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Preparation method for intermediate phase asphalt

A kind of technology of mesophase pitch and polymerization kettle

Inactive Publication Date: 2009-09-09
汝南县东旭碳材塑料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When preparing high-performance pitch-based carbon materials and other advanced carbon materials, it is required that the raw material pitch forming the mesophase has low heteroatom and ash content, uniform structural composition, high aromaticity, low condensation degree, and rich alkyl short chains in the structure. and naphthenic groups, etc. However, the commonly used raw materials such as coal tar pitch and petroleum pitch cannot fully meet the above requirements, and they need to be pretreated or / and modified to remove ash impurities and adjust the structure and composition distribution of raw materials
In this way, the mesophase pitch prepared by using petroleum pitch and coal tar pitch has some disadvantages, such as complicated preparation process, high preparation cost, and little improvement in carbon fiber performance.
At present, there are also methods for preparing mesophase pitch from refined naphthalene, but these methods have deficiencies in temperature and pressure selection, and the resulting products have poor performance, high softening point, and poor spinnability

Method used

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  • Preparation method for intermediate phase asphalt
  • Preparation method for intermediate phase asphalt
  • Preparation method for intermediate phase asphalt

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The method comprises the following steps: (1) batching refined naphthalene, hydrogen fluoride and boron trifluoride in a mass ratio of 10:1:2, and feeding them into a polymerization kettle made of Monel 400 material; (2) starting stirring and controlling the pressure 10MPa, temperature 200°C, react for 4 hours; (3) Then increase the pressure to 25MPa, raise the temperature to 310°C, continue to react for 4 hours to obtain mesophase pitch. In the process of steps (2) and (3), nitrogen is purged for purification, and nitrogen is introduced from the bottom of the polymerization tank.

[0028] The optical anisotropy micromorphology of the product that embodiment 1 makes sees figure 1 .

Embodiment 2

[0030] The method comprises the following steps: (1) batching refined naphthalene, hydrogen fluoride and boron trifluoride in a mass ratio of 10:3:4, and feeding them into a polymerization kettle made of Monel 400 material; (2) starting stirring and controlling the pressure 15MPa, temperature 190°C, react for 5 hours; (3) Then raise the pressure to 27MPa, raise the temperature to 300°C, continue to react for 5 hours to obtain mesophase pitch. In the process of steps (2) and (3), nitrogen is purged for purification, and nitrogen is introduced from the bottom of the polymerization tank.

[0031] The optical anisotropy micromorphology of the product that embodiment 2 makes sees figure 2 .

Embodiment 3

[0033] The method comprises the following steps: (1) feeding refined naphthalene, hydrogen fluoride and boron trifluoride in a mass ratio of 10:4:5 into a polymerization kettle made of Monel 400; (2) starting stirring and controlling the pressure 20MPa, temperature 160°C, react for 5 hours; (3) Then increase the pressure to 29MPa, raise the temperature to 270°C, continue to react for 5 hours to obtain mesophase pitch. In the process of steps (2) and (3), nitrogen is purged for purification, and nitrogen is introduced from the bottom of the polymerization tank.

[0034] The optical anisotropy micromorphology of the product that embodiment 3 makes sees image 3 .

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Abstract

The invention provides a preparation method for intermediate phase asphalt, which comprises the following steps: (1) refined naphthalene, fluorine hydride and boron triflouride are mixed according to the mass ratio of 10:1-5:2-6 and sent into a polymeric kettle; (2) the polymeric kettle is opened and the mixture is stirred, the pressure is controlled to be 10-25 Mpa, the temperature is 150-200 DEG C, and the reaction lasts for 4-6 hours; (3) and the pressure is increased to be 25-30Mpa, the temperature is increased to be 260-310 DEG C and the reaction continously lasts for 4-6 hours, thus obtaining the intermediate phase asphalt. The method has simple process and low preparation cost. Except of few of superficial globules, most of the optical anisotropy microscopic morphology of the obtained intermediate phase asphalt presents streamline state or large field melting bodily form state. The intermediate phase asphalt is excellent, has low softening point, low ash content, good spinnability, excellent structure, high tensile strength and module.

Description

technical field [0001] The invention relates to a method for preparing mesophase pitch, in particular to a method for preparing mesophase pitch by using refined naphthalene as a raw material. Background technique [0002] Pitch-based carbon materials and high thermal conductivity carbon-based materials are new materials for military and civilian use. The raw material for manufacturing pitch-based carbon materials and high thermal conductivity carbon-based materials is mesophase pitch. The more commonly used mesophase pitch is made of petroleum pitch and coal tar pitch. Prepared. When preparing high-performance pitch-based carbon materials and other advanced carbon materials, it is required that the raw material pitch forming the mesophase has low heteroatom and ash content, uniform structural composition, high aromaticity, low condensation degree, and rich alkyl short chains in the structure. and naphthenic groups, etc. However, the commonly used raw materials such as coal ...

Claims

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Application Information

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IPC IPC(8): C10C3/02
Inventor 郭有镜巫得收
Owner 汝南县东旭碳材塑料有限公司
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