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Synthesis Of (3,4-Epoxycyclohexyl) Methyl Methacrylate

Posted on:2017-06-21Degree:MasterType:Thesis
Country:ChinaCandidate:X H SunFull Text:PDF
GTID:2311330503459911Subject:Chemical Engineering and Technology
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3-Cyclohexenylmethyl methacrylate was synthesized by transesterification using methyl methacrylate and 3-cycloexene-1-methanol as raw materials. The effects of the factors such as catalyst type, catalyst amount, raw material ratio, reaction time,inhibitor type and amount on reaction results were investigated. The obtained optimum reaction conditions were using Organotin as catalyst, m?Organotin?:m?3-cycl-ohexene-1-methanol?=0.06, inhibitor 1 as inhibitor, m?inhibitor1?:m?3-cyclohexene-1-methanol?=0.001, reaction time 5h, reaction temperature105-120 ?, raw materal ratio n?MMA?:n?3-cyclohexene-1-methanol?=3:1. Under above conditions, the conversion of 3-cyclohexene-1-methanol was> 97 %, while the product yield was> 94 %. The structure of the product was characterized by FT-IR and 1H NMR.3-Cyclohexenyl methacrylate was synthesized by transesterification using methacrylate and 3-cycloexene-1-methanol as raw materials. The effects of the factors such as catalyst type, catalyst amount, raw material ratio, reaction time, inhibitor type and amount on reaction results were investigated. The obtained optimum reaction conditions were using Organotin as catalyst, m?catalyst?:m?3-cyclohexene-1-methanol?=0.04, inhibitor 1 as inhibitor, m?inhibitor 1?:m?3-cyclohexene-1-methanol? =0.001, reaction time 7h, reaction temperature100-110 ?, raw materal ratio n?MMA? : n?3-cyclohexene-1-methanol?=3.5:1. Under above conditions, the conversion of 3-cyclohexene-1-methanol was > 95 %, while the product yield was > 91 %. The structure of the product was characterized by FT-IR and 1H NMR.The synthesis of?3, 4-Epoxycyclohexyl? methyl methacrylate was studied, using3-cyclohexenylmethyl methacrylate as material, KHSO5 as oxidant. The effects of the factors such as feeding methods and the amount of KHSO5, the amount of solvent,reaction time, feeding methods and the amount of NaHCO3, dropping rate of KHSO5,stirring speed and reaction temperature on reaction results were investigated. The obtained optimum reaction conditions were n?3-cyclohexenylmethyl methacrylate?:n?KHSO5?:n?NaHCO3?:n?solvent 1?=1:1.4:3:22, dropping time of KHSO5 30 min,stirring speed 500 r/min, reaction time 6 h, reaction temperature 0 ?. Under above conditions, the conversion of 3-cyclohexenylmethyl methacrylate was > 97 %, while the product yield was > 96 %. The structure of the product was characterized by FT-IR and 1H NMR.The synthesis of?3,4-Epoxycyclohexyl? methacrylate was studied, using3-cyclohexenyl methacrylate as material, KHSO5 as oxidant. The effects of the factors such as feeding methods and the amount of KHSO5, the amount of solvent, reaction time, feeding methods and the amount of NaHCO3, dropping rate of KHSO5, stirring speed and reaction temperature on reaction results were investigated. The obtained optimum reaction conditions were n?3-cyclohexenyl methacrylate?:n?KHSO5?:n?NaHCO3?:n?solvent 1?=1:1.4:2.5:18, dropping time of KHSO5 30 min, stirring speed400 r/min, reaction time 4 h, reaction temperature 0 ?. Under above conditions, the conversion of 3-cyclohexenylmethyl methacrylate was > 99 %, while the product yield was > 96 %. The structure of the product was characterized by FT-IR and 1H NMR.
Keywords/Search Tags:3-cyclohexene-1-methanol, 3-cyclohexenylmethyl methacrylate, KHSO5, epoxidation transesterification
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