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Mesophase pitch prepared from heavy oil and method thereof

A technology of mesophase pitch and heavy oil, which is applied in the processing of tar pitch/petroleum pitch/natural pitch, chemical processing of tar pitch/petroleum pitch/natural pitch, petroleum industry, etc., and can solve the problems affecting the quality of carbon fiber. , easy residue and other problems, to achieve the effect of good spinnability, low price and low saturated content

Pending Publication Date: 2022-05-27
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the method ZrO 2 It is easy to remain in the mesophase pitch product, which will affect the further improvement of the subsequent carbon fiber quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Using catalytic cracking oil slurry as raw material and using inorganic membrane filtration to obtain clarified oil, wherein the yield of clarified oil is 90wt.%, the ash content removal rate is 95%, and the ash content is 30ppm.

[0030] γ-neutral alumina was activated at 490°C for 6h, cooled to 20°C, added with 1.5 wt.% deionized water, mixed evenly, and then added to the chromatographic column. Dilute the clarified oil with a small amount of benzene and add it to the chromatographic column. Use benzene-ethanol with a volume ratio of 8:2 as the mobile phase to flush the stationary phase; continue to use benzene-ethanol with a volume ratio of 2:8 as the mobile phase to flush the stationary phase. Rinse dosage 1mL / g Al 2 O 3, the elution phase was obtained, and the whole process was carried out at a constant temperature of 50 °C. The aromatic-rich component was obtained by taking the elution phase and evaporated the solvent, and the yield of the aromatic-rich componen...

Embodiment 2

[0034] Using catalytic cracking oil slurry as raw material and using inorganic membrane filtration to obtain clarified oil, wherein the yield of clarified oil is 90wt.%, the ash content removal rate is 95%, and the ash content is 30ppm.

[0035] The stationary phase in the column is γ-neutral alumina, activated at 490°C for 6h, cooled to 20°C, added with 1.5wt.% deionized water, mixed evenly, and then added to the chromatographic column. Dilute the clarified oil with a small amount of benzene and add it to the chromatographic column. Use n-heptane as the mobile phase to flush the stationary phase; continue to use toluene as the mobile phase to flush the stationary phase, and the amount of flushing agent is 1mL / g Al 2 O 3 , the elution phase was obtained, and the whole process was carried out at a constant temperature of 50 °C. The aromatic-rich component was obtained after the elution phase was evaporated to remove the solvent, and the yield of the aromatic-rich component was...

Embodiment 3

[0039] Taking medium and low temperature coal tar as raw material, adding 1 wt.% of market-oriented settling aids, mixing uniformly, and then settling at 90 °C for 24 hours, and taking the upper clarified oil, the yield of clarified oil was 90 wt.%, and the ash removal rate was 90 wt.%. 90%, the ash content is 90ppm.

[0040] The stationary phase in the column is γ-neutral alumina, activated at 450°C for 6h, cooled to 20°C, added with 1.5wt.% deionized water, mixed evenly, and then added to the chromatographic column. Dilute the clarified oil with a small amount of benzene and add it to the chromatographic column. Use benzene-ethanol with a volume ratio of 10:0 as the mobile phase to flush the stationary phase; continue to use benzene-ethanol with a volume ratio of 9:1 as the mobile phase to flush the stationary phase. Rinse dosage 1mL / g Al 2 O 3 , the elution phase was obtained, and the whole process was carried out at a constant temperature of 50 °C. The aromatic-rich com...

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Abstract

The invention discloses mesophase pitch prepared from heavy oil and a method thereof. The method comprises the following steps: selecting the heavy oil as a raw material; carrying out deliming treatment on the raw materials to obtain clarified oil; the clarified oil is separated by adopting a solid-liquid adsorption method, the polarity of an aluminum oxide stationary phase and the washing strength of a mobile phase are respectively adjusted according to different raw materials, a first mobile phase and a second mobile phase are subjected to gradient elution to obtain an aromatic-rich component, and the first mobile phase and the second mobile phase adopt a mixed or single solvent, preferably a mixed solvent; and performing liquid-phase carbonization on the aromatic-rich component in a high-pressure reaction kettle to obtain the mesophase pitch. The preparation method provided by the invention has no harsh requirements on equipment, and the finally obtained mesophase pitch has good spinnability.

Description

technical field [0001] The invention relates to a method for preparing mesophase pitch, in particular to a method for preparing mesophase pitch and pitch-based carbon fiber by heavy oil ash removal-aromatic enrichment-thermal polycondensation, belonging to the technical field of petroleum deep processing. Background technique [0002] Mesophase pitch is a nematic liquid crystal substance composed of flat macromolecules or rod-shaped molecules, which is obtained by thermal polycondensation and catalytic polycondensation using high molecular polymers, heavy oil, petroleum and coal pitch as raw materials. It has easy graphitization and can prepare various new high-quality carbon materials. These carbon materials play a huge role in defense industry, high-end technology, aerospace, civil industry and other fields. Among them, the mesophase pitch with high mesophase content has spinnability and sufficient microscopic order, and can obtain pitch-based carbon fibers with high-qual...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/00C10C3/02
CPCC10C3/00C10C3/02
Inventor 何盛宝刘东张博娄斌王路海于庆生张浩然殷长龙刘银东张智琛
Owner PETROCHINA CO LTD
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