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Preparation method of nascent fiber for production of carbon fiber

A technology of primary fiber and carbon fiber, which is applied in the direction of fiber chemical characteristics, conjugated artificial filament, conjugated synthetic polymer artificial filament, etc. It can solve the problems of hydroxyl crosslinking, limit the application of carbon fiber, and cannot be quickly stabilized

Inactive Publication Date: 2016-03-02
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyacrylonitrile-based carbon fibers have an absolute advantage in the production of high-performance carbon fibers, but the high price of petroleum-based raw materials and the corresponding process costs limit the application of carbon fibers
The problem of preparing carbon fiber from polyacrylonitrile precursor fiber is that the manufacturing cost of polyacrylonitrile precursor accounts for about 51% of the total cost of carbon fiber, and the time-consuming and long-term stabilization process requiring high temperature is the main energy-consuming process of carbon fiber production
There are two disadvantages in the existing melt spinning of lignin precursor fibers: one is that lignin is prone to hydroxyl crosslinking and self-thermal degradation at the melting temperature, resulting in a decrease in the quality of the precursor fibers and ultimately affecting the mechanical properties of carbon fibers
Another disadvantage is that the lignin fiber is difficult to stabilize and cannot be stabilized quickly, which leads to a great increase in the process cost of carbon fiber production. The heating rate of the lignin fiber stabilization method reported in the literature is basically controlled below 0.5°C / min. No fusion of fibers and no skin-core structure

Method used

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  • Preparation method of nascent fiber for production of carbon fiber
  • Preparation method of nascent fiber for production of carbon fiber
  • Preparation method of nascent fiber for production of carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) 0.8 L of acetic anhydride was added to 1 kg of kraft lignin (Sinopharm Group, Aldrich), the reaction temperature was 86° C., and the reaction time was 15 min to prepare acetylated kraft lignin for use.

[0035] (2) Dissolve 400g of acetylated kraft lignin in 1.6kg of dimethylformamide to make solution a, and dissolve 400g of polyacrylonitrile resin (Sinopharm Group, Aldrich) in 1.6kg of dimethylformamide under a nitrogen atmosphere. Solution b was prepared in formamide. Under a nitrogen atmosphere, solution a and solution b were mechanically stirred, the mass ratio of acetylated kraft lignin to polyacrylonitrile in the blend solution was 150:100, and the blend solution was kept at a constant temperature of 40°C to obtain a solid content of 20 wt% homogeneous spinning solution.

[0036] (3) Transfer the spinning solution to the spinning kettle and keep the spinning solution at a constant temperature of 40°C. Under the nitrogen pressure of 0.9MPa, the spinning solut...

Embodiment 2

[0038](1) Mix 1.2L of concentrated sulfuric acid (98%wt) and 2kg of distilled water to make a sulfuric acid solution, then add 1kg of alkali lignin (Sinopharm Group, TCI-L0082) into the sulfuric acid solution, keep the reaction temperature at 80°C, and the reaction time is 1.5 h. After the reaction, the reaction liquid is dried to prepare sulfoalkali lignin for future use.

[0039] (2) Dissolve 400g of sulfoalkali lignin in 1.6kg of dimethylacetamide to make solution a, and dissolve 600g of polyacrylonitrile resin (Sinopharm Group, Aldrich) in 1.4kg of dimethylacetamide under a nitrogen atmosphere. Solution b was prepared in amide. Under a nitrogen atmosphere, solution a and solution b were kneaded by a kneader, the mass ratio of sulfoalkali lignin to polyacrylonitrile in the blend solution was 53:100, and the blend solution was kept at a constant temperature of 50°C to obtain a solid content of 25 wt% homogeneous spinning solution.

[0040] (3) Transfer the spinning solutio...

Embodiment 3

[0042] (1) Add 100 g of concentrated ammonia water (28% wt) to 1 kg of kraft lignin (Sinopharm Group, Aldrich), stir mechanically for 1 hour, and store the ammoniated kraft lignin in a sealed container.

[0043] (2) Dissolve 440 g of ammoniated kraft lignin in 1.6 kg of dimethyl sulfoxide to make solution a, and dissolve 800 g of polyacrylonitrile resin (Sinopharm Group, Aldrich) in 1.2 kg of dimethyl sulfoxide under a nitrogen atmosphere. Prepare solution b in sulfoxide. Under a nitrogen atmosphere, solution a and solution b were extruded and mixed through a twin-screw machine, the mass ratio of ammoniated kraft lignin to polyacrylonitrile in the blended solution was 35:100, and the blended solution was kept at a constant temperature of 60°C. A homogeneous spinning solution with a solid content of 31% by weight was obtained.

[0044] (3) Transfer the spinning solution to the spinning kettle and keep the spinning solution at a constant temperature of 60°C. Under the nitrogen...

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Abstract

A preparation method of nascent fiber for production of carbon fiber comprises the following steps: uniformly mixing modified lignin or commercialized lignosulfonate and a solvent to prepare a solution a; uniformly mixing polyacrylonitrile resin and the solution to prepare a solution b, or directly using a de-monomerized polyacrylonitrile spinning solution as the solution b; blending the solution a and the solution b; keeping the blended solution at the constant temperature of 40-80 DEG C to obtain a uniform spinning solution with solid content being 12-33 wt%; pressing the spinning solution into coagulating bath through a spinneret plate to generate polyacrylonitrile / modified lignin nascent fiber; and finally winding at constant rate to obtain the nascent fiber for production of carbon fiber. The preparation method of the invention has advantages of low cost and high quality.

Description

technical field [0001] The invention belongs to a fiber forming technology, in particular to a method for preparing nascent fibers used for producing carbon fibers. Background technique [0002] Carbon fiber has excellent mechanical properties and is mainly used as a reinforcement of composite materials, widely used in various fields such as aerospace, national defense and military. Polyacrylonitrile-based carbon fibers have an absolute advantage in the production of high-performance carbon fibers, but the high price of petroleum-based raw materials and the corresponding process costs limit the application of carbon fibers. The problem of preparing carbon fiber from polyacrylonitrile precursor fiber is that the manufacturing cost of polyacrylonitrile precursor accounts for about 51% of the total cost of carbon fiber, and the time-consuming and high-temperature stabilization process is the main energy-consuming process of carbon fiber production. The future goal of carbon fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F8/08D01F8/18D01F9/14
CPCD01F8/08D01F8/18D01F9/14
Inventor 吕春祥董晓忠周普查
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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