阅读说明：本技术 一种功能化氧化石墨烯-碳毡复合材料的制备方法 (Preparation method of functionalized graphene oxide-carbon felt composite material ) 是由 王远鹏 蔡丽芳 于 2019-08-13 设计创作，主要内容包括：本发明提供了一种功能化氧化石墨烯-碳毡复合材料的制备方法,如下步骤：制备的氧化石墨烯溶液作为浸渍材料；将聚丙烯氰基碳毡用去离子水洗涤烘干之后,将聚丙烯氰基碳毡置于浓硫酸、浓硝酸混合液中经80℃水浴加热3小时,用超纯水洗至pH为7.2后,置于烘箱烘干；按烘干后的聚丙烯氰基碳毡与氧化石墨烯溶液混合,在超声仪器中超声后,再放置室温下进行浸渍、烘干得氧化石墨烯浸渍的聚丙烯氰基碳毡；将氧化石墨烯浸渍的聚丙烯氰基碳毡与乙二胺在90℃水浴碱性条件下进行酰胺化反应,取出用超纯水洗涤至pH为7.2后,置于烘箱烘干。(The invention provides a preparation method of a functionalized graphene oxide-carbon felt composite material, which comprises the following steps: the prepared graphene oxide solution is used as a dipping material; washing and drying the polypropylene cyano-carbon felt by deionized water, placing the polypropylene cyano-carbon felt in a mixed solution of concentrated sulfuric acid and concentrated nitric acid, heating in a water bath at 80 ℃ for 3 hours, washing by ultrapure water until the pH value is 7.2, and then placing in an oven for drying; mixing the dried polypropylene cyano carbon felt with a graphene oxide solution, carrying out ultrasonic treatment in an ultrasonic instrument, and then soaking and drying at room temperature to obtain a graphene oxide impregnated polypropylene cyano carbon felt; carrying out amidation reaction on the graphene oxide impregnated polypropylene cyano carbon felt and ethylenediamine under the water bath alkaline condition of 90 ℃, taking out, washing with ultrapure water until the pH value is 7.2, and then placing in an oven for drying.)

1. A preparation method of a functionalized graphene oxide-carbon felt composite material is characterized by comprising the following steps:

(1) the graphene oxide solution prepared by an improved Hummers method is used as a dipping material;

(2) washing and drying the polypropylene cyano-carbon felt by deionized water, placing the polypropylene cyano-carbon felt in a mixed solution of concentrated sulfuric acid and concentrated nitric acid, heating in a water bath at 80 ℃ for 3 hours, washing by ultrapure water until the pH value is 7.2, and then placing in an oven for drying;

(3) mixing the dried polypropylene cyano carbon felt with a graphene oxide solution, carrying out ultrasonic treatment in an ultrasonic instrument, and then soaking and drying at room temperature to obtain a graphene oxide impregnated polypropylene cyano carbon felt;

(4) carrying out amidation reaction on the graphene oxide impregnated polypropylene cyano carbon felt and ethylenediamine under the water bath alkaline condition of 90 ℃, taking out, washing with ultrapure water until the pH value is 7.2, and then placing in an oven for drying.

2. The preparation method of the functionalized graphene oxide-carbon felt composite material according to claim 1, wherein the preparation method comprises the following steps: in the step (2), the mass ratio of the polypropylene cyano carbon felt to the mixed solution of concentrated sulfuric acid and concentrated nitric acid is 1: 3.

3. The preparation method of the functionalized graphene oxide-carbon felt composite material according to claim 1, wherein the preparation method comprises the following steps: and (4) the mass ratio of the polypropylene cyano carbon felt dried in the step (3) to the graphene oxide solution is 1: 5.

4. The preparation method of the functionalized graphene oxide-carbon felt composite material according to claim 1, wherein the preparation method comprises the following steps: the mass ratio of the graphene oxide impregnated polypropylene cyano carbon felt to the ethylene diamine in the step (4) is 1: 6.

5. The preparation method of the functionalized graphene oxide-carbon felt composite material according to claim 1, wherein the preparation method comprises the following steps: the alkaline condition in the step (4) is in 2M sodium hydroxide solution.

Technical Field

The invention relates to the field of biological materials, in particular to a functionalized graphene oxide-carbon felt composite material.

Background

The microbial electrochemical system converts the chemistry in organic matters into electric energy by utilizing the catalytic action of microbes, thereby realizing the purpose of energy conversion. The method has the advantages of generating clean energy, electric energy, efficiently degrading organic pollutants and the like, and is widely concerned in the fields of energy, environment and wastewater treatment. The main disadvantages of this system are slow system start-up time and low output power. In the system, the bacteria after forming the biological membrane have stronger resistance to external environment, chemical bactericides and other variable factors, and are more stable in an electrochemical system, so that higher power density output is maintained. The adhesion of microorganisms to the surface of the electrode material is a prerequisite for colonization and is also the basis for biofilm formation. Therefore, how to efficiently adsorb and continuously load microorganisms on the surface of an electrode in a microbial electrochemical system to form a biological membrane is one of the keys for improving the performance of the microbial electrochemical system.

