Preparation method of polyacrylonitrile based three-dimensional macroporous carbon block

A polyacrylonitrile-based, three-dimensional macroporous technology is applied in the preparation/purification of carbon, chemical instruments and methods, carbon compounds, etc. Simple, efficient hole making, low cost effect

Active Publication Date: 2018-08-10
SHANDONG UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

[0009] In order to overcome the above deficiencies, the present invention provides a preparation method of polyacrylonitrile-based three-dimensional macroporous carbon block, which aims to solve the problem of hot pressing of polyacrylonitrile below the decomposition temperature and the problem of polyacrylonitrile-based three-dimensional macroporous carbon blocks in the prior art. The carbon block preparation process is complex, the processing cost is high, the environmental protection is poor, and the pore structure is uncontrollable.

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  • Preparation method of polyacrylonitrile based three-dimensional macroporous carbon block
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  • Preparation method of polyacrylonitrile based three-dimensional macroporous carbon block

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[0039] A method for preparing a polyacrylonitrile-based three-dimensional macroporous carbon block. The process includes three steps of preparing a foaming precursor, preparing a polyacrylonitrile foam, and preparing a polyacrylonitrile-based three-dimensional macroporous carbon block.

[0040] Specific steps are as follows:

[0041] (1) Preparation of foaming precursor: After adding an organic solvent and 8-12wt% polyacrylonitrile into the flask, stir at 55-75°C for 8-24 hours until the polyacrylonitrile is completely dissolved, then pour the solution into the culture In the dish, dry at 60°C for 10-16 hours, and after part of the solvent is evaporated to dryness, the mass ratio of the remaining solvent to polyacrylonitrile should be controlled within the range of 35-55wt%.

[0042] Obtain thin slices and cut them into thin slices with the same size as the cavity of the hot-pressing mold. Take 10-16 slices, heat-press at 140-160°C and 10-20Mpa for 10-20 minutes to obtain bloc...

Embodiment 1

[0052] The process of the preparation method of the polyacrylonitrile-based three-dimensional macroporous carbon block involved in this example includes three steps of preparing a foaming precursor, preparing a polyacrylonitrile foam and preparing a polyacrylonitrile-based three-dimensional macroporous carbon block:

[0053] (1) Preparation of foaming precursor: After adding dimethyl sulfoxide and 10wt% polyacrylonitrile powder into the flask, mechanically stir at 60°C for 10 hours until the polyacrylonitrile is completely dissolved, and then pour the solution into a petri dish , drying at 60°C for 12h (at this time, the mass of the remaining solvent and polyacrylonitrile is about 42wt%) to obtain thin slices and cut them into thin slices with the same size as the cavity of the hot-pressing mold. Take 12 slices and heat through 160°C , 10Mpa hot pressing for 10 minutes to obtain a block sample, and finally punch it into small pieces as a foaming precursor.

[0054] (2) Prepara...

Embodiment 2

[0058] The process of the preparation method of the polyacrylonitrile-based three-dimensional macroporous carbon block involved in this example includes three steps of preparing a foaming precursor, preparing a polyacrylonitrile foam and preparing a polyacrylonitrile-based three-dimensional macroporous carbon block:

[0059] (1) Preparation of foaming precursor: After adding dimethyl sulfoxide and 10wt% polyacrylonitrile powder into the flask, mechanically stir at 60°C for 10 hours until the polyacrylonitrile is completely dissolved, and then pour the solution into a petri dish , drying at 60°C for 12h (at this time, the mass of the remaining solvent and polyacrylonitrile is about 42wt%) to obtain thin slices and cut them into thin slices with the same size as the cavity of the hot-pressing mold. Take 12 slices and heat through 160°C , 10Mpa hot pressing for 10 minutes to obtain a block sample, and finally punch it into small pieces as a foaming precursor.

[0060] (2) Prepara...

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Abstract

The invention provides a preparation method of a polyacrylonitrile based three-dimensional macroporous carbon block. According to the operational path, polyacrylonitrile is completely dissolved into an organic solvent, then, drying, cutting, hot pressing and blanking are performed to obtain a foaming precursor, then, a supercritical carbon dioxide batch foaming method is adopted for preparing polyacrylonitrile foams with controllable foam structures, and finally pre-oxidation and carbonization are performed to obtain the polyacrylonitrile based three-dimensional macroporous carbon block. The preparation method of the polyacrylonitrile based three-dimensional macroporous carbon block is simple, easy to control, environmentally friendly, low in cost and capable of achieving large-scale production. The prepared polyacrylonitrile based three-dimensional macroporous carbon block has the advantages that the porous structure is uniform and controllable and has the good electric conductivity and the wide application prospect. The method is simplified in steps, convenient to implement and good in practicability.

Description

technical field [0001] The invention relates to a method for preparing porous carbon, in particular to a method for preparing a polyacrylonitrile-based three-dimensional macroporous carbon block. Background technique [0002] Porous carbon materials have the advantages of rich pore structure, large specific surface, low density, excellent chemical stability and electrical conductivity, and low production cost, and are widely used in fuel cell electrode materials, electric double layer capacitors and lithium-ion batteries. Electrode materials, catalyst carriers, electromagnetic shielding materials, water purification and filtration, sound-absorbing materials and other fields. Pore ​​structure is a key factor affecting the application of porous carbon materials. Among them, the controllable preparation of macropores is the key to obtain 3D monolithic carbon blocks. However, most of the currently prepared macroporous carbon materials have problems such as extremely uneven por...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01B32/05C08J9/122C08J2201/034C08J2203/08C08J2333/20C08J5/18C01B32/318C01B32/336
Inventor 赵国群龚洁
Owner SHANDONG UNIV
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