阅读说明：本技术 一种石墨烯和纳米银复合抗菌材料的制备方法 (Preparation method of graphene and nano-silver composite antibacterial material ) 是由 马丽 陈宝元 陈利佳 郑新香 李耀峰 梁丰春 于 2019-10-22 设计创作，主要内容包括：本发明公开了一种石墨烯和纳米银复合抗菌材料的制备方法,然而这种抗菌材料化学性能不稳定,容易与细菌产生新物质,从而降低了使用寿命,且现有的抗菌材料的制备方法较为复杂,从而增加了工作的难度,降低了工作的效率,且在制备的过程中容易产生大量的有害气体,从而对环境和工作人员造成一定的影响,从而不利于普遍使用,且制备的过程中容易造成原料的浪费。本发明通过石墨粉和无水NANO<Sub>3</Sub>加入到浓硫酸中,在强力的搅拌下加入KMNO<Sub>4</Sub>,并通过双氧水还原剩余的高锰酸钾和MNO<Sub>2</Sub>,使气变为无色,MNSO<Sub>4</Sub>在双氧水的处理下,悬浮液呈亮黄色,然后过滤,清洗和干燥,从而得到氧化石墨烯,该种方法反应时间短,且避免了有害气体CIO<Sub>2</Sub>的产生,安全性能高,且利于普遍使用。(The invention discloses a preparation method of a graphene and nano-silver composite antibacterial material, which is unstable in chemical property and easy to generate new substances with bacteria, so that the service life is shortened, the existing preparation method of the antibacterial material is complex, the working difficulty is increased, the working efficiency is reduced, a large amount of harmful gas is easy to generate in the preparation process, so that certain influence is caused on the environment and workers, the general use is not facilitated, and raw materials are easy to waste in the preparation process. The invention uses graphite powder and anhydrous NANO 3 Adding into concentrated sulfuric acid, adding KMNO under strong stirring 4 And reducing the residual potassium permanganate and MNO by hydrogen peroxide 2 Rendering the gas colorless, MNSO 4 Under the treatment of hydrogen peroxideThe suspension is bright yellow, and then is filtered, cleaned and dried to obtain the graphene oxide, the reaction time of the method is short, and harmful gas CIO is avoided 2 The safety performance is high, and the universal use is facilitated.)

1. A preparation method of a graphene and nano-silver composite antibacterial material is characterized by comprising the following steps: the method specifically comprises the following steps:

step 1: oxidizing and stripping graphene in graphite, taking a flask A, and adding H into the flask A₂SO₄The solution was added and a quantity of NANO was added to flask A₃Then is filled by a stirring rodStirring to obtain a mixed solution A;

step 2: introducing graphite while stirring the mixed solution A, and adding a certain amount of KMNO₄Thereby obtaining a mixed solution B;

and step 3: adding deionized water into the mixed solution B, continuously stirring, then placing the flask A on a heater for heating, and heating the solution in the flask A to 100 ℃ to obtain a mixed solution C;

and 4, step 4: adding 30% hydrogen peroxide solution into the mixed solution C, stirring until the mixed solution C is golden yellow, washing the generated solid particles with water, filtering, and drying to obtain graphene oxide;

and 5: taking a flask B again, putting the graphene oxide into the flask B, and ultrasonically stripping the graphite oxide in distilled water for 1 hour until the solution is dark brown to obtain a mixed solution D;

step 6: adding a silver nitrate solution into the mixed solution D, continuing to perform ultrasonic vibration for 40 minutes, heating the mixed solution D through a magnetic stirrer, and then adding a sodium hydroxide solution until the solution is black, so as to obtain a mixed solution E;

and 7: centrifuging the mixed solution E by a centrifuge to separate liquid from solid, thereby obtaining black solid A;

and 8: washing the black solid A with distilled water until the washed liquid becomes neutral, thereby obtaining a black solid B;

and step 9: and then centrifuging, drying and grinding the black solid B to obtain the graphene and nano-silver composite material.

