A kind of continuous preparation method of oil-based raw material for mesophase pitch production

A technology for mesophase pitch and raw material, which is applied in the field of continuous preparation of oil-based raw materials, can solve the problems of complex composition of aromatic-rich distillate oil, high impurity content, difficulty in obtaining refined raw material oil, etc., and achieves low content of heteroatoms and solid impurities, The effect of single structure composition and low softening point

Active Publication Date: 2022-05-17
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Abstract
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Problems solved by technology

[0007] In view of the characteristics of complex composition and high impurity content of aromatic-rich distillate oil obtained by traditional treatment technology, it is difficult to obtain refined raw material oil that meets the requirements by using a single raw material pretreatment process. Therefore, according to different treatment process characteristics and mesophase pitch product performance requirements , the development of a highly universal and flexible feed oil combined pretreatment process has important economic and social benefits

Method used

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  • A kind of continuous preparation method of oil-based raw material for mesophase pitch production

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Embodiment 1

[0029] Under the condition of absolute pressure of 5KPa, 3000g of catalytic oil slurry was subjected to vacuum precision fractionation to obtain aromatic-rich distillate oil above 300°C. Take 350g of rich-aromatic distillate oil and place it in an ultrasonic generator and adjust the power to 600W. Conditions for 60min. Then, the treated distillate oil was hot filtered at 130°C using a 20nm filter medium, followed by ion exchange at 100°C, using n-heptane, toluene, and toluene-ethanol mixed solvent (1:1) as solvents in sequence. Phase, adjust the colloid and asphaltene content of the mixed components. The filtered distillate was subjected to solvent extraction, and in a 500mL three-neck flask, furfural was used as the solvent, and the ratio of component to solvent was 1:4, and refluxed for 2h. Obtain refined raw material, get 200g refined raw material oil and place in autoclave, and add 1.5gAlCl 3 The particles are used as a catalyst, and reacted at 300°C and 0.1MPa for 30 mi...

Embodiment 2

[0032]Under the condition of absolute pressure of 5KPa, 3000g of catalytic oil slurry was subjected to vacuum precision fractionation to obtain aromatic-rich distillate oil above 300°C. Take 350g of rich-aromatic distillate oil and place it in an ultrasonic generator and adjust the power to 800W. Conditions for 70min. Then, the treated distillate oil was hot filtered at 130°C using a 50nm filter medium, followed by ion exchange at 110°C, using n-heptane, toluene, toluene-ethanol mixed solvent (1:1) solvent as the flow Phase, adjust the colloid and asphaltene content of the mixed components. The distillate oil after hot filtration is subjected to solvent extraction, in a 500mL three-necked flask, N-methylpyrrolidone is used as a solvent, the ratio of component to solvent is 1:4, and the refined raw material is obtained by reflux for 2.5h, and 200g of the refined raw material oil is taken Place in a high pressure reactor and add 2g of AlCl 3 The particles are used as a catalys...

Embodiment 3

[0035] Under the condition of absolute pressure of 5KPa, 3000g of catalytic oil slurry was subjected to vacuum precision fractionation to obtain aromatic-rich distillate oil above 300°C. Take 350g of rich-aromatic distillate oil and place it in an ultrasonic generator and adjust the power to 700W. Conditions for 90min. Then, the treated distillate oil was hot filtered at 140°C using a 30nm filter medium, followed by ion exchange at 130°C, using n-heptane, toluene, toluene-ethanol mixed solvent (1:1) solvent as the flow Phase, adjust the colloid and asphaltene content of the mixed components. The hot filtered distillate oil is subjected to solvent extraction, and in a 500mL three-necked flask, a mixture of N-methylpyrrolidone and N,N-dimethylformamide (mixing ratio 2:1) is used as the solvent, and the ratio of component to solvent = 1:4, reflux for 3 hours to obtain refined raw materials, take 200g of refined raw material oil and place it in a high-pressure reactor, and add 3g...

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Abstract

The invention discloses a continuous preparation method of oil-based raw material for producing mesophase pitch. The method uses one or more heavy distillation fractions above 300°C in aromatic-rich heavy oil, catalytic oil slurry, coal tar or ethylene tar as raw material, (1) the raw material is subjected to ultrasonic cavitation treatment, and its four components are controlled Composition and distribution, and its aromatic carbon ratio (C A ) and naphthenic carbon ratio (C N ) sum between 55%-80%, obtain the raw material oil with the absolute rate of change of naphthenic ring number and aromatic ring number>3.5%; And realize the group composition distribution control, and further control the molecular weight distribution within 300-650; (3) Solvent extraction further optimizes the group composition distribution of the raw material oil, and the aromatic carbon ratio C A Control between 60%-85%; (4) Catalyze polycondensation reaction to obtain mesophase pitch with softening point of 270°C-300°C, mesophase content>97%, and good spinning performance.

Description

technical field [0001] The invention relates to a continuous preparation method for oil-based raw materials used in the production of mesophase pitch, and belongs to the research fields of petroleum deep processing technology and carbonaceous mesophase materials. Background technique [0002] The amount of catalytic oil slurry by-product of catalytic cracking unit is increasing. At present, it is mainly used as asphalt blending component or mixed with fuel oil. The utilization rate is extremely low, and the value of precious oil resources has not been fully utilized; heavy oil, coal Tar and ethylene tar also face the problem of low utilization due to their complex structure and composition. [0003] Mesophase pitch is an effective way to realize high value-added utilization of inferior oil products. However, it is required that the raw materials used for the production of mesophase pitch have uniform structural composition distribution, suitable molecular weight range, etc....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/00C10C3/08C10C3/02
CPCC10C3/00C10C3/08C10C3/02Y02P20/54
Inventor 刘东柴鲁宁沈国波杜辉段雅静付玉娥张建国袁辉志
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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