Process method for preparing intermediate phase lignin and carbon fibers thereof

A process method and lignin technology, which are applied in the field of high-performance mesophase lignin and carbon fiber production and manufacturing processes, can solve the problems of inability to form a graphite sheet structure, limited use, no fluidity and spinnability, etc. The effect of high value utilization and low modulation cost

Active Publication Date: 2013-12-18
吴佟生
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The alkali lignin and sulfonate lignin produced by traditional pulping and papermaking contain high content of inorganic substances, including impurities such as sodium, sulfur, calcium, magnesium, etc., which make the lignin carbon fiber performance poor, while ethanol lignin, acetic acid The performance of the carbon fiber produced by purifying and purifying lignin such as lignin and phenolic lignin can only reach the level of general-purpose. Its tensile strength is 300-900MPa, and its tensile modulus is about 40GPa. It cann

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0034] Example 1:

[0035] Select ethanol lignin, the weight average molecular weight is between 2000 and 10000, the dispersion coefficient is 1.8, and the ash content is ≤0.025%. Take 500g of lignin and add it to the reaction kettle, add 1000g of anthracene oil, pass nitrogen, blow out the air in the kettle, and then pass The salt bath is heated to the reaction kettle to 380 ℃, and the pressure is kept not more than 3.5MPa for 5 hours. After cooling, it is taken out and added to the salt bath glass reaction kettle. After the anthracene oil and the light components were kept for 7 hours, the mesophase lignin was obtained after cooling. Observed under a polarizing microscope, the content of the mesophase reached 75% by mass, and the measured softening point was 272 ° C. The spinning was carried out in a single-hole melt spinning machine, the diameter of the spinneret was 0.3 mm, and the spinning temperature was 305 ° C. After the original fiber was placed in a pre-oxidation fu...

Example Embodiment

[0036] Embodiment 2:

[0037]Select ethanol lignin, the weight average molecular weight is 2000-10000, the dispersion coefficient is 1.8, and the ash content is ≤ 0.025%. Take 500g of lignin and add it to the reaction kettle, add 500g of naphthol, pass nitrogen, blow out the air in the kettle, and then pass The salt bath was heated to the reaction kettle to 400 ℃, and the pressure was kept not more than 3.5MPa for 4 hours. After cooling, it was taken out and added to the salt bath glass reaction kettle. After 3 hours, the mesophase lignin was obtained after cooling. Observed under a polarizing microscope, the content of the mesophase reaches 90% by mass, and the measured softening point is 282 ° C. The spinning is carried out in a single-hole melt spinning machine, the diameter of the spinneret is 0.3 mm, and the spinning temperature is 312 ° C. After the original fiber was placed in a pre-oxidation furnace, the temperature was programmed, the maximum temperature was 310 ° C,...

Example Embodiment

[0038] Embodiment three:

[0039] Select ammonia lignin, the weight average molecular weight is 2000-5000, the dispersion coefficient is 1.4, and the ash content is less than or equal to 0.01%. Take 500g of lignin, add it to the reaction kettle, and add 150g of fluoranthene, pass nitrogen, blow out the air in the kettle, and then pass The salt bath is heated to the reaction kettle to 420 ° C, the pressure is kept not more than 3 MPa, and the time is 10 hours. After cooling, it is taken out, added to the salt bath glass reaction kettle, introduced with nitrogen, heated with stirring at 420 ° C, and evaporated after light components. , kept for 5 hours, and the mesophase lignin was obtained after cooling. Observed under a polarizing microscope, the content of the mesophase reached 100% by mass, the softening point was measured to be 265°C, and the spinning was performed in a single-hole melt spinning machine, the diameter of the spinneret was 0.3mm, and the spinning temperature ...

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Abstract

The invention relates to a process method for preparing intermediate phase lignin and carbon fibers thereof. The process method is characterized in that a condensing agent is added for carrying out heat treatment reaction modification and further condensation polymerization on various lignin to obtain a polycyclic aromatic hydrocarbon substance with an intermediate phase, the polycyclic aromatic hydrocarbon substance is prepared into the intermediate phase lignin, and the intermediate phase lignin can be used for preparing various carbon materials. The high-intensity and high-modulus lignin carbon fibers can be prepared by melt spinning, pre-oxidation and carbonization of the intermediate phase lignin prepared by the method, and is comparable with high-performance pitch-based carbon fibers and high-modulus polyacrylonitrile-based carbon fibers.

Description

technical field [0001] The invention relates to a production method of lignin carbon fiber, which is a production process of high-performance mesophase lignin and carbon fiber. Background technique [0002] Carbon fiber is a fibrous material with a carbon content of more than 90% by mass. It has various types. Its high strength and high modulus can be used to make various composite materials, which can be used as structural materials and have a wide range of uses. There are many ways to produce carbon fiber. At present, polyacrylonitrile-based carbon fiber accounts for more than 75% of the total, followed by pitch-based carbon fiber, while the global production of viscose-based carbon fiber only accounts for about 1%. [0003] Mesophase aromatics prepared from asphalt, naphthalene and other raw materials have the characteristics of high modulus, high thermal conductivity, and high electrical conductivity. They have a wide range of uses and can be used to produce high-perform...

Claims

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Application Information

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IPC IPC(8): D01F9/17C08H7/00
CPCY02P20/54
Inventor 张子宇
Owner 吴佟生
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