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Graphitized short fibers and composition thereof

A technology of graphitization and short fibers, applied in fiber processing, fiber chemical characteristics, textiles and papermaking, etc., can solve problems such as difficult curing reactions, and achieve the effects of excellent mechanical strength, high thermal conductivity and softness

Inactive Publication Date: 2012-03-14
TEIJIN LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, for the rubber composition, a vulcanizing agent, a vulcanization accelerator, etc. are added to the rubber to cure, but if it is desired to fill the rubber with a high degree of normal carbon fiber, it is difficult to carry out the curing reaction of the rubber, and it is difficult to highly fill the carbon fiber.

Method used

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  • Graphitized short fibers and composition thereof
  • Graphitized short fibers and composition thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] The main raw material is mesophase pitch containing condensed polycyclic hydrocarbon compounds. The optical anisotropy ratio is 100%, and the softening point is 286°C. Using a cap with a hole diameter of 0.2 mmφ, heated air was sprayed from the slit at a speed of 9700 m / min to draw molten pitch to produce a pitch-based carbon fiber precursor with an average diameter of 15.5 μm. The spinning temperature at this time was 341° C., and the melt viscosity was 9.5 Pa·S (95 poise). The spun pitch-based carbon fiber precursor is collected on a belt to form a net, and then cross-laid to form a unit area weight of 380g / m 2 A pitch-based carbon fiber precursor network comprising a pitch-based carbon fiber precursor.

[0089] The pitch-based carbon fiber precursor web was heated from 170° C. to 320° C. at an average temperature increase rate of 7° C. / min in air to infusible it. At this time, the amount of oxygen attached to the pitch-based infusible fiber web was 6.6 wt%. Furth...

Embodiment 2

[0094] 15 parts by weight of the pitch-based graphitized short fibers (short fibers B) obtained in Example 1 and polyether-modified polydimethylsilane were mixed using an autorotation-revolving mixer (trade name "Awatori Rentaro ARV310" manufactured by Sinki Corporation). 100 parts by weight of oxane (trade name "BYK-302" manufactured by Big Chemical Co., Ltd.) was mixed for 6 minutes to obtain a rubber composition. After treating this at 80° C., it was cured over 70 minutes. The curing time of BYK-302 at 80°C is 70 minutes. That is, the curing time of the thermally conductive rubber composition is 1.0 times the curing time of the rubber component.

[0095] Next, the obtained rubber composition was press-processed by a vacuum press machine (Kitagawa Seiki Co., Ltd.) to obtain a flat composite molded body with a thickness of 0.5 mm, which was cured at 130° C. for 2 hours to produce a sheet-shaped thermally conductive material. Shaped body. The thermal conductivity of the she...

Embodiment 3

[0101] The main raw material is mesophase pitch containing condensed polycyclic hydrocarbon compounds. The optical anisotropy ratio is 100%, and the softening point is 283°C. Using a cap with a hole diameter of 0.2 mmφ, heated air was sprayed from the slit at a speed of 8500 m / min to draw molten pitch to produce a pitch-based carbon fiber precursor with an average diameter of 14.5 μm. The spinning temperature at this time was 335° C., and the melt viscosity was 10.5 Pa·S (105 poise). The spun pitch-based carbon fiber precursor is collected on a belt to form a net, and then cross-laid to form a weight per unit area of ​​400g / m 2 A pitch-based carbon fiber precursor network comprising a pitch-based carbon fiber precursor.

[0102] The pitch-based carbon fiber precursor web was heated from 170° C. to 320° C. at an average temperature increase rate of 6° C. / min in air to prevent melting. The amount of oxygen attached to the pitch-based infusible fiber web at this time was 6.5 w...

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Abstract

Pitch-based graphitized short fibers formed from mesophase pitch as a raw material, the fibers having an average fiber diameter of 5-20 [mu]m, a percentage of fiber diameter dispersion to the average fiber diameter, CV value, of 8-15%, a number-average fiber length of 20-500 [mu]m, and a crystallite size in the growth direction of the hexagonal net plane, La, of 30 nm or larger. When an end of the filler is examined with a transmission electron microscope, the graphene sheets are closed. When examined with a scanning electron microscope, the surface is substantially flat. The fibers have an R value in the range of 0.01 to 0.07, the value being the relative-intensity ratio between the intensity of a Raman band around 1,360 cm-1 (ID) and the intensity of a Raman band around 1,580 cm-1 (IG), (ID) / (IG), determined by laser Raman spectroscopy. The fibers can be incorporated into a rubber composition in a large amount without inhibiting the curing of the composition.

Description

technical field [0001] The present invention relates to pitch-based graphitized short fibers. The pitch-based graphitized short fibers of the present invention have excellent surface crystallinity, and are suitable for use as thermally conductive fillers and reinforcing agents for resins or rubbers. Among them, the pitch-based graphitized short fibers of the present invention can provide a rubber composition highly filled with graphitized short fibers without hindering the curing of rubber when a composition is produced from graphitized short fibers and a rubber component. Background technique [0002] Carbon fiber has higher thermal conductivity than other synthetic polymers. However, for applications aimed at heat treatment, it is required to further increase the thermal conductivity of carbon fibers. The thermal conductivity of commercially available PAN-based carbon fibers is generally lower than 200 W / (m·K). This is because PAN-based carbon fibers are so-called non-g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/145D01D5/00D01D5/42
CPCC08J5/042C08K7/06D01F9/145Y10T428/2918
Inventor 樱井博志佐野弘树原宽高木正一
Owner TEIJIN LTD
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