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Chinese Journal of Materials Research  2017, Vol. 31 Issue (2): 96-101    DOI: 10.11901/1005.3093.2016.260
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Influence of Acid Treatment on Properties of Dry-spinning Jialun Polyimide Fibers Reinforcement
Le CHEN1,2,Zhu LONG1(),Shihua WANG3,Zhiqiang LI3,Shuai GUO3,Bin WANG2
1 Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi 214122, China
2 State Key Laboratory of Pulp and Paper Engineering, South China University of Technology, Guangzhou 510640, China
3 Lianyungang Industry Investment Group Co., Ltd, Lianyungang 222002, China
Cite this article: 

Le CHEN,Zhu LONG,Shihua WANG,Zhiqiang LI,Shuai GUO,Bin WANG. Influence of Acid Treatment on Properties of Dry-spinning Jialun Polyimide Fibers Reinforcement. Chinese Journal of Materials Research, 2017, 31(2): 96-101.

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Abstract  

The effect of chemical treatment with HCl solution on the wetting properties, surface morphology, thermal properties, fineness and mechanical properties, chemical structure and microscopic state of aggregation structure was investigated for polyimide fiber-reinforcements The results show that after HCl treatment, the fiber surface exhibits characters of etching with increased surface roughness, higher surface free energy, and enhanced wetability, while certain reactive group is introduced onto the surface; With the increase of HCl concentration, the rise of temperature as well as the the increase of processing time, the wetability was sharply enhanced, the fineness and mechanical properties decrease slightly while the thermal property keeps preferably within a certain range. The existence of H+ in the treatment solution could result in that a few of imide rings on the fiber was broken and then hydrolyzed to polyamide acid, thereby its microscopic state of aggregation structure was changed and the ratio of amorphous region was enhanced, therewith its chemical structure does not change significantly. In general, HCl treatment is feasible for modifying the polyimide fiber surface.

Key words:  composites      acid treatment      polyimide fibers      wetting properties      properties and structure     
Received:  16 May 2016     
Fund: Supported by National Natural Science Foundation of China (No.31270633), State Key Laboratory of Pulp and Paper Engineering (No.201512), Lianyungang “555 Talents Project” Program (No.2015-13), Hangzhou Qianjiang Distinguished Experts Programme of China and A Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions

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https://www.cjmr.org/EN/10.11901/1005.3093.2016.260     OR     https://www.cjmr.org/EN/Y2017/V31/I2/96

Fig.1  SEM images under different HCl treating conditions (a) untreated; (b) 7.2% HCl 90℃ 3 h; (c) 10.8% HCl 90℃ 3 h
Temperature/℃ Time/h 7.2% 10.8%
Height/cm Height/cm
30 1 6.6 6.8
2 7.1 7.3
3 7.3 7.5
60 1 7.0 7.2
2 7.4 7.7
3 7.6 7.8
90 1 7.2 7.4
2 7.5 7.6
3 7.8 8.0
Table 1  Fiber wetting properties test results by HCl treatment
Fig.2  TG (a) and DTG (b) curves of polyimide fibers by HCl, 90℃, 3 h treatment
Temperature/℃ Time/h 7.2% 10.8%
Fineness/μm Strength/cN/dtex Elongation/% Fineness/μm Strength/cN/dtex Elongation/%
30 1 21.02 4.14 14.11 20.12 4.12 14.20
2 19.69 4.08 13.83 19.28 4.05 13.65
3 18.38 4.00 13.20 18.36 3.97 13.16
60 1 18.38 4.01 13.43 18.87 3.96 13.23
2 18.36 3.93 13.24 18.68 3.88 12.98
3 18.22 3.85 12.78 18.68 3.81 12.65
90 1 17.69 3.99 13.38 19.72 3.91 13.07
2 17.81 3.91 12.86 19.45 3.80 12.63
3 18.03 3.81 12.82 17.26 3.75 12.53
Table 2  Fiber fineness and mechanical properties test results by HCl treatment
Temperature/℃ Time/h 7.2% 10.8%
Strength loss/% Elongation loss/% Strength loss/% Elongation loss/%
30 1 10.58 8.91 11.02 8.33
2 11.88 10.72 12.53 11.88
3 13.61 14.78 14.25 15.04
60 1 13.39 13.30 14.47 14.59
2 15.12 14.53 16.20 16.20
3 16.85 17.50 17.71 18.33
90 1 13.82 13.62 15.55 15.62
2 15.55 16.98 17.93 18.46
3 17.71 17.24 19.01 19.11
Table 3  Change of the fiber mechanical properties by HCl treatment
Fig.3  FT-IR pattern of polyimide fibers by HCl treatment
Fig.4  Hydrolysis process of polyimide fibers in acidic and alkaline condition
Fig.5  XRD pattern of fibers by HCl treatment
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