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Preparation method of petroleum-based high softening point spinning pitch

A technology with high softening point and softening point, which is used in the processing of tar pitch/petroleum pitch/natural pitch, processing tar pitch/petroleum pitch/natural pitch by distillation, and chemically processing tar pitch/petroleum pitch/natural pitch, etc. , which can solve the problems such as the ineffective utilization of ethylene tar light components, and achieve the effects of excellent spinning performance, good controllability and simple process flow.

Active Publication Date: 2013-11-27
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the light components in ethylene tar cannot be effectively utilized in this method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] After 350kg of ethylene tar was preheated to 110°C, the light components were removed by wiping film evaporation at a temperature of 240°C and a vacuum of 90Pa to obtain 130kg of ethylene tar pitch with a softening point of 85°C and a coking value of 40%, and then the ethylene tar pitch was displaced In the reaction kettle, the temperature was raised to 340°C at a heating rate of 3°C / min, and the temperature was thermally polycondensed for 5 hours to increase the softening point of ethylene tar pitch to 225°C. Light components, to obtain high softening point spinning pitch 70kg. The softening point tested by ring and ball method is 275°C, and the coking value measured by GB 8727-88 is 80.7%. The spinning pitch was continuously spun for 15,000 meters, and the filament diameter was 16 μm.

Embodiment 2

[0011] After preheating 350kg of ethylene tar at 115°C, remove the light components by wiping film evaporation at a temperature of 245°C and a vacuum of 95Pa to obtain 126kg of ethylene tar pitch with a softening point of 88°C and a coking value of 43%, and then replace the ethylene tar pitch In the reaction kettle, the temperature was raised to 350°C at a heating rate of 3°C / min, and the constant temperature thermal condensation was carried out for 4.5 hours to increase the softening point of ethylene tar pitch to 220°C. Light component, obtain high softening point spinning pitch 75kg. The softening point is 271°C when tested by the ring and ball method, and the coking value is 80.1% when tested by GB 8727-88. The spinning pitch was continuously spun for 13,000 meters, and the filament diameter was 15 μm.

Embodiment 3

[0013] After 350kg of ethylene tar was preheated to 110°C, the light component was removed by scraping film evaporation at a temperature of 238°C and a vacuum of 85Pa to obtain 135kg of ethylene tar pitch with a softening point of 80°C and a coking value of 39%, and then the ethylene tar pitch was displaced In the reaction kettle, the temperature was raised to 360°C at a heating rate of 4°C / min, and the constant temperature thermal condensation was carried out for 4.5 hours to increase the softening point of ethylene tar pitch to 227°C. Light component, obtain high softening point spinning pitch 72kg. The softening point is 280°C when tested by ring and ball method, and the coking value is 82.4% when tested by GB 8727-88. The spinning pitch was continuously spun for 15,000 meters, and the filament diameter was 14 μm.

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Abstract

The invention discloses a preparation method of petroleum-based high softening point spinning pitch and belongs to the technical field of spinning pitch. The preparation method includes the steps of preheating ethylene tar, performing wiped film vaporization to remove light components at the temperature of 220-280 DEG C under the vacuum degree of 80-120Pa so as to obtain ethylene tar pitch, transferring the ethylene tar pitch into a reactor, heating to 330-360 DEG C, performing constant-temperature thermal polycondensation to obtain ethylene tar pitch softening at 200-225 DEG C, performing wiped film vaporization to the ethylene tar pitch to remove part of the light components at the temperature of 340-370 DEG C under the vacuum degree of 80-120Pa so as to finally obtain spinning pitch which softens at 270-285 DEG C. The preparation method has the advantages of continuity in operation, simplicity in process flow, high controllability and suitability for industrial production. The prepared spinning pitch is high in coking value, excellent in spinning performance, and available for continuous spinning more than 10000m in length.

Description

technical field [0001] The invention relates to a preparation method of petroleum-based high softening point spinning pitch, in particular to a preparation method of ethylene tar high softening point spinning pitch, belonging to the technical field of spinning pitch. Background technique [0002] The research on pitch-based carbon fiber began in the 1960s, and the manufacturing process of pitch-based carbon fiber was invented by Japan Sugiro Otani. Then the research on pitch-based carbon fiber developed rapidly abroad. With the development of my country's economy, the application of carbon fiber has been diversified in recent years, and its application field has been continuously expanded. Some research results have also been obtained, but the production capacity has not yet been formed. [0003] CN101135074A In the preparation method of general-purpose carbon fiber, ethylene tar is used as a raw material, and high softening point spinning pitch is prepared by air oxidati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/00C10C3/06C10C3/02
Inventor 王成扬张立昕陈明鸣王俊杰于宝军姚中君
Owner TIANJIN UNIV
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