mixing the prepared graphene oxide solution and the reducing agent aqueous solution, placing the obtained mixed solution in an oil bath, stirring, and after the reaction is finished, filtering, washing and drying the mixture to obtain the graphene.

2. The method according to claim 1, wherein the chemical reagent in S1 is a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and the concentration of the concentrated sulfuric acid is 80%.

3. The method according to claim 1, wherein the oxidant in S1 is an acidic potassium permanganate solution.

4. The method of claim 1, wherein the temperature of the heating in S3 is controlled at 80 ℃ and the temperature of the cooling in S4 is controlled at 20 ℃.

5. The method according to claim 1, wherein the high temperature in the step S5 is controlled at 85 ℃, and the mass concentration of the graphene oxide solution is 0.25 g/L-1 g/L.

6. The method according to claim 1, wherein the mass concentration of ammonia water in S7 is 28%, and the mass concentration of the aqueous solution of the reducing agent is 0.25 g/L-2 g/L.

Technical Field

The invention relates to the technical field of graphene materials, in particular to a preparation method of a graphene intercalation material.

Background

Graphene (Graphene) is sp²The hybridized and connected carbon atoms are tightly packed into a new material with a single-layer two-dimensional honeycomb lattice structure. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.

Graphene has been primarily used as an electromagnetic shielding material. However, when graphene is made into an electromagnetic shielding material, a physical adhesive or an auxiliary agent is usually required to be added to make a jelly with a certain viscosity to be adhered to the surface of an electromagnetic source, and the added adhesive and auxiliary agent are often poor in conductive capacity, so that the electromagnetic shielding performance of graphene is reduced.

Disclosure of Invention

Based on the technical problems in the background art, the invention provides a preparation method and a construction method of a graphene intercalation material.

The invention provides a preparation method of a graphene intercalation material, which comprises the following steps.

A preparation method of a graphene intercalation material comprises the following steps:

s1, weighing a certain amount of natural graphite, and carrying out oxidation-reduction reaction on the natural graphite through a chemical reagent and an oxidant to prepare a graphite solvent;

s2, adding vanadium oxide into the graphite solvent for multiple times, and fully stirring and mixing to obtain an oxidized graphite mixed solution;

s3, putting the obtained graphite oxide mixed solution into a stirrer, heating, stirring and drying to obtain a solid reactant;

s4, washing the reactant of the immobilized body with water, and drying the washed solid at low temperature to obtain graphite oxide powder;

s5, heating and stripping the graphite oxide powder at high temperature to obtain graphene oxide;

s6, putting graphite oxide into water for mixing, and then dispersing through ultrasonic oscillation to form a uniformly dispersed graphene oxide solution;

s7, dropwise adding ammonia water into the graphene oxide solution, and dissolving a reducing agent in water to form a mixed aqueous solution;

and S8, uniformly mixing the prepared graphene oxide solution and the reducing agent aqueous solution, placing the obtained mixed solution in an oil bath, stirring, and after the reaction is finished, filtering, washing and drying the mixture to obtain the graphene.

Preferably, the chemical reagent in S1 is a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and the concentration of the concentrated sulfuric acid is 80%.

Preferably, the oxidant in S1 is an acidic potassium permanganate solution.

Preferably, the temperature of the heating in S3 is controlled to be 80 ℃, and the temperature of the low temperature in S4 is controlled to be 20 ℃.

Preferably, the high-temperature in the step S5 is controlled at 85 ℃, and the mass concentration of the graphene oxide solution is 0.25 g/L-1 g/L.

Preferably, the mass concentration of ammonia water in the S7 is 28%, and the mass concentration of the reducing agent aqueous solution is 0.25 g/L-2 g/L.

The invention has the beneficial effects that:

the method is simple to operate, the yield is high, the prepared graphene contains abundant vanadium oxide, and the graphene is intercalated by the vanadium oxide, so that the conductivity of the graphene is effectively improved, and the electromagnetic shielding performance of a finished material is further improved.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

The embodiment provides a preparation method of a graphene intercalation material, which comprises the following steps:

s1, weighing a certain amount of natural graphite, and carrying out oxidation-reduction reaction on the natural graphite through a chemical reagent and an oxidant to prepare a graphite solvent, wherein the chemical reagent is a mixed solution of concentrated nitric acid and concentrated sulfuric acid, the concentration of the concentrated sulfuric acid is 80%, and the oxidant is an acidic potassium permanganate solution;

s2, adding vanadium oxide into the graphite solvent for multiple times, and fully stirring and mixing to obtain an oxidized graphite mixed solution;

s3, putting the obtained graphite oxide mixed solution into a stirrer, controlling the temperature at 80 ℃, heating, stirring and drying to obtain a solid reactant;

s4, washing the reactant of the immobilized body with water, and drying the washed solid at a low temperature of 20 ℃ to obtain graphite oxide powder;

s5, heating and stripping the graphite oxide powder at a high temperature of 85 ℃ to obtain graphene oxide;

s6, putting graphite oxide into water for mixing, and then dispersing through ultrasonic oscillation to form a uniformly dispersed graphene oxide solution;

s7, dropwise adding ammonia water with the mass concentration of 28% into the graphene oxide solution, and dissolving a reducing agent into water to form a mixed water solution with the mass concentration of 0.25 g/L-2 g/L;

and S8, uniformly mixing the prepared graphene oxide solution and the reducing agent aqueous solution, placing the obtained mixed solution in an oil bath, stirring, and after the reaction is finished, filtering, washing and drying the mixture to obtain the graphene.

In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown herein, merely for convenience in describing the invention and for simplicity in description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention should be covered by the scope of the present invention.