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Device and method for preparing mesocarbon microbeads from medium-temperature coal pitch

A technology of mesophase carbon microspheres and coal tar pitch, which is applied in the preparation/purification of carbon, etc., can solve the problems of high production cost, easy fusion of small balls, complicated process, etc., and achieve improved product performance level and surface smoothness , separation and clean effect

Inactive Publication Date: 2018-07-06
王强 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for preparing mesophase carbon microspheres from coal tar pitch mainly include direct method and indirect method. The direct method is the direct thermal condensation polymerization method. Production, the disadvantage is that the small balls are easy to melt, and the size distribution is wide, the shape and size are not uniform, and the yield is low. If the yield is increased by retaining the primary quinoline insoluble in the system or adding additives, these substances will affect the intermediate production. Final properties of phase carbon microspheres
The indirect method includes the emulsification method and the suspension method. The mesophase carbon microspheres prepared by the indirect method have a narrow size distribution, low internal light component content, and less impurities. The disadvantage is that the process is complicated and cumbersome. Melting processing, and there are difficulties in the preparation process, and the industrialization prospect is bleak
[0004] At present, the method commonly used in industry to prepare mesophase carbon microspheres is the direct thermal polycondensation method, but in the industrial production process of coal tar pitch-based mesophase carbon microspheres, there are generally complicated procedures, difficult operation, low efficiency, and low yield. , The phenomenon of high production cost, the unclean separation of carbon microspheres leads to rough surface of the product and poor quality

Method used

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  • Device and method for preparing mesocarbon microbeads from medium-temperature coal pitch

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Effect test

Embodiment 1

[0034] Such as figure 1 As shown, the device for preparing mesophase carbon microspheres from medium-temperature coal tar pitch of the present invention includes a reaction kettle 3, a washing kettle 4, a filter kettle 5, a drying kettle 9, an oxidation kettle 11 and a distillation tower 10. The upper part of the reaction kettle 3 is provided with a mass flow rate Meter 1 and sampler 2, the bottom of reaction kettle 3 is connected with the top of washing kettle 4 through pipelines, the lower part of washing kettle 4 is connected with the lower part of filter kettle 5 through pipelines, and a filter disc 8 is arranged in filter kettle 5, and there is a filter screen on filter disc 8 6. There are nitrogen inlet pipes on both sides of the middle of the filter kettle 5, which are separated by nitrogen pressure filtration. The filter kettle 5 is also equipped with an "L"-shaped hollow tube 7, and one end of the hollow tube 7 passes through the filter disc 8 and the filter screen 6 ...

Embodiment 2

[0051] The method for preparing mesophase carbon microspheres from medium-temperature coal tar pitch is completed in the following steps:

[0052] a. Preparation of raw coal tar pitch: mix the secondary coal tar pitch after extracting the mesophase carbon microspheres with the purchased medium-temperature coal tar pitch in a mass ratio of 1:3 to obtain the raw coal tar pitch with a quinoline insoluble content of 4.6%;

[0053] b. Thermal polycondensation reaction: The raw material coal tar pitch is measured by the mass flow meter 1 and then added to the reactor 3 for thermal polycondensation reaction. After heating to 400°C, the particles of the mesophase carbon microspheres are sampled by the sampler 2 every 0.5 hours When the particle size reaches the target particle size, the reaction is stopped to obtain the mother liquor of carbon microspheres. The reaction parameters are as follows: Stirring rate: 85r / min, heating rate: 55°C / h, reaction temperature: 455°C, constant temper...

Embodiment 3

[0065] The method for preparing mesophase carbon microspheres from medium-temperature coal tar pitch is completed in the following steps:

[0066] a. Preparation of raw coal tar pitch: mix the secondary coal tar pitch after extracting mesophase carbon microspheres with the purchased medium-temperature coal tar pitch at a mass ratio of 1:5 to obtain the raw coal tar pitch with a content of quinoline insolubles of 6%;

[0067] b. Thermal polycondensation reaction: The raw material coal tar pitch is measured by the mass flow meter 1 and then added to the reactor 3 for thermal polycondensation reaction. After heating to 400°C, the particles of the mesophase carbon microspheres are sampled by the sampler 2 every 0.5 hours When the particle size reaches the target particle size, the reaction is stopped to obtain the mother liquid of carbon microspheres. The reaction parameters are as follows: stirring rate: 100r / min, heating rate: 60°C / h, reaction temperature: 460°C, constant tempera...

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Abstract

The invention provides a device and method for preparing mesocarbon microbeads from medium-temperature coal pitch, and belongs to the field of high-performance coal pitch-based carbon materials. The device for preparing the mesocarbon microbeads from the medium-temperature coal pitch comprises a reaction kettle, a washing kettle, a filter kettle and a drying kettle, and further comprises an oxidation kettle and a distillation tower, and the upper part of the reaction kettle is provided with a mass flow meter and a sampler; and the method for preparing the mesocarbon microbeads from the medium-temperature coal pitch includes the processes of raw material coal pitch preparation, a thermal polycondensation reaction, washing of a reaction product, separation, drying, oxidation, and recovery ofa washing solvent and secondary coal pitch. The method provided by the invention has the advantages that the process is simple and easy to operate and the efficiency is high, the product yield is high, the particle sizes are uniform, the surface is smooth and the performance is excellent.

Description

technical field [0001] The invention belongs to the field of coal tar pitch-based carbon materials, and in particular relates to a device and method for preparing mesophase carbon microspheres from medium-temperature coal tar pitch. Background technique [0002] When the asphalt compound is heat-treated, a thermal condensation reaction occurs to form anisotropic mesophase spheres, and the micron-scale spherical carbon material formed by separating the mesophase spheres from the asphalt matrix is ​​called mesophase carbon microspheres. Mesophase carbon microspheres are a new type of functional material, which is a discotic nematic liquid crystal structure formed during the carbonization of polycyclic aromatic compounds. It has good chemical stability, high strength, high specific surface area, and high adsorption. Capability, easy graphitization, good thermal stability, and excellent electrical and thermal conductivity, etc., are high-quality precursors for the preparation of...

Claims

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Application Information

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IPC IPC(8): C01B32/05
Inventor 王强郭爱玲
Owner 王强
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