A low-viscosity high-heat-resistant polyimide fiber sizing agent and its preparation method
A technology of polyimide fiber and setting agent, which is applied in the direction of carbon fiber, fiber treatment, heating/cooling fabric, etc., can solve the problem of unclear specific composition of foaming powder, insufficient fluidity and heat resistance, and reduced material heat resistance. and other problems, to achieve the effect of improving operability and efficiency, low viscosity, and simple preparation method
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Embodiment 1
[0040]At room temperature, 23.11g (78.55mmol) of 2,3,3',4'-biphenyltetralic dianhydride and 53.37g (215mmol) of 4-phenylethynylphthalic anhydride were added to a 500mL single-necked bottle, and 85g of Methanol. The above mixed solution was heated to reflux, and after the solution was clarified, it was kept under reflux for 2.5h. Cool the solution to room temperature, add 12.07g (111.63mmol) of m-phenylenediamine and 14.90g (74.42mmol) of 3,4'-diaminodiphenyl ether, and add 18g of methanol to adjust the solid content of the solution to 50wt %. React at room temperature for 6 hours to obtain a fixative solution. The solution was distilled under reduced pressure at 40° C. to obtain a concentrated fixative solution. Molecular weight: 900 g / mol.
[0041] The concentrated fixative solution was placed in a vacuum oven at 80°C (pressure lower than -0.095MPa) for 6 hours, and solid fixative lumps were obtained after cooling down.
[0042] Crush the above-mentioned sizing agent blo...
Embodiment 2
[0044] At room temperature, add 12.03g (40.88mmol) of 2,3,3',4'-biphenyltetralic dianhydride and 124.12g (500mmol) of 4-phenylethynylphthalic anhydride in a 500mL one-necked bottle, and add 224g of ethanol. The above mixed solution was heated to reflux, and after the solution was clarified, it was kept under reflux for 3h. The solution was cooled to room temperature, and 46.58 g (145.44 mmol) of 2,2'-bistrifluoromethyl-4,4'-diaminobiphenyl and 42.5 g (145.44 mmol) of 1,3-bis(4-amino phenoxy)benzene, and add 51g of ethanol to adjust the solid content of the solution to 45wt%. React at room temperature for 8 hours to obtain a fixative solution. The solution was distilled under reduced pressure at 40° C. to obtain a concentrated fixative solution. Molecular weight: 859 g / mol.
[0045] The concentrated fixative solution was placed in a 90°C vacuum oven (pressure lower than -0.095MPa) for 4 hours, and a solid fixative block was obtained after cooling down.
[0046] The above-m...
Embodiment 3
[0048] At room temperature, 136.53 g (550 mmol) of 4-phenylethynylphthalic anhydride and 190 g of ethanol were added to a 500 mL single-necked bottle. The above mixed solution was heated to reflux, and after the solution was clarified, it was kept under reflux for 3h. The solution is down to room temperature, add 17.84g (165.00mmol) of m-phenylenediamine and 32.16g (110mmol) of 1,3-bis(4-aminophenoxy)benzene, and add 12g of methanol, the solution solid content Adjusted to 50wt%. React at room temperature for 6 hours to obtain a fixative solution. Molecular weight: 642 g / mol.
[0049] The solution was distilled under reduced pressure at 40° C. to obtain a concentrated fixative solution. The concentrated fixative solution was placed in a vacuum oven at 80°C (pressure lower than -0.095MPa) for 6 hours, and solid fixative lumps were obtained after cooling down.
[0050] Crush the above-mentioned sizing agent block to 200 mesh, sprinkle it evenly on the surface of the carbon fi...
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