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A method for preparing general-purpose pitch-based carbon fiber from coal liquefaction residue

A pitch-based carbon fiber and coal liquefaction residue technology, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, can solve the problems of complex and cumbersome process flow, unclear service life, large amount of solvent usage, etc., and achieve simple preparation process and spinnable The effect of low asphalt ash content and improvement of softening point

Active Publication Date: 2022-05-06
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the separation efficiency of the above technology, at least two solvents are used for extraction in the process. The amount of solvent used is large, and the entire process is complicated and cumbersome. Moreover, most of the extraction solvents currently used are chemical products with high value, and coal tar 1. When the circulating solvent oil is used as the extraction agent, the extraction efficiency is low and the solvent separation is difficult; although the ionic liquid as the extraction liquid shows the advantages of high selectivity and easy separation, the cost is relatively high and the service life is not clear

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Sedimentation and separation

[0035] Add 1,000g of coal liquefaction residue, 2,000g of extractant, and 0.1g of polyferric sulfate into the settling tank. The extractant is a mixture of n-heptane and phenol oil with a mass ratio of 1:0.5. Stir and mix at 250°C for 2h, and then Settle at this temperature for 3 hours. After the settling is finished, the upper oil slurry that accounts for 90% of the volume is taken out.

[0036] 2. Vacuum filtration

[0037] Put the upper oil slurry obtained in step 1 in a magnetically stirred reactor, feed nitrogen gas at a flow rate of 20mL / min, turn on the magnetic stirrer, and perform suction filtration under constant temperature and reduced pressure for 10min at a pressure of -0.08MPa and a temperature of 330°C. The extracted extractant is recycled.

[0038] 3. Oxidative polycondensation reaction

[0039] After vacuum filtration, replace the nitrogen with air with a flow rate of 100mL / min, continue to stir at the same temperat...

Embodiment 2

[0047] 1. Sedimentation and separation

[0048] Add 1000g of coal liquefaction residue, 2000g of extractant, and 0.5g of polyferric sulfate into the settling tank. The extractant is a mixture of kerosene and anthracene oil with a mass ratio of 1:0.3. Stir and mix at 250°C for 2 hours, and then Settle at constant temperature for 3 hours. After the settling is finished, the upper oil slurry that accounts for 80% of the volume is taken out.

[0049] 2. Vacuum filtration

[0050] Put the upper oil slurry obtained in step 1 in a magnetically stirred reactor, feed nitrogen gas at a flow rate of 20mL / min, turn on the magnetic stirrer, and perform suction filtration under constant temperature and reduced pressure for 50min at a pressure of -0.08MPa and a temperature of 330°C. The extracted extractant is recycled.

[0051] 3. Oxidative polycondensation reaction

[0052] After vacuum filtration, replace the nitrogen with air with a flow rate of 300mL / min, continue to stir at the sam...

Embodiment 3

[0060] 1. Sedimentation and separation

[0061] Add 1,000g of coal liquefaction residue, 2,000g of extractant, and 1g of polyethyleneimine into the settling tank. The extractant is a mixture of diesel oil and anthracene oil with a mass ratio of 1:0.7. Stir and mix at 200°C for 1.5h, and then Settle at this temperature for 4 hours at a constant temperature. After the settling is finished, the upper oil slurry that accounts for 75% of the volume is taken out.

[0062] 2. Vacuum filtration

[0063] Put the upper oil slurry obtained in step 1 in a magnetically stirred reactor, feed nitrogen gas at a flow rate of 30mL / min, turn on the magnetic stirrer, and perform suction filtration at a constant temperature and reduced pressure for 30min at a pressure of -0.08MPa and a temperature of 350°C. The extracted extractant is recycled.

[0064] 3. Oxidative polycondensation reaction

[0065] After vacuum filtration, replace the nitrogen with air with a flow rate of 300mL / min, continue...

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Abstract

The invention discloses a method for preparing general-purpose pitch-based carbon fibers from coal liquefaction residues. Coal liquefaction residues rich in asphaltenes are obtained through comprehensive technologies such as sedimentation separation, vacuum suction filtration, oxidative polycondensation, non-melting treatment, and carbonization treatment. General purpose base pitch carbon fiber. Among them, sedimentation separation greatly reduces the ash content of coal liquefaction residue and effectively separates asphaltene; vacuum filtration and oxidative polycondensation reaction further increase the softening point of asphalt, which solves the problem of excessive crosslinking during high temperature polycondensation, loss of fluidity and easy coking and other problems; the non-melting treatment and carbonization treatment solve the problems of easy fusion of pre-oxidized fibers and low strength of pitch fibers after carbonization. The preparation process of the invention is simple, the cost is low, the reaction conditions are mild, the extractant can be recycled, no modifier is needed for the preparation of spinning pitch, the ash content of the spinnable pitch is low, the prepared carbon fiber has a small inner diameter and high strength, and the coal liquefaction residue It becomes a high value-added carbon material suitable for industrial applications.

Description

technical field [0001] The invention relates to a method for preparing general-purpose pitch-based carbon fibers, in particular to a method for preparing general-purpose pitch-based carbon fibers from coal liquefaction residue. Background technique [0002] The main products of coal direct liquefaction are clean fuels such as gasoline, diesel and liquefied petroleum gas, and the by-products are chemical raw materials such as benzene, toluene, xylene, phenol and sulfur. In addition, there is a part of the liquefaction residue discharge device. The unconverted organic parts, inorganic minerals, new substances generated during the liquefaction reaction, added catalysts and entrained oil in the raw coal constitute the main body of the liquefaction residue, which accounts for about 30% of the liquefied raw coal. How to efficiently clean and utilize liquefaction Residue is an important problem that must be solved in industrialization. [0003] At present, there is basically no la...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/15
CPCD01F9/15
Inventor 刘春玲董文生高鹏杨军
Owner SHAANXI NORMAL UNIV
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