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Method for preparing spinning-grade synthetic mesophase pitch

A technology of mesophase pitch and spinning grade, which is applied in the field of catalytic synthesis and preparation of mesophase pitch, can solve the problems of high impurity content of mesophase pitch, low yield and product performance, and high equipment material requirements, and achieves low equipment requirements, high resistance to The effect of low pressure capacity and corrosion resistance requirements, and the effect of saving equipment costs

Active Publication Date: 2019-12-31
ANHUI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the deficiencies in the prior art, the present invention provides a method for preparing spinning-grade synthetic mesophase pitch; the method can solve the problem of high impurity content and difficult removal of mesophase pitch produced by conventional methods in China, high requirements for equipment materials, and high yield. rate and low product performance

Method used

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  • Method for preparing spinning-grade synthetic mesophase pitch
  • Method for preparing spinning-grade synthetic mesophase pitch

Examples

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Embodiment 1

[0040] A method for preparing spinning grade synthetic mesophase pitch, comprising the steps of:

[0041] (1) Catalyst ZrCl 4 Add refined naphthalene, ZrCl 4 The mixing ratio with refined naphthalene is a molar ratio of 1: 100, and the resulting mixture was stirred and reacted for 5 hours under 280° C. 2 Carried out under the atmosphere to obtain a solid-liquid mixed product;

[0042] (2) The product obtained in step (1) is mixed with 5 times the volume of solvent pyridine, then the liquid and solid components in the product are separated by a medium-speed qualitative filter paper, and the pyridine solvent in the liquid component is distilled off to obtain polycyclic Aromatic oligomers;

[0043] (3) step (2) is made polycyclic aromatic hydrocarbon oligomer, at reaction temperature 420 ℃, reaction time 15 hours, normal pressure N 2 The thermal polycondensation reaction is carried out under conditions such as atmosphere to prepare mesophase pitch compounds.

[0044] (4) Adj...

Embodiment 2

[0046] A method for preparing spinning grade synthetic mesophase pitch, comprising the steps of:

[0047] (1) Catalyst ZrCl 4 Add refined naphthalene, ZrCl 4 The mixing ratio with refined naphthalene is a molar ratio of 2: 100, and the resulting mixture was stirred and reacted for 2 hours under 270°C temperature condition in the reactor, the reaction pressure was 0.6MPa, and the 2 Carried out under the atmosphere to obtain a solid-liquid mixed product;

[0048] (2) The product obtained in step (1) is mixed with 5 times the volume of solvent pyridine, then the liquid and solid components in the product are separated by a medium-speed qualitative filter paper, and the pyridine solvent in the liquid component is distilled off to obtain polycyclic Aromatic oligomers;

[0049] (3) step (2) is made polycyclic aromatic hydrocarbon oligomer, at reaction temperature 420 ℃, reaction time 15 hours, normal pressure N 2 The thermal polycondensation reaction is carried out under conditi...

Embodiment 3

[0052] A method for preparing spinning grade synthetic mesophase pitch, comprising the steps of:

[0053] (1) Catalyst ZrCl 4 Add methylnaphthalene, ZrCl 4 The mixing ratio with refined naphthalene is a molar ratio of 1.5: 100, and the resulting mixture is stirred and reacted for 3 hours under 280° C. 2 Carried out under the atmosphere to obtain a solid-liquid mixed product;

[0054] (2) The product obtained in step (1) is mixed with 5 times the volume of solvent pyridine, then the liquid and solid components in the product are separated by a medium-speed qualitative filter paper, and the pyridine solvent in the liquid component is distilled off to obtain polycyclic Aromatic oligomers;

[0055] (3) step (2) is made polycyclic aromatic hydrocarbon oligomer, at reaction temperature 420 ℃, reaction times 18 hours, normal pressure N 2 The thermal polycondensation reaction is carried out under conditions such as atmosphere to prepare mesophase pitch compounds.

[0056] (4) Adj...

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Abstract

The invention relates to a preparation method for spinning-grade synthetic mesophase pitch. The preparation method comprises the following steps: (1) adding a catalyst into a pure aromatic hydrocarboncompound, and carrying out a stirring reaction at 200-320 DEG C for 2-5 h under a reaction pressure of 0.6 MPa to obtain an aromatic hydrocarbon oligomer; and (2) subjecting the aromatic hydrocarbonoligomer to a reaction at a reaction temperature of 390-420 DEG C for 10-20 h to obtain the mesophase pitch. The invention discloses a process for preparing the mesophase pitch by adding ZrCl4 into anaromatic hydrocarbon compound as a catalyst and carrying out a polymerization reaction for the first time. Due to the directional catalytic action of ZrCl4, aromatic rings in the polymerization product, namely aromatic hydrocarbon oligomer are arranged in a chain shape, so the finally formed large-plane molecular structure of the mesophase pitch is guaranteed. Meanwhile, due to the fact that theZrCl4 catalyst is small in use amount and easy and convenient to remove, requirements for the pressure resistance, the air tightness and the corrosion resistance of equipment are low, so equipment cost is saved, and the prepared mesophase pitch meets the requirements of preparation of carbon fibers.

Description

technical field [0001] The invention relates to a method for preparing spinning-grade synthetic mesophase pitch, and belongs to the technical field of mesophase pitch prepared by catalytic synthesis. Background technique [0002] Mesophase pitch is an important raw material for preparing high-performance carbon materials such as high-performance carbon fibers, needle coke, carbon / carbon composite materials, lithium-ion secondary battery anode materials, and mesophase pitch-based carbon foam. In particular, the high-performance carbon fiber prepared by using mesophase pitch has unique properties such as high thermal conductivity, high modulus and high strength, which are significantly better than polyacrylonitrile-based carbon fiber. Therefore, mesophase pitch-based carbon fiber material products are widely used in aviation and aerospace , national defense and military industry, new energy storage devices, atomic energy industry (nuclear reactor) and other cutting-edge fields...

Claims

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Application Information

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IPC IPC(8): C10C3/02D01F9/145
CPCC10C3/02D01F9/145
Inventor 李伏虎沈曾民刘辉
Owner ANHUI UNIV OF SCI & TECH
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