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Method for preparing mesophase pitch through hydrogenation upgrading and co-carbonization of FCC (Fluid Catalytic Cracking) decant oil

A mesophase pitch and hydrogenation modification technology, which is applied in the processing of tar pitch/petroleum pitch/natural pitch, chemically processing tar pitch/petroleum pitch/natural pitch, petroleum industry, etc., can solve the softening of mesophase pitch. High spot, poor spinning performance and other problems, to achieve the effect of moderating the reaction rate of carbonization, improving spinning performance, and avoiding excessive carbonization of coke

Inactive Publication Date: 2017-11-03
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of distillate oil with process range of 400~540 ℃ in the clarified oil of catalytic cracking of naphthenic crude oil as raw material, the method for preparing mesophase pitch through hydrogenation upgrading-co-carbonization composite process, to solve 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 180g of vacuum distillate oil from the catalytically cracked clarified oil of Bohai Oilfield naphthenic crude oil into a 300ml stainless steel high-pressure reactor; purge and replace the air in the autoclave with high-purity nitrogen. The temperature in the autoclave rises to 80℃ and starts stirring. The temperature is 450r / min, the reaction temperature is 400℃, the pressure is increased to 4MPa, the constant temperature and pressure reaction is 4h, and the petroleum pitch with a softening point of 140℃ is obtained; then 9g (5wt% of the raw material addition) is added to the reactor 9, 10-Dihydroanthracene, purge and replace the air in the kettle with high-purity nitrogen, continue to fill with nitrogen to an initial pressure of 5MPa; start stirring, rotate at 500r / min, heat up to 410°C, react by boosting pressure for 2h, then release the pressure To normal pressure, reduce the temperature to 350°C, use high-purity nitrogen with a flow rate of 80mL / (h·g) to purge for...

Embodiment 2

[0024] Add 160g of vacuum distillate oil from the catalytically cracked clarified oil of Bohai Oilfield naphthenic crude oil into a 300ml stainless steel high-pressure reactor; purge and replace the air in the autoclave with high-purity nitrogen. The temperature in the autoclave rises to 80℃ and starts stirring. The reaction temperature is 450r / min, the reaction temperature is 460℃, the pressure is increased to 4MPa, the constant temperature and pressure reaction is 1h, and the petroleum pitch with a softening point of 150℃ is obtained; then 24g (15wt% of the raw material addition) is added to the reactor 9, 10-Dihydroanthracene, purge and replace the air in the autoclave with high-purity nitrogen, continue to fill with nitrogen to an initial pressure of 5MPa; start stirring, rotate at 500r / min, heat up to 420℃, react for 1.5h from the boost, and then release The pressure is brought to normal pressure, the temperature is lowered to 350℃, and the high-purity nitrogen gas with a f...

Embodiment 3

[0026] Add 180g of vacuum distillate oil from the catalytically cracked clarified oil of Bohai Oilfield naphthenic crude oil into a 300ml stainless steel high-pressure reactor; purge and replace the air in the autoclave with high-purity nitrogen. The temperature in the autoclave rises to 80℃ and starts stirring. The reaction temperature is 450r / min, the reaction temperature is 430℃, the pressure is increased to 4MPa, the constant temperature and pressure reaction is 2h, and the petroleum pitch with a softening point of 145℃ is obtained; then 18g (10wt% of the raw material addition) is added to the reactor 9, 10-Dihydroanthracene, purge and replace the air in the autoclave with high-purity nitrogen, continue to fill with nitrogen to an initial pressure of 5MPa; start stirring, rotate at 500r / min, heat up to 410℃, react by self-boosting for 2h, then release the pressure To normal pressure, reduce the temperature to 350°C, use high-purity nitrogen at a flow rate of 100mL / (h·g) to p...

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Abstract

The invention provides a method for preparing a petroleum-based mesophase pitch with high anisotropic structure content and low softening point. The method comprises the following steps: conducting reduced pressure distillation on an FCC (Fluid Catalytic Cracking) decant oil of a naphthenic crude, taking a cut fraction with the boiling point of 400-540 DEG C as a raw material, and reacting for 1-8 hours at the temperature of 400-460 DEG C and under the pressure of 4 MPa to obtain a petroleum pitch; then adding a hydrogen donor, reacting under condition of the self-generated pressure at the temperature of 380-450 DEG C at the initial nitrogen pressure of 5 MPa, then reducing the pressure to the normal pressure, cooling to 340 DEG C, and blowing with high-purity nitrogen for 0.5 hour to obtain a hydrogenated pitch; finally adding a co-carbonization additive, and reacting for 2-16 hours at the temperature of 400-480 DEG C at the pressure of 4MPa to obtain the high-quality mesophase pitch. The preparation process is simple, the production cost is low, the anisotropic structure content (more than 98%) of the prepared mesophase pitch is high, the softening point (230-270 DEG C) is low, the spinning property is good, and the mesophase pitch is an excellent precursor for preparing a high-modulus carbon fiber.

Description

Technical field [0001] The invention relates to a method for preparing mesophase pitch from a catalytically cracked clarified naphthenic crude oil through a combined process of hydrogenation upgrading and co-carbonization, 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 nematic liquid crystal substance composed of a variety of flat disc-shaped fused ring aromatic hydrocarbons. It has special crystal-like physical properties in terms of heat, light, electricity, and magnetism. It still has liquid characteristics in terms of fluidity, viscosity and deformation. Due to its excellent performance, high carbon yield, and strong processability, mesophase pitch is an excellent matrix for many advanced functional materials, and can prepare a variety of high-performance carbon materials, such as ultra-high modulus pitch-based carbon fiber, needle coke, and carbon Foams, mesoph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/02
CPCC10C3/026
Inventor 李明于世涛刘仕伟
Owner QINGDAO UNIV OF SCI & TECH
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