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A high thermal stability spinning pitch preparation method and its special device

A technology with high thermal stability and asphalt, which is applied in the direction of melting and processing tar pitch/petroleum pitch/natural pitch, and chemical processing of tar pitch/petroleum pitch/natural pitch, etc. It can solve the problem of coking of adhering materials and reduce the content , reduce the reaction temperature and time, the effect of efficient mass transfer and separation

Active Publication Date: 2021-02-23
湖南东映碳材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, patents ZL201510972599.X and ZL201710362016.0 use film evaporators to remove light components under negative pressure. However, in practical application of this technology, it is difficult to effectively update the materials adhered to the inner wall of the equipment, and long-term reaction will cause The "coking" of the adhered material has to add a filter device to remove the coked carbon particles generated in the later process of the product

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  • A high thermal stability spinning pitch preparation method and its special device

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Embodiment 1

[0021] The high thermal stability spinning pitch preparation method can be used as a special device, which consists of a reactor cover 1, a reactor body 2, a filter screen and a porous plate 3, a receiving tank bottom cover 4, a tank bottom pump 5, and a vacuum system 6 and granulation equipment 7 composition. The top of the reaction kettle body 2 is equipped with a kettle cover 1, a filter screen and a porous plate 3 are installed in the middle of the interior, and the bottom is a receiving kettle bottom cover 4, which is connected to the bottom pump 5 of the kettle, and the bottom pump 5 of the kettle is connected to the granulation equipment 7 connection, the kettle cover 1 is equipped with a feed valve 1-1, an air outlet valve 1-2, and a stirring 1-3, and the lower part of the reaction kettle body 2 perforated plate is equipped with an inlet pipe valve 2-1 and an exhaust pipe valve 2-2, and through The exhaust pipe valve 2-2 is connected with the vacuum system 6.

[0022]...

Embodiment 2

[0027] The filter screen is 3000 mesh, the diameter of the porous plate is 800mm, the aperture is 0.05mm, and the number of holes is 4 holes / cm 2 , the pores are uniformly distributed.

[0028] Use 250kg of coal tar pitch with a softening point of 120°C, melt it and put it into the special device through the feed valve 1-1, heat it to 410°C, and feed 10L / kg∙min (2500L / min) nitrogen through the inlet pipe valve 2-1 , Nitrogen enters the material through the perforated plate 3, the stirring rate is 800rpm, the waste gas is extracted from the outlet valve 1-2 with a slight negative pressure, reacted for 15hr, and obtained asphalt with a softening point of 290°C.

[0029] (2) Cool down and keep the temperature of the reactor body 2 at 330°C, close the outlet valve 1-2, the inlet pipe valve 2-1, open the exhaust pipe valve 2-2, adjust the vacuum system 6 to 1000Pa, and pass the feed valve 1 -1 Pressurized to 0.4MPa, the asphalt falls slowly to form asphalt strands with a diameter ...

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Abstract

The invention discloses a high thermal stability spinning pitch preparation method and a special device thereof. The mesophase-inverted precursor pitch is heated to 350-450°C, the stirring rate is 100-1000rpm, and an inert gas bubble of 2-40L / kg is introduced. ∙min, control the diameter of the air bubbles passing through the porous plate at 0.03-0.5mm, react for 2-30hrs, until the softening point is 250-300°C. Then pressurize and extrude through the filter screen and holes with a pore size of 0.03-0.5mm, and extract the waste gas generated by decomposition and separation through a vacuum system. The pitch strands are collected by falling and re-melted and granulated to obtain mesophase pitch. The reaction device consists of a heated reaction kettle body, kettle cover, filter screen and perforated plate, receiving tank bottom cover, tank bottom pump, granulation equipment and vacuum system. The invention is suitable for the preparation of high-viscosity spinning pitch materials, and can obtain high-quality spinning pitch with a thermal weight loss of less than 0.4% at 330°C.

Description

technical field [0001] The invention relates to a method and a device for preparing spinning pitch, in particular to a method and a special device suitable for preparing high thermal stability spinning pitch from heat-sensitive raw materials. Background technique [0002] Spinning pitch is mainly used in the preparation of pitch-based carbon fibers, and it is a fused-ring aromatic compound with extremely high performance requirements. In order to obtain high-quality carbon fibers, there are extremely high requirements on the solid impurity content, low molecular weight compound content, and thermal stability of spinning pitch. Due to the complexity of the asphalt itself and its molecular structure, it is not only necessary to heat treat the asphalt for thermal condensation, but also to remove the small molecules in the asphalt that cannot participate in the reaction and the long fatty chains that are easy to break. The viscosity of the asphalt will be greatly increased, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/02C10C3/10
CPCC10C3/02C10C3/10
Inventor 刘金水伍孝叶崇李凯黄东沈威威张仕杰
Owner 湖南东映碳材料科技股份有限公司