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Preparation method for mesophase pitch-based high-thermal conductivity graphite material

A technology of mesophase pitch and high thermal conductivity graphite, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as difficulty in large-scale preparation of high thermal conductivity graphite materials, and achieve regular arrangement, short production cycle, and high price. cheap effect

Inactive Publication Date: 2013-01-30
华侨大学厦门园区 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problem that the large-scale preparation of the above-mentioned high thermal conductivity graphite material is relatively difficult, the present invention proposes a method for preparing a high thermal conductivity graphite material based on mesophase pitch, and its technical scheme is as follows:

Method used

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  • Preparation method for mesophase pitch-based high-thermal conductivity graphite material

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Experimental program
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Effect test

Embodiment 1

[0025] The existing mesophase pitch can be prepared in many ways, such as:

[0026] Mesophase pitch can be prepared in two ways:

[0027] The first is to use pure aromatics as raw materials, such as alkylbenzene, naphthalene, methylnaphthalene, anthracene and phenanthrene, etc. to directly synthesize; generally, HF / BF3, AlCl3, ZrO2 / SO42-solid super acid, etc. are used as catalysts, and the preparation method can be divided into for:

[0028] 1. Heat treatment method: Tetrabenzophenazine is heat-treated at a temperature higher than 500°C for more than 3 hours, and each molecule is directly converted into 100% mesophase pitch after removing 3 hydrogen atoms.

[0029] 2. AlCl3 catalytic method: heat-treat anthracene or naphthalene in the presence of AlCl3 and a small amount of water or nitrogen flow for several hours to cause cationic condensation reaction to produce mesophase pitch with a C / H atomic ratio of 1.22-1.33.

[0030] 3. HF / BF3 catalytic method: Use HF / BF3 as aromat...

Embodiment 2

[0041] Crushing 10: Crushing 200g of mesophase pitch into particles with a particle size of ≤0.154mm, and putting them into a container;

[0042] Foaming 20: Place in an autoclave. The autoclave is filled with nitrogen, and the nitrogen pressure is 1-10MPa. In an autoclave, the mesophase pitch was heated to 390° C. and kept at a constant temperature for 4 hours to obtain an initial foam-like product.

[0043] Prefabrication 30: Place the initial foamed product in a hot-press furnace under an inert atmosphere at a heating rate of 0.1-100°C / min and a pressure of 5-100MPa, and heat the initial product to 600°C-2000°C to obtain an intermediate product .

[0044] Sintering 40: placing the intermediate product in a graphitization furnace under argon flow, heating the intermediate product to 2000-3000°C at a heating rate of 1-50°C / min. After natural cooling, the graphite material with high thermal conductivity can be obtained. The prepared material has a density of 2.08g / cm3 and ...

Embodiment 3

[0046] Crushing 10: Crushing 200g of mesophase pitch into particles with a particle size of ≤0.154mm, and putting them into a container;

[0047] Foaming 20: Place in an autoclave. The autoclave is filled with nitrogen, and the nitrogen pressure is 1-10MPa. In an autoclave, the mesophase pitch was heated to 420°C and held at constant temperature for 3 hours to obtain an initial foam-like product.

[0048] Prefabrication 30: Place the initial foam product in a hot-pressed furnace under an inert atmosphere at a heating rate of 0.1-100°C / min and a pressure of 5-100MPa, and heat the initial product to 600°C-2000°C to obtain an intermediate product.

[0049] Sintering 40: place the intermediate product in a graphitization furnace under argon flow, and heat the intermediate product to 2000-3000° C. at a heating rate of 1-50° C. / min. After natural cooling, the graphite material with high thermal conductivity can be obtained. The prepared material has a density of 2.14g / cm3 and a t...

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Abstract

The invention discloses a preparation method for a mesophase pitch-based high-thermal conductivity graphite material. The preparation method is characterized by comprising the following steps: crushing mesophase pitch which uses coal tar, petroleum residue or a naphthalene molecule as a raw material to obtain a pitch particle with a particle size of no more than 0.154 mm; then putting the pitch particle into an autoclave, gradually heating the pitch particle to a temperature of 370 to 550 DEG C in an inert gas atmosphere and taking the pitch particle out after natural cooling; placing the pitch particle into a hot pressing furnace, gradually heating the pitch particle to a temperature of 600 to 2000 DEG C under the protection of an inert gas atmosphere at a pressure of 5 to 100 MPa and taking the pitch particle out after cooling so as to obtain an intermediate product; and placing the intermediate product in a graphitization furnace, gradually heating the intermediate product to a temperature of 2000 to 3000 DEG C in an inert gas flow and carrying out discharging after natural cooling so as to obtain a final product. According to the invention, the structure of the pitch is adjusted through adjusting foaming temperature of the pitch, so the pitch is allowed to have good plasticity, and components with a caking property in the pitch are retained; thus, the graphite material with high thermal conductivity can be prepared.

Description

technical field [0001] The invention relates to a preparation method of a high thermal conductivity graphite material. Background technique [0002] With the rapid development of science and technology, the problem of heat dissipation has become the key to the development of many high-tech electronic products, thus putting forward higher and higher requirements for the performance of heat dissipation devices as an important part of the thermal control system. Moreover, such heat dissipation devices often require Work in complex and demanding environments. For example, heat sinks for high-power electronic instruments of aerospace vehicles, nose cones for missiles and aircraft, solid rocket motor nozzles, high-power density devices for communication satellites, high-power LED devices, etc., not only require materials to have low density and good Mechanical properties also require the material to have good thermal conductivity. As a basic physical property of carbon graphite ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/205
Inventor 李四中
Owner 华侨大学厦门园区