阅读说明：本技术 一种氧化石墨的制备方法 (Preparation method of graphite oxide ) 是由 任洁 于 2018-09-11 设计创作，主要内容包括：本发明公开了氧化石墨造领域内的一种氧化石墨的制备方法,包括以下步骤：(1)、将硫酸冷却后加入石墨进行反应；(2)、之后再加入硝酸钠和高锰酸钾进行一次升温反应；(3)、之后再进行二次升温反应；(4)、最后进行三次升温反应；(5)、得到的反应物经过离心分离后得到分离固体；(6)、分离固体经过洗涤后烘干得到氧化石墨；将硫酸冷却后加入石墨进行反应；之后再加入硝酸钠和高锰酸钾进行一次升温反应；之后再进行二次升温反应；最后进行三次升温反应；得到的反应物经过离心分离后得到分离固体；分离固体经过洗涤后烘干得到氧化石墨,可以提升氧化石墨的产量和品质,降低了生产成本,扩大了氧化石墨的应用范围,本发明可以用于氧化石墨的制备。(The invention discloses a preparation method of graphite oxide in the field of graphite oxide manufacturing, which comprises the following steps: (1) cooling the sulfuric acid, and adding graphite for reaction; (2) then adding sodium nitrate and potassium permanganate to carry out primary heating reaction; (3) then carrying out secondary heating reaction; (4) finally carrying out three times of heating reaction; (5) centrifugally separating the obtained reactant to obtain a separated solid; (6) washing and drying the separated solid to obtain graphite oxide; cooling sulfuric acid, and adding graphite for reaction; then adding sodium nitrate and potassium permanganate to carry out primary heating reaction; then carrying out secondary heating reaction; finally, carrying out three times of heating reaction; centrifugally separating the obtained reactant to obtain a separated solid; the separated solid is washed and dried to obtain the graphite oxide, so that the yield and the quality of the graphite oxide can be improved, the production cost is reduced, the application range of the graphite oxide is expanded, and the method can be used for preparing the graphite oxide.)

1. The preparation method of graphite oxide is characterized by comprising the following steps:

(1) cooling the sulfuric acid, and adding graphite for reaction;

(2) then adding sodium nitrate and potassium permanganate to carry out primary heating reaction;

(3) then carrying out secondary heating reaction;

(4) finally carrying out three times of heating reaction;

(5) centrifugally separating the obtained reactant to obtain a separated solid;

(6) and washing and drying the separated solid to obtain the graphite oxide.

2. The method for preparing graphite oxide according to claim 1, wherein: the sulfuric acid is concentrated sulfuric acid.

3. The method for preparing graphite oxide according to claim 2, wherein: the temperature after cooling is 0 ℃.

4. The method for preparing graphite oxide according to claim 1 or 3, wherein: the temperature after the primary heating is 4 ℃, and the reaction time is 90 min.

5. The method for preparing graphite oxide according to claim 4, wherein: the temperature after the secondary heating is 32-40 ℃, and the reaction time is 30 min.

6. The method for preparing graphite oxide according to claim 5, wherein: the temperature of the three times of temperature rise is 70-100 ℃, and the reaction time is 30 min.

7. The method for preparing graphite oxide according to claim 1, wherein: the drying temperature is 40 ℃.

Technical Field

The invention relates to a preparation method of graphite oxide.

Background

The loose graphite oxide is dispersed in an alkaline solution to form single atom thick fragments resembling graphene structures. Graphite oxide has the possibility of being used for industrial production of graphene because of the property, and thus attracts a plurality of scientists to participate in research. However, until 2010, this graphene preparation route still had a number of structural problems. The structure and properties of graphite oxide depend on the method of synthesizing it. The graphite oxide still retained the lamellar structure of the graphite matrix, but the spacing between the two layers (about 0.7 nm) was about twice that of the layers in the graphite. Strictly speaking, the word "oxidation" is incorrect and is only retained for historical reasons. In graphite oxide, in addition to the peroxy bond purely introducing oxygen atoms, experiments have confirmed that other kinds of functional groups, such as carbonyl (= CO), hydroxyl (-OH), and phenolic hydroxyl groups, are present in the structure. The thickness of the graphite oxide layer is about 1.1 +/-0.2 nm. Scanning tunneling microscopy showed that in some regions of graphite oxide, the oxygen atoms are arranged in a rectangular pattern with a lattice constant of 0.27 nm by 0.41 nm. The extreme edges of the graphite oxide layer are carbonyl or carboxyl. Has antibacterial effect, and can be used for treating bacillary dysentery. Has astringent, hemostatic, and antidiarrheal effects, and can be used as antiseptic, pyrogallic acid, medicine, ink, mordant dye, and explosion-proof agent, and also used as developer and analytical reagent for detecting free inorganic acid, dihydroxyacetone, alkaloid, metal, etc. However, in the prior art, the yield of graphite oxide is low, the quality is low, the production cost is high, and the application of graphite oxide is restricted.

