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Method for preparing intermediate-phase asphalt by crosslinking modifying and settling separation of FCC (fluid catalytic cracking) clear oil

A mesophase pitch and mesophase technology, which is applied in the direction of chemical processing of tar pitch/petroleum pitch/natural pitch, etc., can solve the problems of poor spinning performance and low content of anisotropic structure, so as to promote the formation and benefit Sequential arrangement, good fluidity effect

Inactive Publication Date: 2017-09-29
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 method that takes naphthenic crude oil catalytic cracking clarified oil boiling point between 380~540 ℃ as raw material, and prepares the method for mesophase pitch through cross-linking modification-sedimentation separation compound process, to solve Petroleum-based mesophase pitch has low anisotropic structure content and poor spinning performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The naphthenic crude oil catalytic cracking clarified oil decompression distillate oil 300g and 15g (5wt% of raw material addition) polybutadiene diol are joined in the volume of 500ml stainless steel autoclave with the naphthenic crude oil catalytic cracking clarified oil vacuum distillate oil; Sweep the air in the displacement kettle, continue to fill nitrogen to the initial pressure of 5MPa, start stirring at a speed of 500r / min, raise the temperature to 380°C, and react for 4 hours from the booster, then release the pressure to normal pressure, cool down to 300°C, and use a flow rate of 80mL / (h·g) of high-purity nitrogen was purged for 0.5h to obtain modified oil; continue to heat up to 430°C, rotate at 500r / min, self-boost to 4MPa, react at constant temperature and pressure for 8h, and obtain a softening point of 216°C mesophase precursor; then lower the temperature to 320°C and settle for 2 hours under normal pressure. The product in the reactor is divided into two...

Embodiment 2

[0021]The naphthenic crude catalytic cracking clarified oil decompression distillate oil 280g and 42g (15wt% of raw material addition) polybutadiene diol of Bohai Oilfield joins volume as in the stainless steel autoclave of 500ml; Sweep the air in the replacement kettle, continue to fill nitrogen to the initial pressure of 5MPa, start stirring at a speed of 500r / min, raise the temperature to 450°C, and react for 1h from the booster, then release the pressure to normal pressure, cool down to 300°C, and use a flow rate of 80mL / (h·g) of high-purity nitrogen was purged for 0.5h to obtain modified oil; continue to heat up to 440°C, rotate at 500r / min, self-boost to 4MPa, react at constant temperature and pressure for 6h, and obtain a softening point of 231°C mesophase precursor; then lower the temperature to 330°C and settle for 2 hours under normal pressure. The product in the reactor is divided into two layers. The mesophase pitch with watershed optical structure has a softening ...

Embodiment 3

[0023] The naphthenic crude oil catalytic cracking oil slurry vacuum distillate oil 300g and 24g (8wt% of raw material addition) polybutadiene diol of Bohai Oilfield are joined in the 500ml stainless steel autoclave; Pass into high-purity nitrogen to blow Sweep the air in the replacement kettle, continue to fill nitrogen to the initial pressure of 5MPa, start stirring at a speed of 500r / min, raise the temperature to 420°C, and react for 2.5 hours from the booster, then release the pressure to normal pressure, cool down to 300°C, and use the flow rate Purging 80mL / (h·g) of high-purity nitrogen for 0.5h to obtain modified oil; continue to raise the temperature to 440°C, rotate at 500r / min, self-boost to 4MPa, react at constant temperature and pressure for 6h, and obtain a softening point of 223 ℃ mesophase precursor; then lower the temperature to 320℃, and settle for 2 hours under normal pressure. The mesophase pitch with large watershed optical structure has a softening point o...

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Abstract

The invention provides a preparation method of petroleum-based intermediate-phase asphalt with centralized distribution of molecular weight, high content of soluble intermediate phase and low softening point. The preparation method comprises the following steps of performing pressure-relief distillation on catalytic cracking clear oil of naphthenic crude oil, selecting fractions with boiling point of 380 to 540 DEG C as raw materials, uniformly mixing with a crosslinking agent, and performing self-pressure increase reaction for 1 to 10h at the temperature of 380 to 450 DEG C and nitrogen initial pressure of 5MPa; then, cooling to 300 DEG C, and using high-purity nitrogen to purge for 0.5h at normal pressure, so as to obtain modified oil; enabling the modified oil to continue to react for 2 to 14h at the temperature of 400 to 480 DEG C and pressure of 4MPa, so as to obtain an intermediate-phase precursor; settling the intermediate-phase precursor for 0.5 to 6h at the temperature of 280 to 340 DEG C and normal pressure, wherein the interior of the container contains two layers of products, and the lower layer of product is the prepared high-quality intermediate-phase asphalt. The preparation method has the advantages that the technology is simple, and the production cost is low; the content of anisotropic structure is high and is greater than 98%, the large-flow domain type optical structure is realized under the polarizing condition, the softening point is low and is 230 to 250 DEG C, the content of the soluble intermediate phase is high and is 46 to 51%, and the spinnability is good.

Description

technical field [0001] The invention relates to a method for preparing mesophase pitch from catalytic cracking clarified oil of naphthenic crude oil through a composite process of cross-linking modification-sedimentation separation, 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 mixture of various flat disk-shaped fused-ring aromatic hydrocarbons with relatively concentrated relative molecular weights, and a nematic liquid crystal material formed from a mixture of heavy aromatic hydrocarbons. Mesophase pitches have the characteristics of liquid crystals. They have special crystal-like physical properties in terms of heat, light, electricity, and magnetism, but they are still liquid in terms of fluidity, viscosity, and deformation. Therefore, they have excellent performance and carbon production. It is an excellent matrix for many advanced functional materials, a...

Claims

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Application Information

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