| Coal,oil and natural gas are the main source of modern synthetic polymer materials. With the depletion of fossil resources, as well as the emphasis of environmental protection, people are forced to turn to the use of natural raw materials instead of the fossil materials. As a natural source of biomass, sucrose is derived from plants. The macromolecular derivatives of sucrose have wide applications prospect in food, daily chemical industry, agriculture, medicine and other industry, it has a great market potential for development of fine chemical products. Carrying out the synthesis and research of sucrose and its macromolecular derivatives has important theory and application value.In this article, methacrylic acid acyl chloride(MAC) was synthesized through the acylation reaction of methyl acrylic acid(MAA) and thionylchloride, and then the methacrylic acid sucrose ester(MASE) was synthesized with MAC and sucrose. Basing on the synthesis of MASE and MAA, the copolymers of MASE and MAA was obtained. The new sucrose-based polycarboxylate superplasticizer was synthesized by MASE, methacrylic acid, sodium allyl sulfonate and allyl polyethylene glycol. The products synthesized were characterized and analyzed by fourier transform infrared spectroscopy(FT-IR), nuclear magnetic resonance spectrometer(NMR), gas chromatography- mass spectrometry(GC-MS), X ray diffraction(XRD) and other analytical instruments. The main research work contents include the following aspects:1) Study on synthesis of MASE: The MASE was obtaind by MAC and sucrose through nucleophilic substitution reaction. The MASE was characterized by FT-IR and 1H NMR, and the reaction activity of the sucrose primary hydroxyl was analysed by GC-MS. The results showed that one primary hydroxyl was participated in the reaction first, and the other two primary hydroxyls in the reaction late. By changing the reaction time, reaction temperature and monomer molar weight ratio, the optimum synthesis conditions for MASE was obtained.2) Study on copolymerization of MASE and MAA: The co-polymers of MASE and MAA were obtained from MAA and MASE by free radical reaction by FT-IR and 13 C NMR. The intrinsic viscosity of the copolymers in different reaction conditions was measured by the viscosity method. The contact angle of the copolymer solution in different concentration was measured on the surface of PMMA, PTFE and PE. We also researched the influence of reaction time on the contact angle of the copolymers.3) Study on synthesis and properties of new sugar-based polycarboxylate type superplasticizer: Taking MASE, AA, MAA, APEG, SAS as main raw materials, new sugar-based polycarboxylate type superplasticizer(PC-1) was synthesized by means of free radical polymerization and was characterized by FT-IR. The factors influencing on the reaction were determined through orthogonal experiment. The optimum reaction conditions of PC-1 were determined by the changes of initiator amount, reaction time and dosage of MASE. Through analysis of the intrinsic viscosity, the influence of different molecular weight of PCA on the fluidity of cement paste was tested. The PC-1 has effect on the decentralized stabilization of cement particle by testing of Zeta potential. The test of compression strength and the analysis of cement paste porosity show that the cement pore size distribution was changed by the adding of PCA, which lead a greater flexural strength, and compression strength on the cement paste. The analysis of XRD and cement hydration heat showed that the PCA has retarding effect on initial hydration of cement.In this dissertation, the optimum conditions for synthesis of MASE were studied and discussed. The copolymers in different types and different functions with MASE were obtained though the copolymerization reaction. All of this work has some innovation. It would broad the research fields of sucrose derivatives and provide important theoretical basis for biomass energy to replace traditional oil energy. |
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