Process for preparing spinnable pitch

A technology for refining asphalt and asphalt, which is applied in the direction of processing tar pitch/petroleum pitch/natural pitch by distillation and processing tar pitch/petroleum pitch/natural pitch by selective extraction, which can solve air pollution, high production cost, high operating temperature, etc. problems, to achieve the effect of reducing production difficulty and cost, reducing operation difficulty and cost, and making the separation process simple and easy

Active Publication Date: 2021-05-11
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the main problem of this method is: a large amount of tail gas will be produced during the oxidation process, which contains a large amount of carcinogens, nitrides, etc., causing serious air pollution; the distribution of air or oxygen in the reactor is not easy to achieve uniformity, resulting in uneven reaction. , the softening point is uneven; the air concentration in some areas of the reactor is too high, resulting in excessive temperature, excessive oxidation, and the appearance of carbon black-like substances and intermediate solid substances, which directly affect the spinning effect
The other is distillation, which relies entirely on high-vacuum molecular distillation to remove light components, thereby increasing the softening point of asphalt. The required operating temperature is very high and the vacuum degree is also extremely high, such as an absolute pressure of 120Pa or lower. , the required equipment investment is very large, which is very difficult to implement in industry, the production cost is high, and it is easy to produce secondary QI
In addition, there are also literatures that use lower operating temperatures, but only spinnable pitch with a very low softening point can be produced.
[0004] In general, for general-purpose pitch-based carbon fibers, low QI and high softening point are a pair of insoluble contradictions, which restrict the development of pitch-based carbon fibers
Due to the above reasons, the quality of domestic pitch-based carbon fiber products is not high, and there are few industrialized ones.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In 200g refined asphalt (110 ℃ of softening points, QI=0.08%), add the mixed solvent (mass ratio of straight-run gasoline and methyl naphthalene oil is 1: 0.3) that adds 400g by straight run gasoline and methyl naphthalene oil, in Stir and mix at 150° C. for 2.0 h, then stand still for 0.5 h, separate and remove the supernatant, and the obtained lower heavy phase has fluidity (at 150° C., viscosity is 300 mPa·s). The lower heavy phase was distilled at 350° C. and 1000 Pa to remove the solvent to obtain 80 g of spinnable pitch. The softening point of the spinnable pitch is 240°C, QI=0.5%.

[0039] The spinnable pitch was spun at 345° C. and 0.016 MPa, the line speed was 450 m / min, the spinning duration was 15 minutes, and the filament diameter was 20 μm.

Embodiment 2

[0041]Add 600g of a mixed solvent of kerosene (distillation range 150-210°C, purchased from Beijing Tianyijingren Petrochemical Company) and methyl naphthalene oil to 200g of refined pitch (softening point 130°C, QI=0.06%) (The mass ratio of kerosene to methylnaphthalene oil is 1:0.1), stirred and mixed at 180°C for 1.0h, then left to stand for 0.5h, separated and removed the supernatant, and the obtained lower heavy phase had fluidity (180°C, viscosity is 260mPa·s). The lower heavy phase was distilled at 330° C. and 310 Pa to remove the solvent to obtain 90 g of spinnable pitch. The softening point of the spinnable pitch is 260°C, QI=0.7%.

[0042] The spinnable pitch was spun at 370° C. and 0.016 MPa, the line speed was 400 m / min, the spinning duration was 13 minutes, and the filament diameter was 18 μm.

Embodiment 3

[0044] In 200g refined asphalt (softening point 120 ℃, QI=0.05%), add 200g mixed solvents (the mass ratio of kerosene and methylnaphthalene oil is 1: 0.8) that is made up of kerosene (with embodiment 2) and methylnaphthalene oil , stirred and mixed at 180° C. for 1.5 h, then stood still for 0.5 h, separated and removed the supernatant, and the obtained lower heavy phase had fluidity (180° C., viscosity 100 mPa·s). The lower heavy phase was distilled at 300° C. and 500 Pa to remove the solvent to obtain 75 g of spinnable pitch. The softening point of the spinnable pitch is 230°C, QI=0.5%.

[0045] The spinnable pitch was spun at 330° C. and 0.015 MPa, the line speed was 420 m / min, the spinning duration was 17 minutes, and the filament diameter was 15 μm.

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Abstract

The invention relates to the field of pitch-based carbon fibers, and discloses a method for preparing spinnable pitch. The method includes: (1) extracting refined pitch with a mixed solvent at a temperature of 150-180°C to obtain a supernatant liquid and a lower heavy phase; Wherein, the mixed solvent is a mixture containing petroleum products and methylnaphthalene oil, the distillation range of the petroleum product is within 150~210°C, and the distillation range of the methylnaphthalene oil is within 230~260°C; The mass ratio of the petroleum product and the methyl naphthalene oil is 1: (0.1~0.8); the mass ratio of the refined asphalt and the mixed solvent is 1: (1~3); (2) the lower layer is weighed The phase is distilled to remove the mixed solvent to obtain spinnable pitch. The method of the invention can change the existing problems such as low softening point and high QI of the spinnable pitch, high vacuum degree requirement in the production process, large equipment investment and high product cost.

Description

technical field [0001] The invention relates to the field of pitch-based carbon fibers, in particular to a method for preparing spinnable pitch. 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 preparation method of general-purpose pitch-based carbon fiber usually includes, using isotropic spinnable pitch as raw material, after melt-spinning, pre-oxidation, and carbonization, to obtain general-purpose pitch-based carbon fiber. Among them, the most basic conditions for the preparation of general-purpose pitch-based carbon fibers are that the softening point of the spinnable pitch needs to be increased to about 250°C, and the QI (quinoline insoluble) content is <1.0%. [0003] At present, there are two main methods to increase the softening point of asphalt, one is ox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/08C10C3/06
CPCC10C3/06C10C3/08
Inventor 熊杰明宋以常李佩佩马文明李海军何启军倪前银
Owner CHINA PETROLEUM & CHEM CORP
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