Method for FCC oil slurry hydrogenation modification-fractional thermal polycondensation preparation of mesophase pitch

A technology of mesophase pitch and hydrogenation modification, which is applied in the direction of melting and processing tar pitch/petroleum pitch/natural pitch, and chemical processing of tar pitch/petroleum pitch/natural pitch, etc., which can solve the problem of poor spinning performance and softening point High-level problems, to achieve the effect of improving spinning performance, simple process, and avoiding the use of hydrogen-supplying agent

Inactive Publication Date: 2017-09-22
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a kind of distillate with the boiling point between 380-540 ℃ in the catalytic cracking oil slurry of naphthenic crude oil as raw material, and prepare mesophase pitch through thermal condensation polymerization-hydrogenation modification-thermal condensation polymerization composite process method to solve the problems of high softening point of petroleum-based mesophase pitch and poor spinning performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 300 g 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 500ml; feed high-purity nitrogen gas to purge and replace the air in the kettle, and the temperature in the kettle is raised to 70°C to start stirring, and the rotation speed The reaction temperature is 500r / min, the reaction temperature is 380°C, the pressure is boosted to 4MPa, and the constant temperature and pressure are reacted for 4h to obtain petroleum pitch with a softening point of 120°C; then add 15g (5wt% of raw material addition) tetrahydro For naphthalene, feed high-purity nitrogen to purge and replace the air in the kettle, continue to fill with nitrogen to an initial pressure of 5MPa, start stirring at a speed of 500r / min, raise the temperature to 400°C, and react for 3 hours from the booster, and then release the pressure to normal pressure. Cool down to 350°C, use high-purity n...

Embodiment 2

[0020] Add 300 g 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 500ml; feed high-purity nitrogen gas to purge and replace the air in the kettle, and the temperature in the kettle is raised to 70°C to start stirring, and the rotation speed The reaction temperature is 500r / min, the reaction temperature is 450°C, the pressure is increased to 4MPa, and the constant temperature and pressure are reacted for 2h to obtain petroleum pitch with a softening point of 150°C; For naphthalene, feed high-purity nitrogen to purge and replace the air in the kettle, continue to fill nitrogen to an initial pressure of 5MPa, start stirring at a speed of 500r / min, raise the temperature to 420°C, and react for 1.5 hours from the booster, and then release the pressure to normal pressure , lower the temperature to 350°C, and use high-purity nitrogen with a flow rate of 100mL / (h g) ...

Embodiment 3

[0022]Add 300 g 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 500ml; feed high-purity nitrogen gas to purge and replace the air in the kettle, and the temperature in the kettle is raised to 70°C to start stirring, and the rotation speed The reaction temperature is 500r / min, the reaction temperature is 410°C, the pressure is boosted to 4MPa, and the constant temperature and pressure are reacted for 3 hours to obtain petroleum pitch with a softening point of 135°C; then add 30g (10wt% of the amount of raw material added) tetrahydro For naphthalene, feed high-purity nitrogen to purge and replace the air in the kettle, continue to fill with nitrogen to an initial pressure of 5MPa, start stirring at a speed of 500r / min, raise the temperature to 410°C, and react for 2 hours from the booster, and then release the pressure to normal pressure, Cool down to 350°C, u...

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Abstract

The invention provides a preparation method of petroleum-based mesophase pitch having a uniform molecular structure and a low softening point. The method comprises carrying out reduced pressure distillation on catalytic cracking oil slurry of naphthenic crude oil, taking a fraction having a boiling point of 380 and 540 DEG C as a raw material, carrying out a reaction process at a temperature of 380 to 450 DEG C under pressure of 4 MPa for 1 to 14 hours to obtain petroleum asphalt having a softening point of 110 to 180 DEG C, adding 1 to 15wt% of a hydrogen donor into the raw material, carrying out a self-pressure reaction process at 380 to 420 DEG C under nitrogen initial pressure of 5MPa for 1 to 8h, reducing the pressure to the normal pressure, cooling the product to 350 DEG C, carrying out high purity nitrogen purging for 0.5h to obtain hydrogenated asphalt, and carrying out a reaction process on the hydrogenated asphalt at 400 to 480 DEG C under pressure of 4MPa for 2 to 16h to obtain high quality mesophase pitch. The preparation method has simple processes and realizes a low production cost. The petroleum-based mesophase pitch has anisotropic structure content greater than 98%, a lower softening point of 230 to 250 DEG C, has a large basin type optical structure and good spinnability and is an excellent precursor for production of high modulus carbon fibers.

Description

technical field [0001] The invention relates to a preparation method of mesophase pitch, which is particularly suitable for the catalytic cracking oil slurry of naphthenic crude oil as a raw material to prepare mesophase pitch, and 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 kind of nematic liquid crystal material obtained from coal tar pitch, heavy oil, high molecular polymer and other aromatic compounds through thermal condensation or catalytic polycondensation. It is a mixture of various flat disk-shaped condensed aromatic hydrocarbons. Due to the advantages of wide sources, excellent performance, low price, high carbon yield and strong processability, mesophase pitch is recognized as an excellent precursor for many advanced functional materials, such as activated carbon fibers, carbon molecular sieves, carbon microspheres, needle coke , carbon foam, electrod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/02C10C3/10
CPCC10C3/02C10C3/10
Inventor 李明于世涛刘仕伟
Owner QINGDAO UNIV OF SCI & TECH
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