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Method for preparing spinnable petroleum mesophase pitch

A mesophase pitch and petroleum technology, applied in the field of high-performance pitch-based carbon fiber spinning raw material preparation, can solve the problems of high risk, high cost, and high requirements for reaction equipment

Active Publication Date: 2017-07-07
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the strong corrosiveness of the catalyst used in this method, the requirements for the reaction equipment are very high, and it will bring about the problem of operation protection, so that the industrialization of this kind of asphalt has the disadvantages of high cost and high risk.

Method used

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  • Method for preparing spinnable petroleum mesophase pitch

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Petroleum-based medium-temperature asphalt with the properties shown in Table 1 was used as raw material, and heat-treated in an autoclave at a temperature of 410°C, a pressure of 1 MPa, and a residence time of 5 hours. After the reaction, the reaction product was distilled under reduced pressure at 330° C. and 2000 Pa (absolute pressure) to obtain pitch with a high softening point. The yield and properties of the pitch are shown in Table 2.

[0019] In an autoclave, dissolve one part by weight of high softening point asphalt and three parts by weight tetralin, and carry out hydrogenation treatment at a temperature of 430 ° C, a pressure of 5 MPa, and a time of 120 minutes, and then let it settle for 1 hour to remove After the undesired components, the hydrogenated product was flashed at 400°C under normal pressure to obtain hydrogenated pitch. The yield and properties of the hydrogenated pitch are shown in Table 2.

[0020] The hydrogenated pitch undergoes thermal poly...

Embodiment 2

[0023] The first step is the same as in Example 1.

[0024] In an autoclave, one part by weight of high softening point pitch was dissolved in four parts by weight of tetralin. The reaction conditions were the same as the second step in Example 1. The yield and properties of the hydrogenated pitch obtained are shown in Table 2.

[0025] The conditions of the third step in the implementation case 1 are the same, and the properties and yield of the obtained mesophase pitch are shown in Table 2.

[0026] The obtained mesophase spinning pitch was spun at 348°C with spinning equipment, and carbonized to make carbon fibers. The properties are shown in Table 2.

Embodiment 3

[0028] The first step is the same as in Example 1.

[0029] In an autoclave, one part by weight of high softening point pitch was dissolved in three parts by weight of tetrahydroquinoline. The reaction conditions were the same as the second step in Example 1. The yield and properties of the hydrogenated pitch obtained are shown in Table 2.

[0030] The conditions of the third step in the implementation case 1 are the same, and the properties and yield of the obtained mesophase pitch are shown in Table 2.

[0031] The obtained mesophase spinning pitch was spun at 355°C with spinning equipment, and carbonized to make carbon fibers. The properties are shown in Table 2.

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Abstract

The invention discloses a method for preparing spinnable petroleum mesophase pitch. The preparation process comprises the following steps: carrying out heat treatment and reduced pressure distillation on petroleum medium temperature pitch nearly containing no toluene insoluble and quinoline insoluble, carrying out hydrotreatment in the presence of a hydrogen-donor solvent, and finally carrying out heat treatment to obtain the spinnable petroleum mesophase pitch. The prepared spinnable petroleum mesophase pitch has relatively low softening point, the content of mesophase is high, and the method is suitable for preparing high-performance carbon fibers.

Description

technical field [0001] The invention belongs to the technical field of the preparation method of high-performance pitch-based carbon fiber spinning raw materials, and in particular relates to a preparation method of petroleum-based mesophase pitch. Background technique [0002] Pitch-based carbon fibers can be divided into two categories: one is general-purpose grade, which is prepared from isotropic precursor pitch; the other is high-performance grade, which is prepared from anisotropic mesophase pitch. The key to the preparation of high-performance mesophase carbon fibers is the modulation of mesophase pitch. For high-performance carbon fibers prepared from pitch, the spinning pitch must be a mesophase pitch, that is, an optically anisotropic mesophase as determined by a polarizing microscope, and the spinning pitch must have a suitable softening point. If the Mettler method softening point of pitch exceeds 330°C, its spinning temperature will exceed 360°C. The organic s...

Claims

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Application Information

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IPC IPC(8): C10C3/02C10C3/06D01F9/155
CPCC10C3/02C10C3/06D01F9/155
Inventor 聂毅李佩佩王伟何成友白璐张香平张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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