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Preparation method of intermediate-phase asphalt

A mesophase pitch and asphalt technology, which is applied in the field of mesophase pitch preparation, can solve the problems of high softening point of mesophase pitch and cannot meet the requirements for preparing advanced carbon materials, and achieve the effect of increased fluidity and low softening point of pitch

Active Publication Date: 2013-04-24
CHANGZHOU HEIMA NEW CARBON TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is: to solve the technical problem that the mesophase pitch prepared by the existing method has a high softening point and cannot meet the requirements for preparing high-grade carbon materials. The present invention provides a method for preparing coal-based or petroleum-based mesophase pitch , the softening point of the mesophase pitch prepared by it is lower than 260°C, which can be used to manufacture a variety of important carbon materials, such as needle coke, mesophase pitch-based carbon fiber, mesophase pitch-based carbon negative electrode material, mesophase pitch-based carbon / Carbon composite materials, mesophase pitch-based carbon foam, high-temperature lubricants, catalyst supports, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 800g of medium-temperature coal tar pitch with a softening point of 75°C, put 20g of hydrogen fluoride into a Monel autoclave, feed nitrogen gas at a flow rate of 2L / min, stir with a stirrer at a stirring rate of 250r / min, and feed propylene when the temperature rises to 140°C. The pressure was kept at 3 MPa, and the alkylated pitch was obtained by staying for 4 hours. After the pressure is released, the hydrogen fluoride is volatilized, and the alkylated pitch is heat-treated at 8MPa pressure and 390°C for 10 hours, and then stay at 420°C at a vacuum of 100mmHg for 1 hour to obtain 100% optically anisotropic mesophase pitch. , The softening point is 259°C.

[0016] Among them, the mesophase content is estimated by polarizing microscope; the softening point measurement method: put 1.5 grams of mesophase pitch powder into the sample tube (the side tube is fed with nitrogen), place it in a salt bath, and then heat up at a rate of 2 to 3K / min Raise the temperature at...

Embodiment 2

[0018] Take 800g of medium-temperature coal tar pitch with a softening point of 90°C, put 120g of hydrogen fluoride into a Monel autoclave, feed nitrogen gas at a flow rate of 4L / min, stir with a stirrer at a stirring rate of 300r / min, and feed propylene when the temperature rises to 140°C. The pressure was kept at 15MPa, and the alkylated pitch was obtained by staying for 6 hours. After the pressure is released, the hydrogen fluoride is volatilized, and the alkylated pitch is heat-treated at 10 MPa pressure and temperature 390°C for 10 hours, and then stay at 420°C for 2 hours at a vacuum of 100 mmHg to obtain 100% optically anisotropic mesophase pitch. , The softening point is 255°C.

Embodiment 3

[0020] Take 800g of petroleum asphalt with a softening point of 92°C, put 120g of hydrogen fluoride into a Monel autoclave, feed nitrogen, flow rate 1L / min, stir with a stirrer, stirring rate 200r / min, feed propylene when the temperature rises to 140°C, pressure Keep it at 15MPa and stay for 4 hours to get alkylated pitch. After the pressure is removed, the hydrogen fluoride is volatilized, and the alkylated pitch is heat-treated at 5 MPa pressure and 400°C for 10 hours, and then stay at 420°C for 3 hours in a vacuum of 100 mmHg to obtain 90% optically anisotropic mesophase pitch. , The softening point is 258°C.

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Abstract

The invention relates to a preparation method of intermediate-phase asphalt, in particular to the preparation method of the intermediate-phase asphalt in a coal system or a petroleum system, and the method comprises the following two steps: 1) selecting coal asphalt or petroleum asphalt as raw material, and adding olefin and a friedel-crafts alkylation catalyst for alkylation of the raw material asphalt; and 2) performing pyrocondensation polymerization on the alkylated asphalt for getting a finished product. By adopting the preparation method, the technical problems that the intermediate-phase asphalt prepared by the existing method is high in softening point and can not meet the requirements for preparing high-grade carbon materials can be solved, the intermediate-phase asphalt preparedby the preparation method can be used for manufacturing various important carbon materials, such as needle coke, intermediate-phase asphalt-based carbon fiber, intermediate-phase asphalt-based carbonnegative pole material, intermediate-phase asphalt-based carbon / carbon composite material, intermediate-phase asphalt-based foam carbon, high-temperature lubricant, catalyst carriers and the like.

Description

technical field [0001] The invention relates to a preparation method of mesophase pitch, in particular to a preparation method of coal-based or petroleum-based mesophase pitch. Background technique [0002] Mesophase pitch is a polymer composed of a variety of discoid polycyclic aromatic hydrocarbons with a relative molecular mass of 370-2000. Due to its abundant raw materials, low price, high carbon residue rate, high oxidation activity, high purity, low viscosity, Spinability and other advantages are used to manufacture a variety of important carbon materials, such as needle coke, mesophase pitch-based carbon fiber, mesophase pitch-based carbon anode material, mesophase pitch-based carbon / carbon composite material, mesophase pitch-based foam Carbon, high temperature lubricants, catalyst supports, etc. Among them, needle coke is the only material for ultra-high-power electrodes (UHP) used in ultra-high-power electric furnace steelmaking; the specific strength and specific ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/02
Inventor 李四中琐栋俞庆旸
Owner CHANGZHOU HEIMA NEW CARBON TECH
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