Fluorine-containing diamine monomer and preparation method thereof
A technology of fluorine-containing diamine and diamine monomer, which is applied in the preparation of carboxylic acid nitrile, chemical instruments and methods, preparation of organic compounds, etc. The effect of good catalytic effect, low energy consumption and low temperature
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Embodiment 1
[0040] (1) Under nitrogen protection, add 4,4'-(perfluoropropane-2,2-diyl)bis(2-aminophenol) and 2 , 3,5,6-Tetrafluoro-p-halobenzonitrile, further adding an appropriate amount of organic solvent and alkali, stirring at room temperature for half an hour, then raising the temperature to 80°C for 10 hours, and then ending the reaction;
[0041] (2) White diamine monomer can be obtained after settling, filtering, drying and recrystallization;
[0042]In the above method, the organic solvent is selected from N,N-dimethylformamide, and the amount of the organic solvent is 4,4'-(perfluoropropane-2,2-diyl)bis(2-aminophenol) and 2 , 3 times the mass sum of 3,5,6-tetrafluoro-p-halobenzonitrile, the alkaline reagent is potassium carbonate, and the dosage is 4,4'-(perfluoropropane-2,2-diyl)bis(2 -3 times of the quality of aminophenol);
[0043] The diamine monomer prepared in this example (4,4'-((perfluoropropane-2,2-diyl)bis(2-amino-4,1-phenylene))bis(oxy)bis The structure of (2,3,5,6...
Embodiment 2-10
[0050] The specific method is consistent with Example 1, the difference is that the reaction temperature, reaction time and the molar ratio of the raw materials will be somewhat different, 4,4'-(perfluoropropane-2,2-diyl)bis(2-aminophenol) A represents that 2,3,5,6-tetrafluoro-p-halobenzonitrile is represented by B, and the specific setting parameters and the purity of the target product are shown in Table 2. The by-product content listed in the following table refers to the by-product A, by-product B and the content of all substances of the self-polymer of by-product B:
[0051] Note: by-product content and target product content detection means gas chromatograph, the amount of the measured substance (i) is proportional to its peak area on the chromatogram: m i =f i ×A i ,f i is a quantitative correction factor.
[0052] Table 2. Design Results
[0053]
[0054]
experiment example 1
[0060] The monomer 1 prepared in Comparative Example 1, the monomer 2 prepared in Comparative Example 2, and the monomer 3 prepared in Example 1 were all prepared into PI films.
[0061] By comparing the light transmittance of the PI film made of monomer 1, monomer 2 and monomer 3, it can be seen that the specific comparison results can be found in Figure 4 As shown, when the incident light wavelength is 300nm-400nm, the PI film prepared by monomer 1 has poor light transmittance and is basically opaque. When the incident light wavelength is above 700nm, the light transmittance is roughly between 85% and 90%. The PI film corresponding to monomer 2 has poor light transmission at about 300nm-380nm, and is basically opaque. When the incident wavelength reaches 500nm or more, its light transmission rate reaches about 90%. It can be seen from the comparison that the PI film made of monomer 3 has a relatively excellent light transmittance. At the lower absorption wavelength of 350...
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