Manufacturing method for polyacrylonitrile-based carbon fiber
A polyacrylonitrile-based carbon fiber and polyacrylonitrile resin technology, which is applied in the fields of fiber chemical characteristics, stretch spinning, textiles and papermaking, can solve the problems of raw silk purification and mechanical performance deterioration, and achieve good purification effect, The effect of improving mechanical properties
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Embodiment 1~12
[0041] Carry out the preparation of carbon fiber precursor according to the following steps:
[0042] 1) The polyacrylonitrile resin is prepared into a spinning solution with 45-58wt% NaSCN aqueous solution as a solvent, and the content of the polyacrylonitrile resin in the spinning solution is 10-14wt%. Using 8-16wt% NaSCN aqueous solution as a coagulation bath, adopting a wet spinning process to produce primary fibers through spinning and coagulation forming;
[0043] 2) The as-spun fiber is drawn in a water bath in 1 to 5 wt% NaSCN aqueous solution. The water bath temperature and the draw ratio of each embodiment are shown in Table 1, and this step is defined as pre-drawing in the table;
[0044] 3) The as-spun fibers are rinsed with deionized water, the water temperature is controlled at 45-60°C, and the rinse time is controlled at 2-20 minutes;
[0045] 4) The as-spun fiber is placed in the acidic aqueous solution for immersion, the control data of the acid and pH value,...
Embodiment 13~20、 comparative example 5~6
[0072] Part of the precursors obtained in the above-mentioned Examples 1-12 and Comparative Examples 1-4 were selected to further prepare carbon fibers. The selected precursors are listed in Table 6.
[0073] The raw silk is first pre-oxidized to obtain pre-oxidized silk. The pre-oxidation is carried out in air and is completed in three stages. The oxidation temperature of the first stage is 210-222°C, the oxidation time is 20-24min, and the draw ratio is 0-5; the oxidation temperature of the second stage is 235-245°C. The time is 20~24min, the draw ratio is -1~1; the third oxidation temperature is 255~265℃, the oxidation time is 20~24min, and the draft ratio is -1~1;
[0074] The pre-oxidized silk is further carbonized in nitrogen, and the carbonization is completed in two stages. The carbonization temperature of the first stage is 350-700°C, the carbonization time is 1-2min, and the draw ratio is 3-5 times; the carbonization temperature of the second stage is 800 ~1350℃, th...
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