The invention patent CN 107887615A reports a pretreatment method of a carbon-based electrode material of a microbial electrochemical system, which solves the technical problem that the pretreatment method of the electrode material of the existing microbial electrochemical system is expensive. However, this method does not incorporate the factor of microbial adhesion, which has some uncertainty as to the subsequent microbial adhesion and the outcome of power output.

The invention patent CN 107841462A proposes a novel interface method for rapidly adsorbing and releasing bacteria, but the novel interface method is reversible adhesion, has weak adhesion strength and is not beneficial to the generation of subsequent biological membranes. Therefore, the invention simulates the electrochemical environment for application analysis on the basis of enhancing the adhesion performance and the adhesion strength of the surface of the carbon-based material.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention provides a novel functionalized graphene oxide-carbon felt composite material for enhancing the microbial adhesion and the electrochemical performance.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a preparation method of a functionalized graphene oxide-carbon felt composite material comprises the following steps:

(1) the graphene oxide solution prepared by an improved Hummers method is used as a dipping material;

(2) washing and drying the polypropylene cyano-carbon felt by deionized water, placing the polypropylene cyano-carbon felt in a mixed solution of concentrated sulfuric acid and concentrated nitric acid, heating in a water bath at 80 ℃ for 3 hours, washing by ultrapure water until the pH value is 7.2, and then placing in an oven for drying;

(3) mixing the dried polypropylene cyano carbon felt with a graphene oxide solution, carrying out ultrasonic treatment in an ultrasonic instrument, and then soaking and drying at room temperature to obtain a graphene oxide impregnated polypropylene cyano carbon felt;

(4) carrying out amidation reaction on the graphene oxide impregnated polypropylene cyano carbon felt and ethylenediamine under the water bath alkaline condition of 90 ℃, taking out, washing with ultrapure water until the pH value is 7.2, and then placing in an oven for drying.

In a preferred embodiment: in the step (2), the mass ratio of the polypropylene cyano carbon felt to the mixed solution of concentrated sulfuric acid and concentrated nitric acid is 1: 3.

In a preferred embodiment: and (4) the mass ratio of the polypropylene cyano carbon felt dried in the step (3) to the graphene oxide solution is 1: 5.

In a preferred embodiment: the mass ratio of the graphene oxide impregnated polypropylene cyano carbon felt to the ethylene diamine in the step (4) is 1: 6.

In a preferred embodiment: the alkaline condition in the step (4) is in 2M sodium hydroxide solution.

Compared with the prior art, the invention has the beneficial effects that:

1. the prepared modified carbon felt material has good biocompatibility, and compared with a blank group, the adhesion amount of the electroactive microorganisms is almost increased by 3 times under the condition of no bacterial growth, namely single-layer adhesion, so that a good growth foundation is laid for the subsequent growth of a biological film, and the mechanism researches show that the microorganisms are attached to the surface of the material in an irreversible adhesion mode and have strong adhesion interaction force.

2. Electrochemical tests show that the surface charge accumulation amount of the modified carbon felt material with microorganisms attached is 87.94 times that of a blank group under the same environment and attachment time, so that the electrochemical performance is greatly enhanced, and the extracellular electron transfer rate is accelerated.

Drawings

FIG. 1 is a microscopic magnification of an unmodified carbon felt material;

FIG. 2 is a microscopic enlarged view of a graphene oxide modified carbon felt material;

FIG. 3 is a graph showing a comparison of adhesion of Shewanella on the surface of a material for 5 minutes and 10 minutes in an isotonic phosphate buffer system;

FIG. 4 is an electron micrograph of Shewanella adhesion on the surface of an unmodified material for 10 minutes;

FIG. 5 is an electron micrograph of Shewanella adhesion on the surface of an unmodified material for 30 minutes;

fig. 6 shows the surface charge accumulation amount of shiva bacteria on the unmodified carbon felt material and the graphene oxide modified carbon felt material under the same conditions.

Detailed Description

The invention is further described with reference to the following figures and detailed description.

The invention provides a preparation method of a functionalized graphene oxide-carbon felt composite material, which comprises the following steps:

(1) the graphene oxide solution prepared by an improved Hummers method is used as a dipping material;

(2) washing and drying the polypropylene cyano-carbon felt by deionized water, placing the polypropylene cyano-carbon felt in a mixed solution of concentrated sulfuric acid and concentrated nitric acid, heating in a water bath at 80 ℃ for 3 hours, washing by ultrapure water until the pH value is 7.2, and then placing in an oven for drying;

(3) mixing the dried polypropylene cyano carbon felt with a graphene oxide solution, carrying out ultrasonic treatment in an ultrasonic instrument, and then soaking and drying at room temperature to obtain a graphene oxide impregnated polypropylene cyano carbon felt;

(4) carrying out amidation reaction on the graphene oxide impregnated polypropylene cyano carbon felt and ethylenediamine under the water bath alkaline condition of 90 ℃, taking out, washing with ultrapure water until the pH value is 7.2, and then placing in an oven for drying.