Synthesis And Recognition Of New Calixarenes Compounds, And Study Of Several Absorbent Resins

Six calix[4]recorcinarenes are synthesized by the reaction of resorcin as substrates with six aromatic aldehydes, respectively. These compounds are characterized by IR spectra and 1H NMR spectra. Calix[4]recorcinarenes synthesized with vanillin, isovanillin and 3,4,5-trimethoxy benzaldehyde are first prepared.Single-crystal of coordination compound 4-chlorobenzaldehyde calix[4]resorcinarene 37-DMF is obtained in solution of 4-chlorobenzaldehyde calix[4]resorcinarene in DMF. The crystal adopts the C2h symmetrical chair conformation. The force of intermolecular hydrogen bonds, including C—H…O and O—H…C, results in the formation of this conformation. The crystal has a sheet structure with three-dimensional network, and can be regarded as"quasi-complete solvation"of 37 by DMF in the crystalline state.A compound of calix[4]arene,α-phenylethylamine-amides on whose lower rim, are synthesized with two routes. One route is that the groups are connected to calix[4]arene step by step, and the products are purified with recrystallization. The other is that the groups are first synthesized, and then are connected to calix[4]arene by one step. The products are purified with zinc coordination compound as intermediate. Adopting the two routes, the yields are 45.6% and 23.5%, respectively.The p-tert-butylcalix[4]arenes respectively containing L-phenylane ethyl ester-based Schiff base, aldehyde groups and alkylbromides are synthesised. Hexaaquamanganese(Ⅱ) dipicrate dihydrate is prepared and characterized by single-crystal X-ray diffraction. The anion of picrate is orthorhombic, space group Pccn, and has no coordinative interaction with the manganese metal cation. The picrate anions are uncoordinated, and bound together by electrostatic attraction and hydrogen bonds.They areπ-stacked end to end. There are two lattice water molecules in one unit cell of the compound.Sodium tungstate was first employed as crosslinker in the preparation to achieve a better cross linked polymer WPAA. Sodium hydroxide and tris(2-hydroxyethyl)amine(TEA) are introduced in the preparation of WPAA-Na and WPAA-TEA hydrogels, respectively. The crosslinked polymers are characterized by IR spectra, thermogravimetetric analysis and scanning electron microscopy. The liquid absorbencies of WPAA-Na and WPAA-TEA are investigated. Results indicate that WPAA-Na and WPAA-TEA show better salt-resistances and water-absorbing rates. Results of a series of orthogonal design methods demonstrate that a crosslinked PAA superabsorbent composite with sodium tungstate, which is synthesized with a composition of 45.5 wt% of monomer, 0.4 wt% of crosslinker, 1.0 wt% of initiator, a neutralization degree of 83%, and a reaction temperature of 90℃, has a good water absorbency.Supermolecular compounds with several hydroxyl groups, containing calix[4]arenes and cyclodextrins, are first used to crosslinking copolymerize with acrylic monomers. Small molecules with hydroxyl groups, as of alcohol amines, inositols and capryl alcohols, etc. are introduced in the preparation of the crosslinking copolymers. The liquid absorbencies of these copolymers are investigated, and results show that water-absorbing rates and salt-resistances of copolymers with p-tert-butylcalixarenes are different. They show little absorption to DMF, and obvious absorption to mixture of DMF and a dram of water. Small molecules with hydroxyl groups make the liquid absorbencies of these copolymers correspond to those of some present super absorb resins. The rates of absorbing organic solvents by three poacrylic esters are substantially in accord with the order of polarity of these solvents.Three methods are used to prepare inclusion complexes between cyclodextrins and polystyrene. Only a solid product, which is considered with structure of cyclodextrins and polystyrene by IR spectra, is prepared with THF as solvent. It's specific structure needs further confirm.Silicon dioxide microspherical catalyst, which is prepared with polyethylene glycol 1000 as template, is charactered by IR spectra and SEM. Porous copper tungstate microspherical catalyst, which is prepared with polyacrylic acid as template, is charactered by TEM and XRD.