Disclosure of Invention

The invention aims to provide a preparation method of graphite oxide, which can improve the yield and quality of graphite oxide, reduce the production cost and expand the application range of graphite oxide.

In order to achieve the above object, the present invention provides a method for preparing graphite oxide, comprising the steps of: (1) cooling the sulfuric acid, and adding graphite for reaction;

(2) then adding sodium nitrate and potassium permanganate to carry out primary heating reaction;

(3) then carrying out secondary heating reaction;

(4) finally carrying out three times of heating reaction;

(5) centrifugally separating the obtained reactant to obtain a separated solid;

(6) and washing and drying the separated solid to obtain the graphite oxide.

Compared with the prior art, the invention has the beneficial effects that the sulfuric acid is cooled and then added with the graphite for reaction; then adding sodium nitrate and potassium permanganate to carry out primary heating reaction; then carrying out secondary heating reaction; finally, carrying out three times of heating reaction; centrifugally separating the obtained reactant to obtain a separated solid; the separated solid is washed and dried to obtain the graphite oxide, so that the yield and the quality of the graphite oxide can be improved, the production cost is reduced, the application range of the graphite oxide is expanded, and the method can be used for preparing the graphite oxide.

As a further improvement of the invention, the sulfuric acid is concentrated sulfuric acid, so that better oxidizing property of the reaction can be ensured.

As a further improvement of the invention, the temperature after cooling is 0 ℃, so that the reaction speed is fastest and the reaction is not very violent.

As a further improvement of the invention, the temperature after the primary temperature rise is 4 ℃, and the reaction time is 90min, so that the effect of the primary temperature rise reaction can be best.

As a further improvement of the invention, the temperature after the secondary temperature rise is 32-40 ℃, and the reaction time is 30min, so that the effect of the secondary temperature rise reaction can be best.

As a further improvement of the invention, the temperature of the three times of temperature rise is 70-100 ℃, and the reaction time is 30min, so that the effect of the three times of temperature rise reaction can be the best.

As a further improvement of the invention, the drying temperature is 40 ℃, so that the properties of the graphite oxide can not be changed while the graphite oxide is dried.

Drawings

FIG. 1 is a flow chart of the present invention.

Detailed Description

The invention is further described below with reference to the accompanying drawings:

the preparation method of graphite oxide shown in fig. 1 comprises the following steps: (1) cooling the sulfuric acid, and adding graphite for reaction; (2) then adding sodium nitrate and potassium permanganate to carry out primary heating reaction; (3) then carrying out secondary heating reaction; (4) finally carrying out three times of heating reaction; (5) centrifugally separating the obtained reactant to obtain a separated solid; (6) washing and drying the separated solid to obtain graphite oxide; the sulfuric acid is concentrated sulfuric acid; the temperature after cooling is 0 ℃; the temperature after the primary heating is 4 ℃, and the reaction time is 90 min; the temperature after the secondary heating is 32-40 ℃, and the reaction time is 30 min; the temperature of the third heating is 70-100 ℃, and the reaction time is 30 min; the drying temperature is 40 ℃.

During working, the sulfuric acid is cooled and then added with graphite for reaction; then adding sodium nitrate and potassium permanganate to carry out primary heating reaction; then carrying out secondary heating reaction; finally, carrying out three times of heating reaction; centrifugally separating the obtained reactant to obtain a separated solid; the separated solid is washed and dried to obtain the graphite oxide, so that the yield and the quality of the graphite oxide can be improved, the production cost is reduced, the application range of the graphite oxide is expanded, and the method can be used for preparing the graphite oxide.

The present invention is not limited to the above embodiments, and based on the technical solutions of the present disclosure, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.