Preparation Of Acrylic Epoxy Cyclohexyl Ester And Emulsion Polymerization And Bulk Polymerization

With the increasingly stringent requirements for ecological protection and the successful industrialization of acrylate products and new applications,the world ’ s acrylate production capacity has increased significantly.In this thesis,epoxycyclohexane was used to modify acrylic acid / methacrylic acid under different catalysts.The generated esters were evaluated according to the different catalysts added.In addition,emulsion polymerization and bulk polymerization of the ester were studied.In the process of emulsion polymerization,the problem of organic solvent volatilization and environmental pollution was avoided by adding epoxycyclohexane acrylate.In this thesis,acrylic epoxy cyclohexane ester emulsion was synthesized by core-shell emulsion method,and the properties and structure of the emulsion were analyzed.In addition,poly(acrylic acid-epoxycyclohexane ester)was synthesized by continuous bulk polymerization,and the matching,composition,reaction and conditions of the polymer were investigated.By adjusting the formula group and reaction conditions,the optimal experimental formula for continuous bulk polymerization and polymerization was obtained.The properties of the polymer were tested and analyzed.(1)Firstly,the synthesis of ionic liquid [Beim]Br with 1-ethylimidazole and bromobutane was studied and the structure of the ionic liquid was characterized.Cyclohexyl 1-hydroxymethylacrylate was synthesized by direct esterification using epoxy cyclohexane(CHO)and methacrylic acid(MAA)as raw materials,hydroquinone as inhibitor,ionic liquid[Beim]Br,triethyl benzyl ammonium chloride(TEBAC),benzyl trimethyl ammonium chloride(DMBAC)and tetrabutyl ammonium chloride(TBAC)as catalysts.The structure of the synthesized ester was characterized.The effects of reaction time,reaction temperature,catalyst dosage and molar ratio of reactants on the yield of the product were investigated by orthogonal test with the conversion rate and color gloss as indexes.The optimum process conditions for the preparation of 1-hydroxymethylacrylate ring and hexane ester under catalysis were determined as follows: reaction time,4h,reaction temperature,85°C,catalyst dosage,0.3% and molar ratio of reactants 1.1.By comparison,it was found that ionic liquid[Beim]Br had better catalytic effect in the reaction of MAA and CHO,and the highest yield was 97.4%.Light yellow transparent liquid.(2)Acrylic epoxycyclohexane ester emulsion was synthesized by core-shell emulsion polymerization with dodecyl sulfonic acid,sodium as emulsifier,acrylic acid(AA)as functional monomer,butyl acrylate,ester(BA)as shell monomer,and the target product prepared with(1)as core monomer,and polymerization in redox initiation system.The effects of emulsification,dosage of agent,initiator,functional monomer,dosage and polymerization temperature on the properties of emulsion and liquid were investigated.The following conclusions were obtained in many experiments: emulsifier dosage was about 3%,initiator dosage was about 0.3%,functional monomer dosage was about 1%,core-shell ratio was about1:1,shell emulsion droplet addition time was about 1.5h,polymerization temperature was about 70°C,and the dosage of deionized water was about 2 times.The synthesized emulsion had good performance with solid emulsion,content of about 35%,and monomer conversion rate of about 96.65%.The chemical and chemical structures of acrylic acid and epoxycyclohexane ester emulsions were characterized by FT-IR,and the latex particles were observed in the particle size distribution.The particles distribution is uniform,and the particle radius is about 0.7nm.(3)Continuous bulk polymerization with peroxide,benzoyl(BPO)as initiator and target product(1)as monomer was studied.The synthesized homopolymer was characterized by Fourier transform infrared spectroscopy.The results showed that polymerization could occur under all experimental conditions.The effects of polymerization temperature,polymerization time,initiator dosage and amount on the polymer were investigated by using the method of controlling variables.The experimental results showed that the polymerization time was controlled at about 30 min,the temperature was controlled at about 75°C,and the amount of initiator was about 0.3% of the total reaction amount.The structure and product properties of the polymer were characterized by 1H-NMR,GPC,DSC and infrared spectroscopy.