Method for preparing mesophase pitch through FCC oil slurry two-stage hydroforming-heat polycondensation

A technology of mesophase pitch and reaction time, 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 chemical methods, which can solve the problem of high softening point and poor spinning performance and other problems, to achieve low softening point, maintain uniformity, and good spinning performance

Inactive Publication Date: 2017-11-24
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing mesophase pitch through a two-stage hydrogen modification-thermal polycondensation composite process using the distillate with a boiling point between 380 and 540°C in the catalytic cracking oil slurry of naphthenic crude oil as raw material, so as to solve the problem of Petroleum-based mesophase pitch has high softening point and poor spinning performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 170g of vacuum distillate oil from catalytic cracking slurry of naphthenic crude oil from Bohai Oilfield into a stainless steel high-pressure reaction kettle with a volume of 300ml; introduce high-purity nitrogen to replace the air in the kettle, continue to fill nitrogen to an initial pressure of 4MPa, and start stirring. The rotation speed is 500r / min, the temperature is raised to 380°C, and the reaction is carried out at constant temperature and pressure for 5 hours; then the pressure is released to normal pressure, the temperature is lowered to normal temperature, the air in the kettle is replaced with high-purity nitrogen, and hydrogen is charged to an initial pressure of 6MPa. 500r / min, self-pressurization reaction for 1h; then cool down to normal temperature, release the pressure to normal pressure, replace the air in the kettle with high-purity nitrogen, fill nitrogen to 4MPa, raise the temperature to 430°C, and the speed is 500r / min, constant temperature and ...

Embodiment 2

[0024]Add 170g of vacuum distillate oil from catalytic cracking slurry of naphthenic crude oil from Bohai Oilfield into a stainless steel high-pressure reaction kettle with a volume of 300ml; introduce high-purity nitrogen to replace the air in the kettle, continue to fill nitrogen to an initial pressure of 4MPa, and start stirring. The rotation speed is 500r / min, the temperature is raised to 450°C, and the reaction is carried out at constant temperature and pressure for 1 hour; then the pressure is released to normal pressure, the temperature is lowered to normal temperature, the air in the kettle is replaced with high-purity nitrogen, and hydrogen is charged to an initial pressure of 6MPa, the temperature is raised to 430°C, and the speed 500r / min, self-pressurization reaction for 1h; then cool down to normal temperature, release the pressure to normal pressure, replace the air in the kettle with high-purity nitrogen, fill nitrogen to 4MPa, raise the temperature to 460°C, and ...

Embodiment 3

[0026] Add 170g of vacuum distillate oil from catalytic cracking slurry of naphthenic crude oil from Bohai Oilfield into a stainless steel high-pressure reaction kettle with a volume of 300ml; introduce high-purity nitrogen to replace the air in the kettle, continue to fill nitrogen to an initial pressure of 4MPa, and start stirring. The rotation speed is 500r / min, the temperature is raised to 430°C, and the reaction is carried out at constant temperature and pressure for 2 hours; then the pressure is released to normal pressure, the temperature is lowered to normal temperature, the air in the kettle is replaced with high-purity nitrogen, and hydrogen is charged to an initial pressure of 6MPa, the temperature is raised to 410°C, and the speed is 500r / min, self-pressurization reaction for 1h; then cool down to normal temperature, release the pressure to normal pressure, replace the air in the kettle with high-purity nitrogen, fill nitrogen to 4MPa, raise the temperature to 440°C,...

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Abstract

The invention provides a preparation method for a spinnable petroleum base mesophase pitch with high anisotropic structure content and low softening point. The method comprises the following steps: performing reduced pressure distillation on naphthenic crude catalytic cracking oil slurry, by taking a fraction with the boiling point at 380-540 DEG C as a raw material, and then performing constant-temperature constant-pressure reaction for 1-10h under the primary nitrogen pressure at 4MPa at 380-450 DEG C, thereby acquiring petroleum asphalt; performing self-boosting reaction on the petroleum asphalt for 1-8h under the primary nitrogen pressure at 6MPa at 400-440 DEG C, thereby acquiring the first hydrogenated pitch; performing constant-temperature constant-pressure reaction on the first hydrogenated pitch for 1-8h under the primary nitrogen pressure at 4MPa at 420-480 DEG C, thereby acquiring a first product; performing self-boosting reaction on the first product for 1-8h under the primary nitrogen pressure at 6MPa at 400-440 DEG C, thereby acquiring a secondary hydrogenated pitch; reacting the secondary hydrogenated pitch for 2-16h under the pressure at 4MPa at 420-480 DEG C, thereby acquiring the high-quality mesophase pitch. According to the invention, the production cost is low and the prepared mesophase pitch has the advantages of high anisotropic structure content (above 98%), low softening point (at 230-250 DEG C), large watershed optical structure and excellent spinning property.

Description

technical field [0001] The invention relates to a method for preparing mesophase pitch from catalytic cracking oil slurry of naphthenic crude oil through a two-stage hydrogen modification-thermal polycondensation composite process, which belongs to the cross field of heavy oil processing and preparation of new carbon materials. Background technique [0002] Mesophase pitch (MP for short) is a nematic liquid crystal substance composed of a variety of flat disk-shaped condensed ring aromatics. It has liquid characteristics in terms of fluidity, viscosity, and deformation. However, it has physical properties similar to crystals in aspects such as magnetism and magnetism. Due to its excellent performance, high carbon yield and strong processability, mesophase pitch has become an excellent matrix for many advanced functional materials, and can be used to prepare a variety of high-performance carbon materials, such as ultra-high modulus pitch-based carbon fibers, Needle coke, car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/02C10C3/06
CPCC10C3/02C10C3/06
Inventor 李明于世涛刘仕伟
Owner QINGDAO UNIV OF SCI & TECH
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