Synthesis And Characterization Of Novel Macroporous Alkyl-imide Resin

In the present work,styrene-divinylbenzene microspheres were successfully prepared using styrene as monomer,divinylbenzene as crosslinking agent,liquid paraffin as porogen and styrene peroxide as an initiator by the suspension polymerization.Meanwhile,the porogen was extracted by petroleum ether from the styrene-divinylbenzene microspheres.Moreover,five novel macroporous alkyl imide resin were synthesized using five kind of alkyl imides and chloromethylated styrene-divinylbenzene beads as precursor which were chloromethylated from the styrene-divinylbenzene microspheres.The finished work and achieved results in this paper are summarized as follows:?1?The styrene-divinylbenzene microspheres were prepared using styrene as monomer and divinylbenzene as crosslinking agent by suspension polymerization.The results showed that the surface morphology of microspheres changed greatly before and after the extraction of the porogen.Before extracting the porogen,they are smooth without any holes,while the holes are occurred in the surface of microspheres after the extraction of the porogen.The apparent density and the degree of swelling are 0.9389 g/cm³ and 2.089,respectively.The content of C,H,N is 92.28%,7.66%and<0.5%,respectively.The styrene-divinylbenzene microspheres have good thermal stability and their thermal decomposition started in 221?and decompose completely in 566?.The type of hole is large hole,its BET specific surface area is 33.18m²/g,the single-point adsorption pore volume is 0.2812 cm³/g at P/P₀=0.99,the pore size is distributed from 1.7 nm to 56 nm,and the average pore diameter of the adsorption is 31.03 nm.?2?Chloromethylated styrene-divinyl benzene microspheres were synthesized using chloromethyl ether as the chloromethylation agent and anhydrous zinc chloride as catalyst.Chlorine content of chloromethylated styrene-divinylbenzene microspheres is 4.462 mmol/g,the apparent density and degree of swelling is 1.045 g/cm³ and 1.707,respectively.The surface of microspheres changed significantly after the chloromethyl.The initial temperature of the thermal decomposition is 249?and the terminal temperature of the thermal decomposition is 564?.The hole type is macroporous,its BET specific surface area is 26.42m²/g,the single point adsorption pore volume is 0.2330 cm³/g at P/P₀=0.99,the pore size distribution is from 1.7 nm to 56 nm and average pore diameter of the adsorption is 35.27nm.?3?Five kind of macroporous alkyl imide resin such as di-n-propyl-imide resin,di-n-butyl-imide resin,di-n-pentyl-imide resin,di-n-hexyl-imide resin,di-n-heptyl-imide resin were synthesized using chloromethylated styrene-divinylbenzene microspheres as precursor.The contents of their functional groups are 2.456,2.209,2.484,2.195,2.284 mmol/g,respectively.Their apparent density are 0.8532,0.8168,0.8559,0.8728,0.9412 g/cm³,respectively.The degree of swelling are 1.792,1.710,1.646,1.556,1.457,respectively.The surface of the resin is more rough.The thermal decomposition starts at²30?,thermal decomposition termination temperature is⁵30?,but the thermal decomposition temperature of N-butyl terminated imide resin is 560?.The average pore size of five kind of resins is>40 nm,and N-dipropyl-imide resin has the smallest diameter of 40.00nm,n-heptyl-imide resin has maximum diamater of 47.98 nm.