Method for preparing spinnable asphalt through co-heating condensation polymerization of anhydride-modified coal asphalt and kerosene co-refining residues

A kerosene co-refining residue and acid anhydride modification technology are applied in the processing of tar pitch/petroleum pitch/natural pitch, chemically processing tar pitch/petroleum pitch/natural pitch, melt spinning, etc. Control, low softening point increase, poor spinning performance, etc., to achieve the effect of good spinnability, good fluidity and high softening point

Active Publication Date: 2019-12-17
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these modified asphalt methods still have the disadvantages of difficult control of reaction conditions, complicated operation, low increase in softening point, many infusibles at spinning temperature, low yield and poor spinning performance.

Method used

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  • Method for preparing spinnable asphalt through co-heating condensation polymerization of anhydride-modified coal asphalt and kerosene co-refining residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Medium-low temperature coal tar pitch (softening point: 90°C, ash content 0.2wt%) was crushed to ≤20 mesh, mixed with tetrahydrofuran at a mass ratio of 1:4, the soluble components of medium-temperature coal tar pitch were extracted and filtered, and vacuum-dried for 12 hours to obtain The ash content was 0.03% by weight of asphaltenes B.

[0027] Crush the kerosene co-refining residue (ash content 29wt%) to ≤20 mesh, mix it with tetrahydrofuran at a mass ratio of 1:4, extract and filter the soluble components of the kerosene co-refining residue, and vacuum dry for 12 hours to obtain an ash content of 0.02wt% of asphaltene A.

[0028] Mix the obtained asphaltenes B with pyromellitic anhydride and maleic anhydride in a ratio of 20:1:1 (weight ratio), put it into the reactor, and continuously feed nitrogen gas at a rate of 20mL / min·g, Heat to 350°C at a heating rate of 9°C / min and stay for 3 hours. The obtained asphalt has a softening point of 175°C and a softening melt...

Embodiment 2

[0031] Grind medium-low temperature coal tar pitch (softening point: 88°C, ash content 0.2wt%) to ≤20 mesh, mix with tetrahydrofuran at a mass ratio of 1:5, extract and filter out the soluble components of medium-temperature coal tar pitch, and vacuum dry for 12 hours to obtain The ash content was 0.03% by weight of asphaltenes B.

[0032] Crush the kerosene co-refining residue (ash content 27wt%) to ≤20 mesh, mix with tetrahydrofuran at a mass ratio of 1:5, extract and filter out the soluble components of kerosene co-refining residue, and vacuum dry for 12 hours to obtain an ash content of 0.01wt% of asphaltene A.

[0033] Mix the obtained asphaltenes B with pyromellitic anhydride and maleic anhydride in a ratio of 15:2:1 (weight ratio), put it into the reactor, and continuously feed nitrogen gas at a rate of 30mL / min·g, Heat to 370°C at a heating rate of 10°C / min and stay for 1 hour. The obtained asphalt has a softening point of 179°C and a softening melting range of 179-1...

Embodiment 3

[0036] Medium-low temperature coal tar pitch (softening point: 89°C, ash content 0.2wt%) was crushed to ≤20 mesh, mixed with tetrahydrofuran at a mass ratio of 1:7, the soluble components of medium-temperature coal tar pitch were extracted and filtered, and dried in vacuum for 12 hours to obtain The ash content was 0.02% by weight of asphaltenes B.

[0037] Crush the kerosene co-refining residue (ash content 28wt%) to ≤20 mesh, mix it with tetrahydrofuran at a mass ratio of 1:7, extract and filter the soluble components of the kerosene co-refining residue, and vacuum dry for 12 hours to obtain an ash content of 0.01wt% of asphaltene A.

[0038] Mix the obtained asphaltene B with pyromellitic anhydride and maleic anhydride at a ratio of 15:1:2 (weight ratio), put it into the reactor, and continuously feed nitrogen at a rate of 10mL / min·g, Heat to 420°C at a heating rate of 1°C / min and stay for 5 hours. The obtained asphalt has a softening point of 180°C and a softening meltin...

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Abstract

The invention discloses a method for preparing spinnable asphalt through co-heating condensation polymerization of anhydride-modified coal asphalt and kerosene co-refining residues. The method includes the steps of pulverizing kerosene co-refining residues and medium-and-low-temperature coal asphalt to reach the granularity of 20 mesh or below, extracting and filtering out soluble components through tetrahydrofuran, recovering a solvent to obtain asphaltene A and asphaltene B, mixing the asphaltene B with benzenetetracarboxylic anhydride and maleic anhydride, introducing nitrogen at normal pressure, raising the temperature to 350-450 DEG C at the temperature rise rate of 1-10 DEG C/min, keeping the temperature for 1-10 hours, lowering the temperature to the room temperature to obtain a solid product (substrate asphalt), mixing the substrate asphalt with the asphaltene A, introducing normal-pressure nitrogen, raising the temperature to 350-400 DEG C at the temperature rise rate of 1-10DEG C/min, keeping the temperature for 1-10 hours, and lowering the temperature to the room temperature to obtain the solid product (spinnable asphalt). The modified spinnable asphalt has the advantages of being moderate in softening point, short in softening and melting range and capable of continuously preparing asphalt fiber filaments through melting and spinning.

Description

technical field [0001] The invention belongs to a method for preparing spinnable asphalt, in particular to a method for preparing spinnable asphalt by co-thermal polycondensation of acid anhydride modified coal tar pitch and kerosene co-refining residue. Background technique [0002] Pitch carbon fiber and its composite materials have properties such as light weight, high specific strength, high specific modulus, high temperature resistance, acid and alkali corrosion resistance, fatigue resistance, creep resistance and excellent electrical and thermal conductivity, and are widely used in aerospace and construction industries , transportation, machinery, sporting goods and other fields. In addition, pitch-based carbon fiber has high carbon yield, wide source of precursor, low cost, simple and easy spinning process, low production cost and high added value. It has developed rapidly in recent years. [0003] With the current rapid increase in the share of domestic kerosene co-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/15D01D5/08C10C3/02
CPCC10C3/026D01D5/08D01F9/15
Inventor 左萍萍曲世杰蒋伟牛宏贤申文忠倪国松牛浩杨宜凯
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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