JPS63139051A - Manufacture of high density high strength carbon material - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

Detailed Description of the Invention "Industrial Application Field" The present invention is applicable to steelmaking electrodes, electric brushes, nuclear reactor materials,
The present invention relates to a method for manufacturing high-density, high-strength carbon materials that are used in a wide range of applications such as mechanical materials.

"Prior Art" Carbon materials are usually produced by adding a binder to coke aggregate, kneading it, molding it, firing it, and then graphitizing it.

However, according to this method, the process of adding binder to aggregate coke and mixing it is complicated, which increases manufacturing costs. However, the working environment was poor and there were hygiene issues.

In addition, carbon materials produced by this method become porous due to the volatile matter generated during the firing process due to the porous nature of the aggregate coke and the presence of cool pitch and synthetic resins used as binders. , it is dense and difficult to have high strength, the density is about 1.5 to 1.7 g/-, and the bending strength is at most 5o.

Pupils/-Standing.

Conventionally, in order to eliminate the drawbacks of the conventional manufacturing methods as mentioned above, carbonaceous carbon or river carbon is added to mesophase-containing pitch and heat treated, and the resulting heat-treated product is molded and fired as it is or after pulverization. Alternatively, there is a method for producing high-density and high-strength carbon materials through graphitization treatment.
For example, it is disclosed in Japanese Patent Application Laid-open No. 136906/1983.

"Problems to be Solved by the Invention" According to the method disclosed in JP-A-61-136906,
It is said that it is possible to uniformly adhere mesophase-containing pitch to carbonaceous carbon or graphitic carbon, and that a high-density carbon material can be obtained by molding and firing the heat-treated product as it is or after crushing. Because the caking component is adjusted by a heat treatment process in which mesophase-containing pinches are attached, the caking force cannot be adjusted sufficiently, and the bending strength of the resulting carbon material is about 300 to 700 kg/c+J, making it difficult to use the product. The problem was that it was limited.

The present invention aims to solve such conventional problems.

``Means for Solving the Problems'' The present invention involves adding carbonaceous powder or graphite powder to tars or pinches, heating the mixture with stirring in a temperature range of 300 to 600°C, and then extracting it with a solvent. This is a method for producing a high-density, high-strength carbon material, which is characterized in that the extracted residue is calcined at a temperature range of 200 to 450°C, and then molded and fired.

The present invention will be explained in detail below.

The tars or pitches used in the present invention are not particularly limited in type, and either coal-based or petroleum-based tars can be used.

Examples of the carbonaceous powder or graphitic powder used in the present invention include coal coke, pinch coke, petroleum coke, carbon black, natural graphite, and quiche graphite.

Cools or pitches and the carbonaceous powder or graphite powder are charged into a reactor having a stirring function, stirred, and heat treated while the powder is dispersed in tars or pinches.

The heat treatment temperature is 300 to 600°C.

If the temperature is lower than 300°C, the production of viscous components, such as β component, will not be sufficient, and if it is higher than 600°C, the viscosity components will turn into coke, which is not preferable.

The heat-treated product thus obtained is extracted with a solvent.

The solvent used is a solvent with slightly lower extraction power than quinoline, such as benzene, in order to leave the viscous component.
Use toluene, pyridine, tar oil, etc.

Next, the residue after the extraction is separated, and the separation method may be vacuum filtration, heating filtration, centrifugation, gravity sedimentation, or the like.

The obtained extraction residue is calcined in a temperature range of 200 to 450° C. to volatilize and remove the solvent, and then molded as it is without using a binder, fired, and graphitized if necessary.

In removing the solvent, it is necessary to carry out a calcining treatment to volatilize and remove the solvent component, and to adjust the caking force by subjecting a portion of the caking component to a polycondensation reaction.

This is because while the viscous component acts as a binder and imparts sinterability when the compact is fired, it also generates a large amount of gas when the compact is fired, so if a large amount of the viscous component remains, This is because blisters and cracks occur in the molded body during firing, making it difficult to manufacture industrially useful large blocks.

The calcination treatment is necessary for industrially stably manufacturing large-sized carbon materials because the reactivity of these viscous components can be controlled in advance.

If the calcining salinity is below 200°C, the m-condensation reaction of the viscous components will be difficult to proceed, but if it exceeds 450°C, the binder ability of the viscous components will be lost, so the calcination treatment will be carried out at 200 to 45
It must be carried out in a temperature range of 0°C.

The calcined extraction residue can be molded and fired as it is or after pulverization without using a binder, and further graphitized if necessary, to obtain a high-density and high-strength carbon material.

"Example" Hereinafter, the present invention will be explained in more detail with reference to Examples.

Example 1 9500 g of tar pitch (softening point 90°C) and 500 g of calcined coal coke were placed in an autoclave and heated at 450°C for 1 hour while stirring, then oil in tar was added to the contents, extracted and filtered. An extraction residue was obtained.

This residue was calcined at 350°C for 5 hours, then pulverized and molded, then fired at too much°C, and further graphitized at 2500°C.

The characteristic values of the obtained graphitized block are shown in Table 1.

Example 2 Tar pinch (softening point 90°C) 9500g and graphite powder 5
00g into an autoclave and heat to 450°C while stirring.
After heating for 1 hour, extract in the same manner as in Example 1,
It was calcined, crushed, shaped, fired, and graphitized.

The characteristic values of the obtained graphitized block are shown in Table 1.

Table 1 "Effects of the Invention" As stated above, the method for producing a high-density, high-strength carbon material of the present invention can easily achieve extremely high bending strength of 800 kg/- or more without going through a kneading process. can produce high-density carbon materials.

Claims (1)

[Claims] Carbonaceous powder or graphite powder is added to tars or pitches, heated in a temperature range of 300 to 600°C with stirring, and then extracted with a solvent.
After calcination treatment in the temperature range of 00 to 450℃, molding,
A method for producing a high-density, high-strength carbon material, which involves firing.