A kind of porous organic polymer and its preparation method and application
A polymer, polymerization reaction technology, applied in separation methods, methods of chemically changing substances by atmospheric pressure, alkali metal compounds, etc., can solve problems such as inability to mass-produce operating conditions, shortening reaction time, and low reaction activity, etc. To achieve the effect of easy expansion of reaction scale, increase of reaction rate, and short synthesis cycle
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Embodiment 1
[0028] Pore regulation of B-H coupling polymer PTPA by different reaction temperatures: 1 mmol tris(4-bromophenyl)amine (centron), 1 mmol p-phenylenediamine (linker), 5mol% Pd(dba) 2, 9 mol% xPhos and 7 eq. NaOtBu were added to the micro-autoclave, 70 ml tetrahydrofuran was injected, and the reaction pressure was 2 MPa at 100 °C, 120 °C, 140 °C, and 160 °C, respectively, and the reaction was carried out for 5 hours. The product was successively washed with suction filtration of tetrahydrofuran, chloroform, ethanol and hot water, and the solid product PTPA was vacuum dried at 70° C. for 24 hours to remove the solvent. The product is bright blue, shows obvious redox state polyaniline characteristics, and is insoluble in various organic solvents and acid-base solvents, and the experiment has good reproducibility. The product yield was calculated after drying, and the average yield was more than 95%, and there were abundant micropores with a specific surface area of up to 1145...
Embodiment 2
[0032] Pore regulation of B-H coupled polymer PTPA with different reaction times: 1 mmol tris(4-bromophenyl)amine (centron), 1 mmol p-phenylenediamine (linker), 5mol% Pd(dba) 2 , 9 mol% xPhos and 7 eq. NaOtBu were added into the micro-autoclave, and 70 ml of tetrahydrofuran were injected. Suction filtration and washing of chloroform, ethanol, and hot water, and the solid product PTPA was vacuum-dried at 70° C. for 24 hours to remove the solvent. Experiments have found that even if the reaction time is shortened to 1 hour, a product with good shape can be obtained under the condition of increasing the temperature, which realizes a rapid reaction, and solves the problem that the reaction time is often limited to 2-3 days due to the low reaction activity. , and even weeks of problems.
[0033] image 3 Infrared spectra of linkers and infrared spectra of PTPA obtained by B-H coupling reaction at different reaction times. It can be found that the infrared characteristic peaks ...
Embodiment 3
[0036] Pore regulation of B-H coupled polymer PTPA by different reaction pressures: 1 mmol tris(4-bromophenyl)amine (centron), 1 mmol p-phenylenediamine (linker), 5mol% Pd(dba) 2 , 9 mol% xPhos and 7 eq. NaOtBu were added into the micro-autoclave, 70 ml of tetrahydrofuran was injected, and the reaction was carried out at 120 °C for 5 hours, and the reaction pressure was set to 0 MPa, 1 MPa, and 2 MPa, respectively. The solid product PTPA was vacuum-dried at 70° C. for 24 hours to remove the solvent after successively washing with suction filtration of tetrahydrofuran, chloroform, ethanol and hot water.
[0037] Figure 5 Infrared spectra of linkers and infrared spectra of PTPA obtained by B-H coupling reaction at different reaction times. It can be found that the infrared characteristic peaks of all samples are basically the same as those of Example 1, and the corresponding amino characteristic peaks and the weakening of the C-Br peak appear, indicating the successful synth...
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