Sample Name: Poly(4-amino methyl styrene-b-Styrene) Sample #: P11422A-4AMSS Structure: H C H3C C H2 CH2 CH b CH2 n THF THF/Methanol 90:10 CHCl3 DMF Opaque solution Insoluble opaque Soluble in Hot DMFCH3OH 95:5 soluble CH HNMR of the Monomer 1,1,1,3,3,3-Hexamethyl-2-(4-vinylbenzyl)-disilazane: H m CH3 NH2 Composition: Mn x 103 4AMS-b-S Mw/Mn (PDI) 1.5-b-1.5 1.3 Synthesis Procedure: By anionic process: CH CH2 CH b CH2 n CH CH2 H3C CH2 CH HNMR of the Polymer: n R-Li/LiCl THF -78C CH H2C Li Si H3C n H3C N HCl Si H3C CH3 NH4OH/KOH CH3 CH2 CH b CH2 n CH n CH2 H3C N Si H3C Si H3C H3C CH3 H2C H3C C H2 H C NH2 CH3 H2C SceBuLi H C H2C HCl CH NH4OH/KOH Li CH3 CH2 H3C Si H3C N Si H3C H3C CH3 CH3 H3C H C C H2 soluble Partial Solubility: The solution light blue coloration illustrates formation of micelles. H2C H2C DMF:THF 50:50 CH2 CH b CH2 CH n H m CH3 H2C NH2 Characterization: Polymer analyzed by size exclusion chromatography (SEC) to obtain the molecular weight and polydispersity index (PDI). The final block copolymer composition was calculated from 1H-NMR spectroscopy by comparing the peak area of the styrene protons at 6.3-7.2 ppm with the peak area at 3.76. HNMR analysis was carried out in CdCl3 for the amino protected group with trimethyl silyl groups. Block copolymer PDI is determined by SEC. Solubility of the polymer Poly(styrene-b- 4-(N,N-bis (trimethylsilyl) aminomethyl )styrene) polymer (protected Amino compound) is soluble in THF, CHCl3, Toluene. Once the trimetyl silyl group removed the amino methyl styrene (salt with HCl) block polymer was found insoluble in most of the solvents. It was brought back to free amino group by treatment with NH4OH solution in THF/water mixture. The solubility of such type of polymer in different solvent is based on its composition: The following table illustrate the solubility in the following solvents: Figure: SEC profile of the block copolymer P11422-4AMS (NH2 protected) -S 0.0 8 10 12 14 16 18 20 22 24 26 28 30 32 Ve (ml) Size Exclusion Chromatogram of Poly(4-aminomethylstyrene protected -b-styrene) 4-Amino methylstyrene-Protected: Mn=3,200, Mw=3700, Mw/Mn=1.13 4AMS-S: Mn P4AMS(3200)-PS(1500), Mw/Mn=1.3 After deprotection: 1500-b-1500
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