A kind of preparation method of expanded graphite and its application in the adsorption of aromatic compounds

Abstract

The invention relates to a preparation method of expanded graphite and its application in the adsorption of aromatic compounds, and belongs to the field of adsorbents. In the present invention, pre-intercalated graphite is obtained by mixing one or more types of low-boiling alcohols with water and then adding natural flake graphite; the pre-intercalating graphite is mixed with weak or non-polar low-boiling organic compounds and then sealed in an autoclave. Heating the intercalation; cooling to room temperature after intercalation, microwave expansion. The expanded graphite prepared by the invention does not need sulfuric acid, nitric acid, perchloric acid, etc., which are strong corrosive substances, nor does it use strong oxidants such as potassium permanganate, potassium dichromate, etc.; The adsorption of compounds has obvious advantages.

Description

technical field

[0001] The invention relates to a preparation method of expanded graphite and its application in the adsorption of aromatic compounds, and belongs to the field of adsorbents. Background technique

[0002] Expanded Graphite (EG) is generally rapidly expanded by pre-oxidation and intercalation followed by high temperature or microwave treatment to obtain a fluffy, large specific surface area, worm-like flexible graphite material. The raw material is purified from natural graphite ore. Natural flake graphite obtained later. The traditional preparation method of expanded graphite needs to consume a large amount of oxidizing concentrated and strong acids such as concentrated sulfuric acid, concentrated nitric acid, concentrated perchloric acid, and high-concentration strong oxidants such as potassium permanganate, potassium dichromate, hydrogen peroxide and other reagents, and sometimes phosphoric acid is used. To be assisted; or to carry out DC electrochemical t...

Examples

Embodiment 1

[0021] A preparation method of expanded graphite, comprising the following steps:

[0022] 5 g of natural flake graphite (80 mesh, 99% carbon content, Qingdao Nanshu Hongda Graphite Products Co., Ltd.), add 5 ml of methanol and 2 ml of water, mix well, then 500 watts ultrasonic for 30 minutes, filter directly and wash 5 times, then dried at 105°C for 1 hour, and cooled to below 50°C to obtain pre-expanded graphite;

[0023] The obtained pre-expanded graphite was transferred to the autoclave, 0.5 ml of benzene was added, and the intercalation was sealed in the autoclave at 120° C. for 90 minutes, and then cooled to room temperature;

[0024] Open the autoclave cover, transfer the intercalated graphite into a 1000mL glass beaker in 5 times, and expand under 500 watt microwave power for 1 minute respectively to obtain the FEG of the present invention;

[0025] Its expansion ratio was 76 times measured by the graduated cylinder method.

Embodiment 2

[0027] A preparation method of expanded graphite, comprising the following steps:

[0028] 5 grams of natural flake graphite (80 mesh, 99% carbon content, Qingdao Nanshu Hongda Graphite Products Co., Ltd.), add 4 ml of ethanol and 4 ml of water, mix well, then 500 watts ultrasonic for 40 minutes, directly filter and wash 5 times, then dried at 105°C for 1.5 hours, and cooled to below 50°C to obtain pre-expanded graphite;

[0029] The pre-expanded graphite was transferred to the autoclave, 0.25 ml of petroleum ether and 0.25 ml of benzene were added, and the intercalation layer was sealed in the autoclave at 150°C for 60 minutes, and then cooled to room temperature;

[0030] Open the autoclave cover, transfer the intercalated graphite into a 1000 mL glass beaker in 5 times, and expand under 500 watt microwave power for 40 seconds to obtain the FEG of the present invention;

[0031] Its expansion ratio was 101 times measured by the graduated cylinder method.

