Halogen ion functionalized organic porous material as well as preparation method and application thereof
A technology of porous materials and halogen ions, applied in separation methods, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of complex material synthesis process, high energy consumption of adsorption technology, poor recyclability, etc., and achieve good recyclability, synthesis The method is simple and the effect of strong thermal stability
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Embodiment 1
[0031] Embodiment 1, preparation of porous organic material:
[0032] S1. Add 0.1 mmol of 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde and 0.15 mmol of 5,5'-diamino-2,2'-bipyridine to o.d.×i.d. =9.5×7.5mm 2 glass tube
[0033] S2. Add dioxane, mesitylene and 6M acetic acid to the sample tube in turn, with a volume ratio of 5:5:1;
[0034] S3. Seal the heat-resistant glass tube in liquid nitrogen under reduced pressure, freeze it, and react it in an oven at 120° C. for 5 days to obtain an orange-red organic porous solid powder;
[0035] S4. Wash the organic porous material powder with anhydrous tetrahydrofuran by Soxhlet extraction for 2 days to remove the residual organic solvent, and dry it in a vacuum oven at 80°C-100°C for 10h-18h to obtain the organic porous material TpBpy with a yield of 70%. .
[0036] figure 1 It is the PXRD pattern corresponding to this embodiment. It can be seen from the figure that the main characteristic peaks observed at 2θ=3.6 are consistent...
Embodiment 2
[0039] Example 2, the preparation of ionic porous organic materials, prepared by the method of modification after ionization, the specific synthesis steps are divided into B-1 and B-2:
[0040] B1:
[0041] S1. Add 0.5 mmol of porous material, 5 mmol of 1,2-dibromo-1,1,2,2-tetrafluoroethane and 70 mL of acetonitrile into a 150 mL high-temperature pressure-resistant bottle, react at 90°C for 24 hours, and then replenish Add 5 mmol of 1,2-dibromo-1,1,2,2-tetrafluoroethane, and continue the reaction at 90°C for 24 hours;
[0042] S2. After cooling to room temperature, filter with suction, then wash the filter cake with a small amount of ethanol several times to remove unreacted 1,2-dibromo-1,1,2,2-tetrafluoroethane, vacuum at 80°C-100°C Dry in a drying oven for 10h-24h to obtain a bromide ion-type porous material.
[0043] B2:
[0044] S1. Add 0.5 mmol of bromide ion-type porous material to saturated potassium iodide solution, stir vigorously at room temperature for 3 hours, f...
Embodiment 3
[0050] Example 3, preparation of halide ion functionalized organic porous material for iodine adsorption:
[0051] S1. Put the organic porous material powder sample functionalized with halogen ions into a thermogravimetric machine, and record the weight after activation at 150°C for 4 hours;
[0052] S2, then feed iodine vapor containing nitrogen at a concentration of 150ppmv at 150°C;
[0053] S3. Record the weight of the sample during the adsorption process, and use the gravimetric method to study the adsorption performance of the sample to iodine vapor.
[0054] Figure 8 It is the iodine vapor adsorption curve graph of this example that changes with time. It can be seen from the figure that the organic porous material functionalized with halide ions has an adsorption capacity of 36.5 wt% for iodine at 150° C. and an iodine vapor concentration of 150 ppmv;
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