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Preparation method of nucleating agent for mesocarbon microbeads

A technology of mesocarbon microspheres and nucleating agent, which is used in the processing of tar pitch/petroleum pitch/natural pitch, processing tar pitch/petroleum pitch/natural pitch by selective extraction, and processing tar pitch/petroleum pitch/natural pitch by heating It can solve the problems of difficult particle size control, low yield of mesocarbon microspheres, etc., to achieve stable product quality, increase the chance of polycondensation into spheres, and optimize the thermal polycondensation reaction conditions.

Pending Publication Date: 2021-11-02
鞍钢化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a preparation method of a nucleating agent for mesocarbon microspheres, to optimize the thermal polycondensation reaction conditions in the formation process of mesocarbon microspheres, and to solve the problem of the yield of mesocarbon microspheres. The problem of low particle size and difficult control of particle size, and the process is easy to realize and the product quality is stable

Method used

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  • Preparation method of nucleating agent for mesocarbon microbeads
  • Preparation method of nucleating agent for mesocarbon microbeads

Examples

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Effect test

Embodiment 1

[0028] The preparation method of the nucleating agent of mesocarbon microspheres is to raise the temperature of low-temperature coal tar pitch in the polymerization reactor from normal temperature to 360°C at 3°C / min, and stay at constant temperature for 2h to obtain nuclei-rich pitch; wash oil and paraffin oil by 1 The mass ratio of : 5 is used to make a mixed solvent, and the mixed solvent and nuclear-enriched asphalt are fully mixed in the oil mixing tank according to the agent-oil ratio of 1: 1. The mixing temperature is 80 ° C, the time is 1.5 h, and the stirring speed is 80 rad / min; mix well Finally, stop stirring, raise the temperature to 120°C and let it stand for 1 hour, and obtain a nuclear-rich solvent oil with a yield of 30% from the bottom of the mixing tank; distill the nuclear-rich solvent oil in a fractionation tower, and the distillation condition is a tower bottom temperature of 380°C , the temperature at the top of the tower is 260°C, the vacuum degree is 0.0...

Embodiment 2

[0030] Raise the temperature of high-temperature coal tar pitch in the polymerization reactor from room temperature to 340°C at 5°C / min, and stay at constant temperature for 1 hour to obtain nuclear-rich pitch; make a mixed solvent of wash oil and kerosene at a mass ratio of 1:1.5, press the agent oil The ratio is 0.5:2, fully mix the mixed solvent and nuclear-rich asphalt in the oil mixing kettle, the mixing temperature is 120°C, the time is 2h, and the stirring speed is 100rad / min; after mixing evenly, stop stirring, raise the temperature to 120°C and let it stand 8h, get the nuclei-enriched solvent oil with a yield of 40% from the bottom of the mixing tank; distill the nuclei-enriched solvent oil in a fractionation tower, the distillation conditions are 400°C at the bottom of the tower, 260°C at the top of the tower, and a vacuum of 0.07MPa, and recover them separately Kerosene and washing oil are obtained from the bottom of the fractionation tower as a nucleating agent. Th...

Embodiment 3

[0032] The heavy oil directly liquefied from coal is heated from normal temperature to 295°C at 5°C / min in a polymerization reactor, and then kept at a constant temperature for 3 hours to obtain nuclei-rich pitch; the coking light oil and petroleum ether are formulated into a mixed solvent at a mass ratio of 1:1 , according to the agent-oil ratio of 5:2, fully mix the mixed solvent and nuclear-rich asphalt in the oil mixing kettle, the mixing temperature is 60°C, the time is 3h, and the stirring speed is 120rad / min; after mixing evenly, stop stirring and raise the temperature to 130 ℃ and stand for 4 hours, the yield of 10% nuclei-enriched solvent oil is obtained from the bottom of the mixing tank; the nuclei-enriched solvent oil is distilled in a fractionation tower, the distillation conditions are 340°C at the bottom of the tower, 220°C at the top of the tower, and a vacuum of 0.09 MPa, recover light oil and petroleum ether respectively, and obtain the nucleating agent from t...

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Abstract

The invention relates to a preparation method of a nucleating agent of mesocarbon microbeads. The preparation method comprises the steps of 1) performing thermal polycondensation treatment on raw oil to obtain nuclear-rich asphalt; 2) fully mixing the nuclear-rich asphalt with a mixed solvent to obtain mixed oil; (3) carrying out settling separation on the mixed oil to obtain nuclear-rich solvent oil; and 4) distilling the nuclear-rich solvent oil, and recovering the residual mixed solvent in the step 2) to obtain the nucleating agent. The method has the advantages that the nucleating agent prepared by the method is in a glassy state and has excellent properties of stable thermal reactivity, easiness in melting and dispersing, easiness in graphitization and the like, the yield of the carbon microspheres prepared by the traditional method is less than 25%, the particle size distribution is 5-40 microns, the yield of the mesocarbon microspheres prepared by the nucleating agent can be increased to 25-40%, the particle size distribution is 15-35 microns, and the method has the characteristics of high yield, good sphericity, narrow particle size distribution, high purity, high graphitization degree and stable electrochemical performance.

Description

technical field [0001] The invention relates to a preparation method of a nucleating agent for mesocarbon microspheres. Background technique [0002] Mesophase carbon microspheres refer to asphalt-like organic compounds (such as petroleum residue and coal tar pitch, etc.) formed by heat treatment in an inert atmosphere at a medium temperature (350-550°C) with large molecular weight, high flatness, and thermodynamic stability. The condensed fused-ring aromatic hydrocarbons are condensed and arranged under the action of surface tension to form optically anisotropic spherical aggregates with a diameter of 5-100 μm. The spheroids obtained in the above process are extracted from the mother liquor to obtain mesophase carbon microspheres. [0003] Mesocarbon microspheres are a new type of carbon material. Due to the structure of parallel stacking of layered molecules and the characteristics of spherical shape, the ball diameter is small and evenly distributed, and it has high elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/00C10C3/06C10C3/08
CPCC10C3/002C10C3/06C10C3/08C10C3/00
Inventor 刘海丰何莹张大奎穆春丰刘雪松姚君张欣王晓楠
Owner 鞍钢化学科技有限公司
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