2. The preparation method of the graphene and nano-silver composite antibacterial material according to claim 1, characterized by comprising the following steps: according to the step 8, the liquid cleaned by the part is sucked by a dropper and is dripped on the acid-base indicating paper, so that the color of the acid-base indicating paper is changed and is compared with the acid-base color list until the liquid cleaned by the dropper is neutral.

3. The preparation method of the graphene and nano-silver composite antibacterial material according to claim 1, characterized by comprising the following steps: according to step 2, the temperature of the mixture B inside the flask a was set at 20 degrees celsius during stirring, and stirring was continued for 2 hours until the solution B became bright yellow.

4. The preparation method of the graphene and nano-silver composite antibacterial material according to claim 1, characterized by comprising the following steps: according to step 4, the mixed solution C is in a high temperature state while adding a 30% hydrogen peroxide solution to the mixed solution C.

5. The preparation method of the graphene and nano-silver composite antibacterial material according to claim 1, characterized by comprising the following steps: and (5) preparing the graphene-loaded nano-silver composite material by adopting a chemical reduction method.

6. The preparation method of the graphene and nano-silver composite antibacterial material according to claim 1, characterized by comprising the following steps: according to step 3, flask A is preheated before being heated.

7. The preparation method of the graphene and nano-silver composite antibacterial material according to claim 1, characterized by comprising the following steps: according to step 2, a quantity of KMNO is added₄Slowly adding the mixture into the mixed solution A for multiple times.

Technical Field

The invention relates to the technical field of antibacterial material preparation, in particular to a preparation method of a graphene and nano-silver composite antibacterial material.

Background

Many substances in nature have good functions of sterilizing or inhibiting microorganisms, such as organic compounds partially having specific groups, some inorganic metal materials and compounds thereof, and partial minerals and natural substances, but at present, the antibacterial materials refer to a novel functional material which has the capability of inhibiting or killing surface bacteria by adding a certain antibacterial substance (called as an antibacterial agent), such as antibacterial plastics, antibacterial fibers and fabrics, antibacterial ceramics, antibacterial metal materials and the like.

However, the antibacterial material is unstable in chemical property and easy to produce new substances with bacteria, so that the service life is prolonged, the existing preparation method of the antibacterial material is complex, the difficulty of work is increased, the efficiency of work is reduced, a large amount of harmful gas is easy to produce in the preparation process, certain influence is caused on the environment and workers, the antibacterial material is not beneficial to general use, the raw materials are easy to waste in the preparation process, and the cost is improved.

Disclosure of Invention

The invention aims to provide a preparation method of a graphene and nano-silver composite antibacterial material, so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a graphene and nano-silver composite antibacterial material specifically comprises the following steps:

step 1: oxidizing and stripping graphene in graphite, taking a flask A, and adding H into the flask A₂SO₄The solution was added and a quantity of NANO was added to flask A₃Then fully stirring the mixture by a stirring rod to obtain a mixed solution A;

step 2: introducing graphite while stirring the mixed solution A, and adding a certain amount of KMNO₄Thereby obtaining a mixed solution B;

and step 3: adding deionized water into the mixed solution B, continuously stirring, then placing the flask A on a heater for heating, and heating the solution in the flask A to 100 ℃ to obtain a mixed solution C;

and 4, step 4: adding 30% hydrogen peroxide solution into the mixed solution C, stirring until the mixed solution C is golden yellow, washing the generated solid particles with water, filtering, and drying to obtain graphene oxide;

and 5: taking a flask B again, putting the graphene oxide into the flask B, and ultrasonically stripping the graphite oxide in distilled water for 1 hour until the solution is dark brown to obtain a mixed solution D;

step 6: adding a silver nitrate solution into the mixed solution D, continuing to perform ultrasonic vibration for 40 minutes, heating the mixed solution D through a magnetic stirrer, and then adding a sodium hydroxide solution until the solution is black, so as to obtain a mixed solution E;

and 7: centrifuging the mixed solution E by a centrifuge to separate liquid from solid, thereby obtaining black solid A;

and 8: washing the black solid A with distilled water until the washed liquid becomes neutral, thereby obtaining a black solid B;

and step 9: and then centrifuging, drying and grinding the black solid B to obtain the graphene and nano-silver composite material.

