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Preparation method of general purpose pitch-based carbon fiber

A pitch-based carbon fiber, general-purpose technology, applied in the chemical characteristics of fibers, the processing of tar pitch/petroleum pitch/natural pitch, and the processing of tar pitch/petroleum pitch/natural pitch by distillation, etc. Melt spinnability, low spinnability and other problems, to achieve the effect of good quality, good continuity and less environmental pollution

Inactive Publication Date: 2013-04-03
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, the polycondensation reaction method is usually used to effectively increase the degree of condensation of asphalt polycyclic aromatic hydrocarbons. However, when the anisotropy formed by excessive polycondensation during the liquid phase carbonization process, that is, the mesophase crystallites and the mother liquor isotropic asphalt coexist, The spinnability of the melt is reduced; the other is to treat by oxidative crosslinking, that is, to conduct oxidation reaction after heat treatment of pitch to increase the degree of polycondensation of pitch, but the spinnability of this method is also very low, and the spinning Difficult to meet the needs of industrial production

Method used

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  • Preparation method of general purpose pitch-based carbon fiber
  • Preparation method of general purpose pitch-based carbon fiber
  • Preparation method of general purpose pitch-based carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Taking 150g of raw coal tar soft pitch as an example, the method for preparing general-purpose pitch-based carbon fibers consists of the following steps:

[0034] (1) heat treatment

[0035] Take 150g of coal tar soft asphalt with a softening point of 59°C, put it in a high-pressure reactor, and heat it to 390°C under the protection of nitrogen. The nitrogen flow rate is 85mL / min, the stirring speed is 350r / min, stirring, and reacting for 60min.

[0036] (2) Thermal filtration

[0037] Let the reaction product of step (1) stand for 30 minutes, the upper bitumen and the coke-forming components are separated, and the upper bitumen is poured into a hot filter kettle, the filter screen of the hot filter kettle is 600 mesh, the temperature is 360°C, and the pressure is 0.5MPa , to remove the coke-forming components in the upper bitumen.

[0038] (3) Distillation under reduced pressure

[0039] Put the bitumen from which the coke components were removed in step (2) in a hi...

Embodiment 2

[0049] Taking 150g of raw coal tar soft pitch as an example, the method for preparing general-purpose pitch-based carbon fibers consists of the following steps:

[0050] (1) heat treatment

[0051] Take 150g of coal tar soft pitch with a softening point of 59°C, put it in a high-pressure reactor, and heat it to 380°C under the protection of nitrogen, with a nitrogen flow rate of 80mL / min, a stirring speed of 300r / min, stirring, and reacting for 80min.

[0052] (2) Thermal filtration

[0053] Let the reaction product of step (1) stand for 15 minutes, the upper bitumen and the coke-forming components are separated, and the upper bitumen is poured into a hot filter kettle, the filter screen of the hot filter kettle is 400 mesh, the temperature is 350°C, and the pressure is 0.8MPa , to remove the coke-forming components in the upper bitumen.

[0054] (3) Distillation under reduced pressure

[0055] Put the bitumen from which the coke components were removed in step (2) in a hig...

Embodiment 3

[0065] Taking 150g of raw coal tar soft pitch as an example, the method for preparing general-purpose pitch-based carbon fibers consists of the following steps:

[0066] (1) heat treatment

[0067] Take 150g of coal tar soft pitch with a softening point of 59°C, put it in a high-pressure reactor, and heat it to 400°C under the protection of nitrogen, with a nitrogen flow rate of 90mL / min, a stirring speed of 400r / min, stirring, and reacting for 50min.

[0068] (2) Thermal filtration

[0069] Let the reaction product of step (1) stand for 40 minutes, the upper bitumen and the coke-forming components are separated, and the upper bitumen is poured into the hot filter kettle, the filter screen of the hot filter kettle is 400 mesh, the temperature is 390°C, and the pressure is 0.1MPa , to remove the coke-forming components in the upper bitumen.

[0070] (3) Distillation under reduced pressure

[0071] Put the bitumen from which the coke components were removed in step (2) in a h...

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Abstract

The invention relates to a preparation method of a general purpose pitch-based carbon fiber. The preparation method has the beneficial effects that isotropic pitch with high softening point and excellent spinnability is obtained through the comprehensive treatment technologies such as heat treatment, heat filtration, reduced pressure distillation, oxidation treatment and modification with an additive and then the general purpose pitch-based carbon fiber is prepared through melt spinning, non-melting treatment and carbonization treatment; the pitch blended by the method is low in heteroatom content, narrow in molecular weight distribution and high in carbon content, contains defined amount of short alkyl side chains and can solve the technical problems that the melt spinning materials are brittle and are not easy to operate and non-melting treatment costs long time; the carbon fiber prepared by the method has good quality, high strength and good continuity; and the preparation method is simple in process, mild in reaction conditions and low in environmental pollution and is applicable to industrial production.

Description

technical field [0001] The invention relates to the technical field of carbon fiber preparation, in particular to a preparation method of general-grade pitch-based carbon fiber. Background technique [0002] Pitch-based carbon fiber refers to a type of carbon fiber prepared from materials rich in condensed aromatic hydrocarbons such as pitch, through polymerization, spinning, non-melting, and carbonization. Pitch carbon fiber, the former is prepared from isotropic pitch, also known as isotropic pitch-grade carbon fiber, and the latter is prepared from mesophase pitch, so it is also called mesophase pitch-grade carbon fiber. Polyvinyl chloride pyrolysis pitch, lignin pitch, coal tar pitch, and petroleum residue pitch can be made into carbon fibers after spinning, non-melting, and carbonization treatments. Among them, the precursor raw materials of pitch-based carbon fibers are cheap and abundant, and the carbonization yield is higher than that of polyacrylonitrile fibers, wh...

Claims

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Application Information

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IPC IPC(8): D01F9/15D01F1/10D01D5/08D01D5/12C10C3/00C10C3/02C10C3/04C10C3/06
Inventor 刘春玲董文生李军王宏斌付凤奇
Owner SHAANXI NORMAL UNIV
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