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A kind of preparation method of large-diameter high-strength medium-modulus carbon fiber and high-strength high-modulus carbon fiber

A large-diameter, carbon fiber technology, applied in the field of large-diameter carbon fiber preparation, can solve the problems of prolonged pre-oxidation time, insufficient pre-oxidation of the core, and difficulty in jumping out of the thinking mode, and achieve simple process operation methods and radial structure differences. Small, improves collimation effect

Active Publication Date: 2021-06-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For large-diameter fibers, it is generally believed that during the pre-oxidation process of PAN fibers, oxygen enters the skin to undergo oxidation reactions, and the skin forms a dense network trapezoidal structure that hinders the further diffusion of oxygen to the core, resulting in core pre-oxidation. Insufficient, forming a skin-core structure
People use the method of prolonging the pre-oxidation time to make oxygen slowly enter the fiber, but in order to improve the production efficiency, the pre-oxidation time cannot be extended without limit. Therefore, in order to balance the production efficiency, the skin-core structure of the large-diameter fiber cannot be eliminated. Fiber can only prepare high-strength carbon fiber
At the same time, people think that the air atmosphere is inexhaustible, convenient, quick and cheap. In addition, the inventor of polyacrylonitrile-based carbon fiber first used air to pre-oxidize the fiber. Break out of the thinking mode bound by traditional crafts

Method used

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  • A kind of preparation method of large-diameter high-strength medium-modulus carbon fiber and high-strength high-modulus carbon fiber
  • A kind of preparation method of large-diameter high-strength medium-modulus carbon fiber and high-strength high-modulus carbon fiber
  • A kind of preparation method of large-diameter high-strength medium-modulus carbon fiber and high-strength high-modulus carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Preparation of spinning dope

[0040] Using azobisisobutyronitrile as the initiator and dimethyl sulfoxide as the solvent, mix acrylonitrile, itaconic acid and methyl acrylate at a molar ratio of 98.5:0.5:1 and add them to the polymerization reaction vessel. The polymerization reaction temperature is 62°C , the polymerization reaction time is 23 hours, the stirring rate is 50rpm, and the spinning stock solution is obtained, and the spinning stock solution is obtained after the single and defoaming, and the acrylonitrile copolymer with a polymer molecular weight of 185,000 is obtained. The sulfone accounts for 78% of the mass percent concentration of acrylonitrile and dimethyl sulfoxide, the azobisisobutyronitrile accounts for 0.15% of the acrylonitrile mole fraction, and the viscosity of the spinning dope measured by a rotational viscometer at 25° C. is 8600 poise.

[0041] (2) Multi-stage coagulation molding of spinning dope

[0042] Adopt the spinneret that hole ...

Embodiment 2

[0061] (1) Preparation of spinning dope

[0062] Using azobisisobutyronitrile as the initiator and dimethyl sulfoxide as the solvent, mix acrylonitrile, itaconic acid and methyl acrylate at a molar ratio of 98.5:0.5:1 and add them to the polymerization reaction vessel. The polymerization reaction temperature is 60°C , the polymerization reaction time is 23 hours, the stirring rate is 55rpm, and the spinning stock solution is obtained, and the spinning stock solution is obtained after the single and defoaming, and the acrylonitrile copolymer with a polymer molecular weight of 175,000 is obtained. The sulfone accounts for 79% of the mass percent concentration of acrylonitrile and dimethyl sulfoxide, the azobisisobutyronitrile accounts for 0.20% of the acrylonitrile mole fraction, and the viscosity of the spinning dope measured by a rotational viscometer at 25° C. is 7500 poise.

[0063] (2) Multi-stage solidification of spinning dope

[0064] Adopt the spinneret that hole diame...

Embodiment 3

[0073] (1) The preparation of spinning dope is the same as in Example 1

[0074] (2) Multi-stage solidification of spinning dope.

[0075] Adopting the spinneret whose aperture is 0.10mm, the linear velocity of the fiber at the spinneret is 5.78m / min, and the fiber passes through the air layer of 10mm after leaving the spinneret, and then enters the first coagulation bath, and the temperature of the first coagulation bath is 30 ℃, the coagulation bath adopts dimethyl sulfoxide aqueous solution, wherein the volume content of dimethyl sulfoxide solvent is 76%, the coagulation time is 2.5 minutes, and the coagulation draft ratio is 3; the speed of coagulation filaments exiting the first coagulation bath is 17.34m / min, then the fiber enters the second coagulation bath, the temperature of the second coagulation bath is 30°C, the coagulation bath adopts the aqueous solution of dimethyl sulfoxide, wherein the volume content of dimethyl sulfoxide solvent is 50%, the coagulation time ...

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Abstract

The invention relates to a method for preparing large-diameter polyacrylonitrile (PAN)-based high-strength middle mold and high-strength high-modulus carbon fiber. The invention adopts dry-wet spinning to prepare large-diameter precursors, and the precursors are pre-oxidized in a pre-oxidation gas atmosphere higher than the oxygen volume concentration in the air to obtain "homogeneous pre-oxidized fibers" with substantially the same radial optical density. ", after low-temperature carbonization and high-temperature carbonization, large-diameter high-strength medium-mode carbon fibers are produced, with a diameter of 8.5-10 μm, a strength of 5.40-6.30 GPa, and a modulus of 280-330 GPa; Obtain large-diameter, high-strength, and high-modulus carbon fibers with a diameter of 7-10 μm, a strength of 3.90-5.70 GPa, and a modulus of 380-688 GPa. The large-diameter, high-strength, medium-mode or high-strength, high-modulus carbon fiber prepared by the present invention increases the diameter of the carbon fiber, effectively improves the alignment of the fiber, improves the resin wettability of the fiber in the preparation of the composite material, and finally improves the mechanical properties of the composite material .

Description

technical field [0001] The invention relates to a method for preparing large-diameter carbon fibers with high-strength medium-mode or high-strength and high-mode characteristics, and belongs to the field of fiber technology. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is one of the new high-strength materials with the largest amount, the fastest development, and the most widely used in recent years, and has the reputation of "the king of new materials". Due to its light weight, high strength, high modulus, electrical conductivity, thermal conductivity, high temperature resistance, corrosion resistance and a series of excellent properties, carbon fiber is widely used in aerospace, national defense and military industry, building reinforcement, petrochemical and leisure sports and other fields. [0003] Carbon fiber is divided into high-strength type, high-strength medium model, high-model, high-strength high-model, etc. according to its strength, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/22
CPCD01F9/225
Inventor 徐樑华王一苇王宇王云峰高爱君李常清童元建赵振文曹维宇
Owner BEIJING UNIV OF CHEM TECH
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