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Preparation method of soluble mesophase pitch

A mesophase pitch, soluble technology, applied in the processing of tar pitch/petroleum pitch/natural pitch, processing tar pitch/petroleum pitch/natural pitch by distillation, processing tar pitch/petroleum pitch/natural pitch by chemical methods, etc. It can solve problems such as difficulties in the industrialization process, high equipment requirements, and complex processes, and achieve the effects of high controllability of molecular structure, low viscosity of the system, and high solubility

Inactive Publication Date: 2014-05-28
SICHUAN CHUANGYUE CARBON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention mainly aims at the existing problems of complex process, high requirements for equipment, high cost and difficult industrialization process in the existing method for preparing mesophase pitch, and provides a method with simple process, mild reaction conditions, low requirements for equipment, low cost and suitable Preparation method of industrially produced soluble mesophase pitch

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Take 100 parts of ethylene tar with an ash content of 0.003%, H / C molar ratio of 0.95, and 100% soluble toluene into an ordinary high-pressure reactor, pressurize to 6MPa in an inert atmosphere, heat-treat at 420°C for 5hr, and Continue to stir, then lower to 250°C, release the pressure, keep stirring, and blow nitrogen gas for 1hr to remove the light fraction, collect the heavy fraction, that is, the heavy fraction pitch, the softening point of the heavy fraction pitch is 120°C, Pyridine is completely soluble, and the toluene soluble component is 76%;

[0024] (2) Heat the heavy component pitch to 370°C in an inert atmosphere, and pass 100 parts of raw material ethylene tar into the heavy component pitch four times, stir evenly, and react for 3 hours under normal pressure to obtain intermediate pitch;

[0025] (3) Reduce the temperature of the intermediate bitumen to 340°C, reduce the pressure to below -0.09MPa for 30 minutes, remove light components, and obtain a ...

Embodiment 2

[0028] (1) Take ash content of 0%, H / C molar ratio of 0.95, 50 parts of toluene soluble 100% ethylene tar pitch, softening point of 78°C, complete pyridine dissolution, toluene soluble components of 76%, ash content of 0.005% 50 parts of isotropic refined coal tar pitch, mixed and put into ordinary high-pressure reactor, pressurized to 6MPa in an inert atmosphere, heat-treated at 400°C for 5hrs, and kept stirring, then lowered to 250°C, released pressure, kept stirring, and Nitrogen was blown and purged for 2.5 hours to remove the light fraction and collect the heavy fraction, namely the heavy fraction pitch. The softening point of the heavy fraction pitch obtained was 130°C, the pyridine was completely soluble, and the toluene soluble fraction was 74%;

[0029] (2) Heat the heavy component asphalt to 370°C in an inert atmosphere, take 50 parts of methyl naphthalene with a softening point of 60°C and a H / C value of 0.95, add it to the heavy component asphalt, stir evenly, and r...

Embodiment 3

[0033](1) Take 50 parts of isotropic refined coal tar pitch with a softening point of 95°C, complete pyridine dissolution, 74% toluene soluble components, and 0.005% ash content, and put it into an ordinary high-pressure reactor, pressurize to 6MPa in a nitrogen atmosphere, and raise the temperature Heat treatment at 370°C for 2 hours, and keep stirring, then lower to 250°C, release pressure, keep stirring, and blow nitrogen gas for 2.5 hours to remove the light fraction, collect the heavy fraction, that is, the heavy fraction asphalt, and obtain the heavy fraction The softening point of asphalt is 130°C, the pyridine insoluble component is 14%, and the toluene insoluble component is 27%;

[0034] (2) Heat the heavy component pitch to 340°C in an inert atmosphere, take 30 parts of durene and add it to the heavy component pitch, stir evenly, and react for 5 hours under a pressure of 1.5MPa to obtain intermediate pitch;

[0035] (3) Reduce the temperature of the intermediate bit...

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Abstract

The invention belongs to the technical field of a preparation method of spinning raw materials of high-performance pitch-based carbon fibers, and particularly relates to a preparation method of soluble mesophase pitch, which mainly solves the problems of the existing mesophase pitch preparation method that the process is complicated, requirements on the equipment are high, the cost is high, the industrialization process is difficult and the like. The invention adopts the technical scheme that the preparation method of the soluble mesophase pitch comprises the following steps of (1) thermally treating raw material pitch or ethylene bottom oil with a low softening point in an inert atmosphere, then distilling the material in a short distance or flashing the material, removing light ends, and collecting heavy fraction, i.e. heavy end pitch; (2) preparing the heavy enbd pitch into mesophase pitch; and (3) cooling the mesophase pitch to 320DEG C to 400DEG C, removing internal light ends, and collecting the heavy fraction, i.e. the mesophase pitch. The preparation method has the advantages of simplicity in process, moderate in reaction condition, low equipment requirement, low cost and adaptability to industrialized production.

Description

technical field [0001] The invention belongs to the technical field of preparation method of high-performance pitch carbon fiber spinning raw material, and in particular relates to a preparation method of soluble mesophase pitch. Background technique [0002] Mesophase pitch is the precursor raw material for preparing high-performance pitch-based carbon fiber, needle coke, C / C composite and other advanced carbon materials. In order to produce high-performance carbon materials, pitches are generally required to have the characteristics of less heteroatoms, low ash content, high aromaticity, low condensation degree, orderly molecular arrangement, high carbon yield, and good fluidity. The formation of a better mesophase structure also requires better planarity, which is the basis of the mesophase structure; this requires that the aromatic compound has a certain molecular weight to provide enough van der Waals force to align the molecules to form mesophase spherulites ; A lower...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/00C10C3/06C10C3/02C10C3/08C10C1/16C10C1/19C10C1/20D01F9/145
Inventor 伍孝永学健余洋
Owner SICHUAN CHUANGYUE CARBON MATERIAL
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