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Mesophase pitch and preparation method thereof

A technology of mesophase pitch and coal tar pitch, which is applied in the field of mesophase pitch and its preparation, can solve the problem of high cost of coating material preparation, achieve excellent oxidation resistance, improve performance, and improve performance

Active Publication Date: 2012-07-18
常州黑码服饰有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of coating technology requires the introduction of a transition layer due to the mismatch of expansion coefficients, resulting in higher preparation costs for coating materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 800g of medium temperature coal tar pitch, AlCl 3 100 g was placed in a stainless steel autoclave, and the temperature was raised to 250° C. under nitrogen protection and mechanical stirring, and the nitrogen pressure was kept at 3 MPa, and the catalytic polycondensation pitch was obtained by staying for 4 hours. Finally, the pressure was released, cooled, and then distilled water was added, heated to 250°C and mechanically stirred, and reacted for 0.5 hours, then the pressure was released, and the water was discharged. Then heat treatment at a vacuum of 100-300mmHg and 430°C for 8 hours to obtain mesophase pitch with 85% optical anisotropy and a softening point of 284°C. The ash content is measured by the method of GB / T 2295-2008, and the ash impurity content is 5.02%. The ash composition was analyzed by XRD, and the result was mainly Al 2 o 3 .

Embodiment 2

[0019] Take 800g of medium temperature coal tar pitch, ZrCl 4 100g, AlCl 3 100 g was placed in a stainless steel autoclave, and the temperature was raised to react under nitrogen protection and mechanical stirring, to 200 ° C, and the nitrogen pressure was kept at 3 MPa, and the catalytic polycondensation pitch was obtained by staying for 6 hours. Then remove the pressure, cool down, then add distilled water, heat to 250°C and perform mechanical stirring, react for 1 hour, release the pressure, and discharge the water. Then heat-treat at a vacuum of 100-300mmHg and 450°C for 5 hours to obtain mesophase pitch with 80% optical anisotropy and a softening point of 284°C. The ash content is measured by the method of GB / T 2295-2008, and the ash content is 10.18%. The ash composition was analyzed by XRD, and the result was mainly Al 2 o 3 with ZrO 2 .

Embodiment 3

[0021] Take 800g of medium temperature coal tar pitch, SiCl 4 300g was placed in a stainless steel autoclave, and the temperature was raised to 180°C under nitrogen protection and mechanical stirring, and the nitrogen pressure was kept at 4MPa, and the catalytic polycondensation pitch was obtained by staying for 10 hours. Then remove the pressure, cool down, then add distilled water, heat to 250°C and perform mechanical stirring, react for 1 hour, release the pressure, and discharge the water. Then heat-treat at a vacuum of 100-300mmHg and 420°C for 10 hours to obtain mesophase pitch with 80% optical anisotropy and a softening point of 294°C. The ash content is measured by the method of GB / T 2295-2008, and the ash content is 12.59%. The ash composition was analyzed by XRD, and the result was mainly SiO 2

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Abstract

The invention relates to mesophase pitch and a preparation method thereof. The mesophase pitch contains 5 to 13 mass percent of Al2O3, SiO2, B2O3, and ZrO2 impurities which have oxidation resistance. The preparation method comprises the following steps of: catalyzing polycyclic aromatic hydrocarbon by using a friedel-crafts alkylation catalyst to perform polycondensation on medium-temperature coal pitch or coal tar which is used as a raw material, wherein the friedel-crafts alkylation catalyst is any one or more of anhydrous AlCl3, ZrCl4, SiCl4, and BCl3; after polycondensation, adding water to perform hydrolysis; and performing pyrocondensation polymerization to covert pitch subjected to polycondensation into the mesophase pitch. The mesophase pitch contains antioxidants, and the prepared carbon material has excellent oxidation resistance.

Description

technical field [0001] The invention relates to a mesophase pitch and a preparation method thereof. Background technique [0002] Carbon / graphite materials have a series of excellent properties, such as low density, high specific strength, high thermal stability, ablation resistance, corrosion resistance and stable friction coefficient, etc., especially the strength and stiffness at room temperature at 1650 ° C, 2000 ℃ can still maintain excellent mechanical properties, it is an ideal high temperature structural material. However, the surface oxidation resistance of carbon / graphite materials is poor in an oxygen environment, and the oxidation weight loss makes the mechanical properties of carbon / graphite materials decrease significantly, thus limiting the wide application of carbon / graphite materials in the field of high-temperature oxygen atmosphere. Solving the problem of high-temperature oxidation protection of carbon / graphite materials is the prerequisite for making ful...

Claims

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Application Information

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IPC IPC(8): C10C3/02
Inventor 李四中顼栋
Owner 常州黑码服饰有限公司
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