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Method for preparing general type coal series asphalt with spinnability by solvent extraction and oxidative thermopolymerization

A technology of spinnability and thermal polymerization, applied in processing tar pitch/petroleum pitch/natural pitch by selective extraction, processing tar pitch/petroleum pitch/natural pitch by distillation, processing tar pitch/petroleum pitch/natural pitch by chemical methods and other directions, it can solve the problems of low softening point, complex process and harsh conditions, and achieve the effects of narrow molecular weight distribution, high product yield and high softening point

Inactive Publication Date: 2012-04-04
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is more complicated, the conditions are harsh, and the yield is low; Chinese Patent Publication (Announcement) No. CN86103441A has reported a "preparation method of coal tar pitch carbon fiber raw material", and the method is to add coal tar heavy fraction in coal tar pitch Post-heat treatment, filtration and flash evaporation to obtain spinnable pitch, the obtained spinnable pitch has wide molecular weight distribution, low softening point and poor spinnability

Method used

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  • Method for preparing general type coal series asphalt with spinnability by solvent extraction and oxidative thermopolymerization
  • Method for preparing general type coal series asphalt with spinnability by solvent extraction and oxidative thermopolymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The first step: put 600g of coal tar soft pitch into a 1L three-necked bottle, the softening point of coal tar soft pitch is 22°C; the mass percentage of coking value is 32.2%; the mass percentage of quinoline insoluble matter is 2.95%; the mass percentage of toluene insoluble matter is 11.51% %, add a total of 480g of kerosene and heavy wash oil mixed solvent with a mass ratio of 0.8:1, heat and stir at 130°C for 30min, then stand still for 75min, separate the extract phase, and distill off the solvent to obtain refined pitch, the yield mass percentage is 50%, and the indicators are shown in Table 1.

[0015] The second step: the refined asphalt prepared in the first step is subjected to oxidative thermal polymerization, the reaction temperature is 260°C, the reaction time is 5h, and the air flow rate is 0.16m 3 / h to obtain oxidized pitch, the mass percentage yield is 92%.

[0016] The third step: the oxidized pitch obtained in the second step is subjected to vacuum ...

Embodiment 2

[0020] The first step: it is exactly the same as the first step in Example 1, except that 540 g of paraffin oil and light wash oil mixed solvent are added with a mass ratio of 0.75: 1.

[0021] The second step: the refined asphalt prepared in the first step is subjected to oxidative thermal polymerization, the reaction temperature is 260°C, the reaction time is 6h, and the air flow rate is 0.16m 3 / h to get oxidized pitch.

[0022] The third step: exactly the same as the third step in Example 1.

[0023] The fourth step; it is exactly the same as the fourth step in the implementation case 1.

[0024] The obtained spinnable pitch is evaluated by spinning equipment, and has good spinnability. After stabilization and carbonization treatment, carbon fibers are made, and the indicators are shown in Table 1 and Table 2.

Embodiment 3

[0026] The first step: It is exactly the same as the first step in the implementation case 1, except that a total of 450 g of diesel oil and heavy washing oil mixed solvent with a mass ratio of 0.85: 1 are added.

[0027] The second step: oxidative thermal polymerization of refined pitch, reaction temperature 260°C, reaction time 7h, air flow 0.16m 3 / h, to get oxidized asphalt.

[0028] Step 3: Exactly the same as Step 3 in Implementation Case 1.

[0029] Step 4: Exactly the same as Step 4 in Implementation Case 1.

[0030] The obtained spinnable pitch was evaluated by spinning, and the spinnability was good. After stabilization and carbonization treatment, carbon fibers are made, and the indicators are shown in Table 1 and Table 2.

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Abstract

The invention discloses a method for preparing general type coal series asphalt with spinnability by solvent extraction and oxidative thermopolymerization. The method comprises the following steps: tasking coal tar soft asphalt as a raw material, extracting and separating by using a mixed solvent of aliphatic hydrocarbon and aromatic hydrocarbon; taking the obtained refined asphalt as a raw material, carrying out oxidative thermopolymerization in a stainless steel reaction vessel, performing flash evaporation after finishing the oxidative thermopolymerization to obtain the general type coal series asphalt with spinnability. According to the invention, a solvent extraction method is used for removing a first quinoline insoluble substance of the asphalt, a process of oxidative thermopolymerization and flash evaporation is used to obtain the product, so that the disadvantages of wide molecular weight distribution of asphalt during the heat treatment process and high secondary quinoline insoluble substance content can be overcome. The general type coal series asphalt with spinnability has optical isotropy under the spinning temperature, has the characteristics of narrow molecular weight distribution, high softening point, good spinnability and high product yield, and is suitable for preparing general carbon fiber.

Description

technical field [0001] The invention relates to a method for preparing general-purpose spinnable pitch by using coal tar soft pitch as raw material. In particular, a method for preparing general-purpose coal-based spinnable asphalt by solvent extraction and oxidative thermal polymerization Background technique [0002] Carbon fiber is a new type of carbon material that emerged in the 1960s. It has the advantages of high temperature resistance, corrosion resistance, small thermal expansion coefficient, good dimensional stability, high specific strength and high specific modulus, and is an ideal functional material and Structural materials. It was originally developed as a material demand for aerospace industry and military aircraft. Now it has been widely used in commercial, civil aviation, cultural and sports, industry, transportation and other fields, and has broad application prospects. The wide application of high-performance carbon fiber composite materials has furthe...

Claims

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Application Information

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IPC IPC(8): C10C3/02C10C3/08C10C3/06D01F9/145
Inventor 赵雪飞齐涛赖仕全高丽娟
Owner UNIV OF SCI & TECH LIAONING
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