Mesoporous polydivinylbenzene material with hypersorption characteristic and synthesis method thereof

[0025] Example 1: Mesoporous polydivinylbenzene PDVB-THF-0 synthesized in a tetrahydrofuran system.

[0026] Dissolve 2g of divinylbenzene (DVB) monomer and 0.05g of azobisisobutyronitrile (AIBN) in 20mL of tetrahydrofuran. After stirring for 4 hours, transfer the above solution to the reactor and place it in an oven at 100℃. hour. The reaction kettle was taken out to volatilize the tetrahydrofuran to obtain mesoporous polydivinylbenzene PDVB-THF-0.

[0027] The results of the nitrogen adsorption experiment are shown in Figure 1. The type IV adsorption isotherm given by the sample PDVB-THF-0 indicates that the sample has a mesoporous structure and has a relatively narrow pore distribution (~3.9nm). Figure 2 is a transmission electron microscope (TEM) photo of the sample PDVB-THF-0. The result further confirms the result of nitrogen adsorption. From Figure 2 we can clearly see the existence of abundant mesopores. The BET specific surface area of ​​the sample PDVB-THF-0 is 557m 2 /g.

[0028] Figure 7 shows the adsorption capacity of sample PDVB-THF-0 to benzene vapor. The adsorption capacity for 1 hour is 880 mg/g, and the adsorption capacity reaches 1400 mg/g after adsorption time to 5 hours, which is about 5.6 times the adsorption capacity of activated carbon.

[0029] Changing the temperature of polymerization and the time of putting it in the oven, the same results can be obtained at 80-180 degrees for 12-48 hours. The polymerization time is too short (for example, less than 12 hours) or the temperature is too low (for example, lower than 80 degrees) resulting in a lower specific surface area or even a non-porous structure.

[0030] Example 2: Synthesis of mesoporous polydivinylbenzene PDVB-THF-x in a composite system of tetrahydrofuran and water.

[0031] Dissolve 2g of divinylbenzene (DVB) monomer and 0.05g of azobisisobutyronitrile (AIBN) in 20mL of tetrahydrofuran, then add xmL of water, where x=1.0, 1.2, 1.4, 1.6, 1.8, 2.0, and stir After 4 hours, the above solution was transferred to the reaction kettle and placed at 100°C for 48 hours. The reaction kettle was taken out to volatilize the tetrahydrofuran to obtain mesoporous polydivinylbenzene PDVB-THF-x.

[0032] In this embodiment, the amount of water is not limited to 1 to 2 mL, and the adjustment range can be 0 to 10 mL, and 1 to 2 mL is selected only for the convenience of discussion. When it is less than 1 mL, the adjustment effect of the pore size is not obvious. When it is greater than 2mL, a further increase in pore size can be achieved. The PDVB-THF-10 sample also has a higher specific surface area of ​​650m 2 /g. But the hole distribution is relatively broad. It contains some macropores (~50nm).

[0033] The nitrogen adsorption isotherm in Fig. 3 shows that the sample PDVB-THF-x (x=1~2) all give IV type adsorption isotherms, indicating that it has a mesoporous structure, which can be determined by the position of the isotherm hysteresis loop It can be seen that when the amount of water added increases, the pore size also gradually increases. The pore distribution results further confirmed this point. By introducing a certain amount of water as a co-template, the size of the mesoporous pore size of the sample can be adjusted by the amount of water. The adjustment range is roughly x=1~2, and the pore size is 4~ 22nm. The BET specific surface area of ​​sample PDVB-THF-2 is 702m 2 /g. The results of transmission electron microscopy (TEM) further confirmed the results of nitrogen adsorption (see Figure 4). From Figure 4, it can be clearly seen that the sample PDVB-THF-2 has larger mesopores (~20nm).

[0034]It can be clearly seen from a in Figure 5 that the sample PDVB-THF-2 has a bulky morphology and a controllable shape. In Figure 5, b is the contact angle of water droplets on the sample PDVB-THF-2, the angle is 156 degrees, indicating that the sample has superhydrophobicity. In Figure 5, c is the contact angle of salad oil droplets on PDVB-THF-2, and the angle is zero, indicating the super lipophilicity of the sample. Figure 6 shows the thermal weight loss curve of the sample PDVB-THF-2, and the decomposition temperature of the sample is between 230 and 500 degrees. Figure 7 shows the sample's adsorption capacity for gaseous organics (benzene vapor) over time, and Figure 8 shows the sample's adsorption capacity for various liquid organics. In the adsorption of gaseous and liquid organics, the sample PDVB-THF-2 shows an ultra-high adsorption capacity, which is far superior to the traditional adsorbent activated carbon, and is 7.6 to 19 times the adsorption capacity of activated carbon. Tests show that per gram of sample PDVB-THF-2 can adsorb 1.95 grams of gaseous benzene, 1.97 grams of acetone, and 1.90 grams of n-heptane. Moreover, the adsorbed sample can be desorbed by simple vacuum distillation to remove the adsorbed substance. After the sample is desorbed, there is no significant change in the BET specific surface area, pore size, pore volume, etc., thereby realizing the mesoporous polydivinylbenzene of the present invention. Reuse.

[0035] Example 3: Synthesis of mesoporous polydivinylbenzene PDVB-acetone in an acetone system.

[0036] 20 mL of acetone was used instead of tetrahydrofuran in Example 1, and the remaining steps were the same as in Example 1. Referring to Figure 9, the nitrogen adsorption isotherm indicates that the sample has the characteristics of a composite pore structure of micropores and mesopores. From the results of BJH pore distribution and DFT pore distribution, it can be seen that the sample has both ~3.9nm mesopores and ~1.1nm pores. Micropores. BET specific surface area can reach 416m 2 /g, of which the micropores are 173m 2 /g, mesopore 242m 2 /g.