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Method for preparing mesophase asphalt and carbon fibers through flash pyrolysis pretreatment-catalytic condensation polymerization of heavy oil

A mesophase pitch and pretreatment technology, applied in the processing of tar pitch/petroleum pitch/natural pitch, processing tar pitch/petroleum pitch/natural pitch by heating, and chemically processing tar pitch/petroleum pitch/natural pitch, etc. , which can solve the problems of difficult control of reaction stability, high softening point of mesophase pitch, high content of anisotropic structure, and achieve the effect of being conducive to self-assembly and directional stacking, high modulus and strength, and less demanding equipment requirements.

Pending Publication Date: 2018-11-02
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Chinese patent CN106435840A is a preparation method of pitch-based carbon fiber, which uses high-pressure hydrogenation pretreatment and co-carbonization additives to prepare spinnable mesophase pitch by two-step polycondensation, which improves the composition of the reaction system and is conducive to the preparation of high-quality spinnable petroleum-based carbon fibers. Mesophase pitch makes up for the defects of single raw material structure and composition structure, but the stability of the reaction is not easy to control
Chinese patent CN107189802A is a method for preparing mesophase pitch by hydrogenation modification of FCC oil slurry-stage thermal polycondensation, which solves the problems of high softening point and poor spinning performance of petroleum-based mesophase pitch, and the obtained mesophase pitch is isotropic High content of anisotropic structure, with a large watershed optical structure, is an excellent precursor for the production of high modulus carbon fibers
However, the hydro-upgrading process is relatively complicated and requires high equipment. It is difficult for the system to completely separate and recover the by-products. The cost is high and it is difficult to realize industrialization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 300g of FCC oil slurry, stay in the fluidized bed for 1s, control the pressure at 0.05MPa, and pyrolysis temperature at 550°C to obtain pyrolysis oil; the pyrolysis oil is distilled to obtain heavy distillate oil above 350°C, which is For modified raw materials.

[0024] The basic properties of the modified raw material are: nitrogen content 0.3wt%, sulfur content 0.8wt%, C / H atomic ratio 1.03, carbon residue value 1.1wt%, viscosity (100°C) 15mm 2 ·s -1 , the density (20°C) is 986 / kg·m -3 , the saturated fraction is 5.15wt%, the aromatic fraction is 78.73wt%, the colloid is 13.69wt%, and the asphaltene is 2.43wt%;

[0025] With the modified raw material of 150g and catalyst ZrO 2 Mix well (the mass ratio of the catalyst to the raw material is 0.02), add it into a stainless steel reaction kettle, start stirring under a nitrogen atmosphere, continue the reaction at 280°C and 4MPa for 20h, release the pressure, and slowly cool down to obtain a mesophase content of ...

Embodiment 2

[0027] Take 300g of cycloalkyl vacuum distillate oil, stay in the fluidized bed for 0.5s, control the pressure at 0.05MPa, and pyrolysis temperature at 550°C to obtain pyrolysis oil; the pyrolysis oil is distilled to obtain heavy distillate oil above 350°C, The heavy distillate is the modified raw material.

[0028]The basic properties of the modified raw material are: nitrogen content 0.32wt%, sulfur content 1.0wt%, C / H atomic ratio 1.05, carbon residue value 1.2wt%, viscosity (100°C) 14mm 2 ·s -1 , the density (20°C) is 985 / kg·m -3 , the saturated content is 6.36wt%, the aromatic content is 77.82wt%, the colloid is 13.55wt%, and the asphaltene is 2.27wt%;

[0029] With the modified raw material of 150g and catalyst ZrO 2 Mix well (the mass ratio of the catalyst to the raw material is 0.05), add it into a stainless steel reaction kettle, start stirring under a nitrogen atmosphere, 300°C, 8MPa, continue the reaction for 28h, release the pressure, and slowly lower the temper...

Embodiment 3

[0031] Take 300g of naphthenic hydrogenation tail oil, stay in the fluidized bed for 0.6s, control the pressure at 0.05MPa, and pyrolysis temperature at 560°C to obtain pyrolysis oil; the pyrolysis oil is distilled to obtain heavy distillate oil above 350°C, The heavy distillate is the modified raw material.

[0032] The basic properties of the modified raw material are: nitrogen content 0.26wt%, sulfur content 1.2wt%, C / H atomic ratio 1.11, carbon residue value 1.3wt%, viscosity (100°C) 16mm 2 ·s -1 , the density (20°C) is 988 / kg·m -3 , the saturated fraction is 3.62wt%, the aromatic fraction is 80.16wt%, the colloid is 13.32wt%, and the asphaltene is 2.90wt%;

[0033] With the modified raw material of 150g and catalyst ZrO 2 Mix well (the mass ratio of the catalyst to the raw material is 0.03), add it into a stainless steel reaction kettle, start stirring under a nitrogen atmosphere, continue the reaction at 290°C and 6MPa for 26h, release the pressure, and slowly lower t...

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Abstract

The invention provides a method for preparing mesophase asphalt and carbon fibers through flash pyrolysis pretreatment-catalytic condensation polymerization of heavy oil. The method comprises the following steps: carrying out short-time high-temperatrure pyrolysis pretreatment on the raw materials, so as to obtain the modified raw materials; and mixing the modified raw materials with a catalyst, so as to prepare mesophase asphalt, wherein raw material oil is FCC oil slurry heavy fraction, naphthene base decompression distillate oil or naphthene base hydrogenation tail oil; and preparing high-modulus the high-strength carbon fibers from the obtained mesophase asphalt. The method has the beneficial effects that the process flow is simple, and the adopted catalyst does not corrode equipment and does not have harsh requirements on the equipment; the prepared mesophase asphalt is low in softening point (230-250 DEG C), the content of an intermediate phase reaches 98% or above, and the mesophase asphalt has a large-wide area streamline optical anisotropy structure and good spinnability; and by carrying out pre-oxidation, carbonization and graphitization on the spun raw yarns, the high-modulus and high-strength asphalt-based carbon fibers can be obtained.

Description

technical field [0001] The invention relates to a method for fast pyrolysis pretreatment of heavy oil-catalytic polycondensation to prepare mesophase pitch and carbon fiber, and belongs to the technical field of petroleum deep processing and the research field of carbon fiber precursor. Background technique [0002] Mesophase pitch is a kind of nematic liquid crystal formed by heat treatment of petroleum residue, coal tar, and pure aromatic compounds. It is easy to graphitize and is an excellent precursor for preparing a variety of high-performance new carbon materials. Using heavy oil as raw material to prepare mesophase pitch is an important way to realize high value-added utilization of heavy oil, and plays an important role in the overall planning and development of the petroleum refining industry. [0003] Using mesophase pitch as the precursor, the raw silk is obtained by melt spinning, and the high-performance carbon fiber (HPCF) can be obtained after the raw silk is ...

Claims

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Application Information

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IPC IPC(8): C10C3/00C10C3/02D01F9/22
CPCC10C3/002C10C3/026D01F9/22
Inventor 刘东温福山付玉娥娄斌于冉王翔宇吴柯殷长龙师楠郭爱军李敏陈清泰李骏龚鑫张智琛
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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