Embodiment 3

[0033] A preparation method of expanded graphite, comprising the following steps:

[0034] 5 grams of natural flake graphite (80 mesh, 99% carbon content, Qingdao Nanshu Hongda Graphite Products Co., Ltd.), add 4 ml of propanol and 4 ml of water, mix well, then 500 watts ultrasonic for 60 minutes, directly filter and wash 5 times, then dried at 105°C for 1.5 hours, and cooled to below 50°C to obtain pre-expanded graphite;

[0035] The pre-expanded graphite was transferred to the autoclave, 0.1 ml of petroleum ether, 0.2 ml of benzene, 0.2 ml of n-hexane were added, and the autoclave was sealed and intercalated at 150 ° C for 60 minutes, and then cooled to room temperature;

[0036] Open the autoclave cover, transfer the intercalated graphite into a 1000 mL glass beaker in 5 times, and expand under 500 watt microwave power for 40 seconds to obtain the FEG of the present invention;

[0037] Its expansion ratio was 108 times measured by the graduated cylinder method.

technical field

[0001] The invention relates to a preparation method of expanded graphite and its application in the adsorption of aromatic compounds, and belongs to the field of adsorbents. Background technique

[0002] Expanded Graphite (EG) is generally rapidly expanded by pre-oxidation and intercalation followed by high temperature or microwave treatment to obtain a fluffy, large specific surface area, worm-like flexible graphite material. The raw material is purified from natural graphite ore. Natural flake graphite obtained later. The traditional preparation method of expanded graphite needs to consume a large amount of oxidizing concentrated and strong acids such as concentrated sulfuric acid, concentrated nitric acid, concentrated perchloric acid, and high-concentration strong oxidants such as potassium permanganate, potassium dichromate, hydrogen peroxide and other reagents, and sometimes phosphoric acid is used. To be assisted; or to carry out DC electrochemical t...

Examples

Embodiment 1

[0021] A preparation method of expanded graphite, comprising the following steps:

[0022] 5 g of natural flake graphite (80 mesh, 99% carbon content, Qingdao Nanshu Hongda Graphite Products Co., Ltd.), add 5 ml of methanol and 2 ml of water, mix well, then 500 watts ultrasonic for 30 minutes, filter directly and wash 5 times, then dried at 105°C for 1 hour, and cooled to below 50°C to obtain pre-expanded graphite;

[0023] The obtained pre-expanded graphite was transferred to the autoclave, 0.5 ml of benzene was added, and the intercalation was sealed in the autoclave at 120° C. for 90 minutes, and then cooled to room temperature;

[0024] Open the autoclave cover, transfer the intercalated graphite into a 1000mL glass beaker in 5 times, and expand under 500 watt microwave power for 1 minute respectively to obtain the FEG of the present invention;

[0025] Its expansion ratio was 76 times measured by the graduated cylinder method.

Embodiment 2

[0027] A preparation method of expanded graphite, comprising the following steps:

[0028] 5 grams of natural flake graphite (80 mesh, 99% carbon content, Qingdao Nanshu Hongda Graphite Products Co., Ltd.), add 4 ml of ethanol and 4 ml of water, mix well, then 500 watts ultrasonic for 40 minutes, directly filter and wash 5 times, then dried at 105°C for 1.5 hours, and cooled to below 50°C to obtain pre-expanded graphite;

[0029] The pre-expanded graphite was transferred to the autoclave, 0.25 ml of petroleum ether and 0.25 ml of benzene were added, and the intercalation layer was sealed in the autoclave at 150°C for 60 minutes, and then cooled to room temperature;

[0030] Open the autoclave cover, transfer the intercalated graphite into a 1000 mL glass beaker in 5 times, and expand under 500 watt microwave power for 40 seconds to obtain the FEG of the present invention;

[0031] Its expansion ratio was 101 times measured by the graduated cylinder method.

Embodiment 3

[0033] A preparation method of expanded graphite, comprising the following steps:

[0034] 5 grams of natural flake graphite (80 mesh, 99% carbon content, Qingdao Nanshu Hongda Graphite Products Co., Ltd.), add 4 ml of propanol and 4 ml of water, mix well, then 500 watts ultrasonic for 60 minutes, directly filter and wash 5 times, then dried at 105°C for 1.5 hours, and cooled to below 50°C to obtain pre-expanded graphite;

[0035] The pre-expanded graphite was transferred to the autoclave, 0.1 ml of petroleum ether, 0.2 ml of benzene, 0.2 ml of n-hexane were added, and the autoclave was sealed and intercalated at 150 ° C for 60 minutes, and then cooled to room temperature;

[0036] Open the autoclave cover, transfer the intercalated graphite into a 1000 mL glass beaker in 5 times, and expand under 500 watt microwave power for 40 seconds to obtain the FEG of the present invention;

[0037] Its expansion ratio was 108 times measured by the graduated cylinder method.

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