Preferably, according to step 8, a dropper is used to suck the liquid washed by the washing part and drop the liquid on the acid-base indicating paper, so that the color of the acid-base indicating paper is changed and compared with the acid-base color list until the liquid washed by the washing part is neutral.

Preferably, according to step 2, the temperature of the mixture B inside the flask a is brought to 20 degrees celsius during stirring and stirring is continued for 2 hours until the solution B becomes bright yellow.

Preferably, according to step 4, mixed liquor C is in a high temperature state while adding 30% hydrogen peroxide solution to mixed liquor C.

Preferably, according to step 5, the graphene-supported nano silver composite material is prepared by a chemical reduction method.

Preferably, according to step 3, flask a is preheated before being heated.

Preferably, according to step 2, an amount of KMNO is added₄Slowly adding the mixture into the mixed solution A for multiple times.

Compared with the prior art, the invention has the beneficial effects that: the invention is through H₂SO₄、NANO₃、KMNO₄The method comprises the steps of carrying out oxidation treatment on graphite, carrying out mixed reaction on deionized water, hydrogen peroxide solution and solution C at high temperature, carrying out oxidation decomposition on graphene in the graphite, and preparing the graphene-loaded nano silver composite material by a chemical reduction method, so that the antibacterial material is more stable in chemical property and is not easy to generate new substances with bacteria, the service life is prolonged, the preparation method of the antibacterial material is simpler, the working difficulty is reduced, the working efficiency is improved, the reaction time is short, and harmful gas CIO is avoided₂The production of (2) and avoided causing certain influence to environment and staff, the security performance is high, and does benefit to universal use, and each solution adds according to certain proportion at the in-process of preparation to make this kind of preparation method of graphite alkene and nanometer silver composite antibacterial material better to the accuse effect of raw materials, avoid causing the waste of raw materials, thereby the cost is reduced.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with 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. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The embodiment provided by the invention comprises the following steps: a preparation method of a graphene and nano-silver composite antibacterial material specifically comprises the following steps:

step 1: oxidizing and stripping graphene in graphite, taking a flask A, and adding H into the flask A₂SO₄The solution was added and a quantity of NANO was added to flask A₃Then fully stirring the mixture by a stirring rod to obtain a mixed solution A;

step 2: introducing graphite while stirring the mixed solution A, and adding a certain amount of KMNO₄Thereby obtaining a mixed solution B;

and step 3: adding deionized water into the mixed solution B, continuously stirring, then placing the flask A on a heater for heating, and heating the solution in the flask A to 100 ℃ to obtain a mixed solution C;

and 4, step 4: adding 30% hydrogen peroxide solution into the mixed solution C, stirring until the mixed solution C is golden yellow, washing the generated solid particles with water, filtering, and drying to obtain graphene oxide;

and 5: taking a flask B again, putting the graphene oxide into the flask B, and ultrasonically stripping the graphite oxide in distilled water for 1 hour until the solution is dark brown to obtain a mixed solution D;

step 6: adding a silver nitrate solution into the mixed solution D, continuing to perform ultrasonic vibration for 40 minutes, heating the mixed solution D through a magnetic stirrer, and then adding a sodium hydroxide solution until the solution is black, so as to obtain a mixed solution E;

and 7: centrifuging the mixed solution E by a centrifuge to separate liquid from solid, thereby obtaining black solid A;

and 8: washing the black solid A with distilled water until the washed liquid becomes neutral, thereby obtaining a black solid B;

and step 9: and then centrifuging, drying and grinding the black solid B to obtain the graphene and nano-silver composite material.

Hair brushMingdong graphite powder and anhydrous NANO₃Adding into concentrated sulfuric acid, adding KMNO under strong stirring₄And reducing the residual potassium permanganate and MNO by hydrogen peroxide₂Rendering the gas colorless, MNSO₄Under the treatment of hydrogen peroxide, the suspension is bright yellow, and then is filtered, cleaned and dried to obtain the graphene oxide₂The safety performance is high, and the universal use is facilitated.