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Preparation method of graphite material for oxygen-nitrogen-hydrogen analysis instrument

A technology for analysis instruments and graphite materials, which is applied in the field of preparation of graphite materials for oxygen, nitrogen and hydrogen analysis instruments, can solve problems such as difficult to meet, and achieve the effects of preventing product adhesion, preventing product cracking, and reducing resistance between materials

Active Publication Date: 2020-10-09
CENT SOUTH UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Usually, the raw material aggregate for the production of massive high-purity graphite products is calcined petroleum coke or calcined pitch coke, the nitrogen content of the raw material is generally 0.2% to 1.5%, and the nitrogen content of the product after graphitization is generally 0.004% to 0.05%. It is difficult to meet the requirement that the nitrogen content of the graphite crucible used for oxygen, nitrogen and hydrogen analysis instruments is less than 1ppm

Method used

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  • Preparation method of graphite material for oxygen-nitrogen-hydrogen analysis instrument
  • Preparation method of graphite material for oxygen-nitrogen-hydrogen analysis instrument
  • Preparation method of graphite material for oxygen-nitrogen-hydrogen analysis instrument

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Embodiment 1

[0024] In this embodiment, the main performance indicators of aggregate microcrystalline graphite and binder coal tar pitch are as follows: microcrystalline graphite: ash content 0.32%; nitrogen content 0.013%; degree of graphitization 93.3%; coal tar pitch: softening point 85°C; Toluene insoluble matter 22.4%; quinoline insoluble matter 7.1%; specific process see figure 1 , the production process of the present embodiment is carried out according to the following steps:

[0025] Step 1: Crush the dried microcrystalline graphite until it passes through a 0.15m sieve, of which the components larger than 0.075mm account for 31%, and use it as aggregate for later use; heat the coal tar pitch to 160°C to fully melt;

[0026] Step 2: weigh according to the percentage by weight of microcrystalline graphite 76%, coal tar pitch 24%;

[0027] Step 3: Put the weighed microcrystalline graphite into the mixing equipment under normal pressure, then add fully melted coal tar pitch, mix at ...

Embodiment 2

[0061] In this embodiment, the main performance indicators of aggregate microcrystalline graphite and binder coal tar pitch are as follows: microcrystalline graphite: ash content 0.32%; nitrogen content 0.013%; degree of graphitization 93.3%; warm coal tar pitch: softening point 85°C ; Toluene insoluble matter 22.4%; Quinoline insoluble matter 7.1%; Specific process see figure 1 , the production process of the present embodiment is carried out according to the following steps:

[0062] Step 1: Crush the dried microcrystalline graphite until it passes through a 0.15m sieve, of which the components larger than 0.075mm account for 39%, and use it as aggregate for later use; heat the coal tar pitch to 165°C to fully melt;

[0063] Step 2: weigh according to the percentage by weight of microcrystalline graphite 78%, coal tar pitch 22%;

[0064] Step 3: Put the weighed microcrystalline graphite into the mixing equipment under normal pressure, then add fully melted coal tar pitch, m...

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Abstract

The invention discloses a preparation method of a graphite material for an oxygen-nitrogen-hydrogen analysis instrument. The preparation method comprises the following steps: 1) preparing a paste material; 2) extruding into a green body bar; 3) carbonizing to prepare a carbonized bar; and 4) purifying to obtain the high-purity graphite material for the oxygen-nitrogen-hydrogen analysis instrument.The low-nitrogen natural microcrystalline graphite is used as a main raw material so that compared with the existing production technology which generally adopts calcined petroleum coke and calcinedpitch coke as raw materials, the nitrogen content of the raw materials is remarkably reduced, and the production of the graphite material meeting the requirements of oxygen-nitrogen-hydrogen analysisinstruments is facilitated. The natural microcrystalline graphite has the advantages of high graphitization degree, good lubricity and the like so that the natural microcrystalline graphite is used asa raw material to be beneficial to reducing the resistance among materials during forming, and a product with a fine and compact structure and good uniformity is obtained; in the carbonization process, a specific heating system is adopted so that the product can be effectively prevented from cracking, the carbon residue rate of the binder is improved, and the density and strength of the product are further improved.

Description

technical field [0001] The invention belongs to the field of deep processing of graphite, and in particular relates to a preparation method of a graphite material for an oxygen, nitrogen and hydrogen analysis instrument. Background technique [0002] The detection of oxygen, nitrogen and hydrogen content in materials has been paid more and more attention. Most of the instruments for testing oxygen, nitrogen and hydrogen use the electrode pulse furnace as the heat source. Under the protection of high-purity helium, the solid sample is melted in the hot graphite crucible, and the hydrogen is released in the form of hydrogen gas; oxygen in various states such as oxides is The carbon reduction from the graphite crucible is released in the form of carbon monoxide and carbon dioxide, and is completely converted into carbon dioxide by hot copper oxide; various states of nitrogen are released as gaseous simple substances; the complete release of nitrogen often requires a high temper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/3504C04B35/52C04B35/622
CPCC04B35/522C04B35/622G01N21/3504
Inventor 李建新黄启忠
Owner CENT SOUTH UNIV
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