Method for preparing fluorine content- and dimension-adjustable carbon fluoride fibers

A technology of carbon fluoride and carbon fluoride adjustment, which is applied in the fields of carbon fiber, fiber treatment, textiles and papermaking, etc. It can solve the problems of high equipment requirements, long processing time, harsh reaction conditions, etc., and achieve simple reaction devices and short reaction time , cheap effect

Active Publication Date: 2017-04-26
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional carbon fiber surface treatment methods (including surface oxidation, coating, deposition) usually require strong acid / alkali, high treatment temperature, complicated steps, long reaction time, high cost and high requirements for equipment and processes (see : N. Gupta, V. I. Artyukhov, E. S. Penev, et al ., Adv. Mater., 2016, DOI:10.1002 / adma.201603009; Y. Y. Wang, J. Y. Meng, X. B. Chen, et al ., Surf.Tech. , 2007, 3, 19.)
In addition, due to the chemical structure and properties of the fluorinated carbon fiber itself, it is difficult to achieve the surface modification of the fluorinated carbon fiber by the above-mentioned treatment method, let alone the regulation of its size.
Specifically, it is mainly due to the following aspects: (1) The chemical inertness of the C-F bond in the fluorinated carbon fiber makes it exhibit chemical stability similar to Teflon, which makes it difficult to realize the chemical method of strong acid and strong base oxidation Its oxidation; (2) fluorinated carbon fiber is an insulator, and it is difficult to complete its modification by electrochemical anodic electrolytic oxidation method; (3) fluorine atom is the most electronegative element among all known elements, with extremely low surface energy, This makes it difficult to modify other surface treatment agents to the surface by surface coating, deposition and plasma treatment.
[0004] At present, fluorinated carbon fibers with different sizes and different element contents have problems such as high equipment requirements, harsh reaction conditions, long processing time and complicated process in the process of preparation and surface treatment. The existence of these difficulties greatly limits the development of fluorinated carbon fibers. practical application
At present, there are no reports on the surface treatment, fluorine content and size control of fluorinated carbon fibers.

Method used

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  • Method for preparing fluorine content- and dimension-adjustable carbon fluoride fibers
  • Method for preparing fluorine content- and dimension-adjustable carbon fluoride fibers
  • Method for preparing fluorine content- and dimension-adjustable carbon fluoride fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 0.1g fluorinated carbon fiber (the size of the raw material is 4000-5000μm, the fluorine content is 47at.%), 30mL ethylenediamine, and stir the reaction at 120°C for 3 hours under the protection of nitrogen. After cooling, use a 0.45 μm organic membrane to suction filter, wash, collect and dry the filter cake to obtain fluorinated carbon fibers with a size of 50-100 μm, a fluorine content of 34.3 at.%, a nitrogen content of 4.2 at.%, and significantly improved dispersion stability. The yield (yield=product mass / raw material mass) was 75%. After collecting the filtrate and removing the solvent with a rotary evaporator, fluorinated carbon fibers with an element content close to that of the filter cake and a size of less than 0.45 μm were obtained, with a yield of 15%.

Embodiment 2

[0028] Add 0.1g fluorinated carbon fiber (raw material size 4000-5000μm, fluorine content 47at.%), 30mL ethylenediamine into a round bottom flask, and stir at 100°C for 5 hours under nitrogen protection. After cooling, use a 0.45 μm organic membrane to suction filter and wash, collect the filter cake and dry it to obtain a fluorinated carbon fiber similar to Example 1, with a yield of 77%. Collect the sample in the filtrate to obtain an element content close to that of the filter cake, and the size is less than 0.45 μm fluorinated carbon fibers with a yield of 17%.

Embodiment 3

[0030] Add 0.1g fluorinated carbon fiber (raw material size 3500-4500μm, fluorine content 57at.%), 10mL ethylenediamine into a round bottom flask, and stir at 60°C for 8 hours under the protection of argon. After cooling, use a 0.45 μm organic membrane to filter and wash, collect the filter cake and dry it to obtain a fluorinated carbon fiber with a fluorine content and size close to that of the raw material and with improved dispersion. The yield is 71%. The cake was close, with a yield of 13% for fluorinated carbon fibers with a size below 0.45 μm.

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Abstract

The invention discloses a method for preparing fluorine content- and dimension-adjustable carbon fluoride fibers. The method comprises the following steps: 1, carrying out carbon fluoride fiber surface treatment: adding a raw material carbon fluoride fibers to a surface treatment reagent, and heating the carbon fluoride fiber and the surface treatment reagent under the protection of a gas to 60-150 DEG C for a reaction in order to obtain pretreated carbon fluoride fibers; and 2, separating carbon fluoride fibers with different dimensions: cooling the pretreated carbon fluoride fibers obtained in step 1, carrying out suction filtration through a filter membrane, separating and washing the filtered pretreated carbon fluoride fibers, and drying the washed carbon fluoride fibers to obtain the finished carbon fluoride fibers. The carbon fluoride fibers prepared through the method have the advantages of controllable fluorine content, controllable dimension, and improved dispersion and stability in water and organic solvents.

Description

technical field [0001] The invention relates to a size control and surface treatment technology of fluorinated carbon fiber, in particular to a method for preparing fluorinated carbon fiber with adjustable fluorine content and size. Background technique [0002] Carbon fiber has a series of excellent properties such as high specific strength / specific modulus, creep resistance, electrical conductivity, heat transfer and small thermal expansion coefficient, and it is also resistant to high temperature, corrosion and fatigue. Therefore, it can be used not only as a structural material, but also as a functional material, and is widely used in high-tech fields such as aerospace and aviation. Fluorinated carbon fiber not only inherits the excellent properties of carbon fiber, but also brings novel interface and physical and chemical properties such as reduced surface energy, enhanced hydrophobicity / thermal stability, widened band gap and improved dielectric properties due to the i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/332D06M101/40
CPCD06M13/332D06M2101/40
Inventor 公培伟孙璐逄铭慧张雨荷刘哲
Owner QUFU NORMAL UNIV
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