The Synthesis Of Pinane-base Hydroxyl-terminated Polyether

This paper use-pinene as raw material, acetic acid peroxide as oxidant, benzyl triethylammonium chloride （TEBA） as phase transfer catalyst, then2,3-pinane epoxy wassynthesized.Influences of single factors on the reaction results were discussed, appropriateepoxidation process conditions of-pinene were put forward:1.0mol of-pinene, benzyltriethyl ammonium chloride as0.1%raw material quality,0.8times of the mass of sodiumcarbonate as raw material, solvent methylene chloride as3times as the quality of raw material,drip1.3times homemade35%peracetic acid of the raw material at20, and mechanicalstirring2h after finish droping. The conversion rate of-pinene close to100%, the yields of2,3-epoxy pinane above90%. Use GPC, FT-IR, GC/MS, GC methods on product structurecharacterization and the epoxidation mechanism of-pinene was discussed.2,3-epoxy pinane and epoxy chloropropane （ECH） as raw material, boron trifluoride ethylether （BF₃·OEt₂） as catalyst, ethylene glycol （EG） as starting agent, then2,3-epoxy pinanehomopolymerization and epoxy chloropropane （ECH） copolymerization reaction werehappened. FT-IR, EA and1H NMR analysis results show that the monomer in thehomopolymerization and copolymerization reaction of low molecular weight,hydroxyl-terminated new pinane-base polyether and pinane-base-ECH polyether wereprepared respectively.The optimal technical conditions for synthesis of two kinds of polyether was discussed,optimum process conditions of pinane-base polyether for:1.0%of the mass of catalyst dosageof BF₃·OEt₂as raw materials, initiator dosages of EG are1.2%of the raw material quality,dosages of CH₂Cl₂as raw material quality, reaction time of5h at temperature0.Pinane-base-ECH polyether:n（2,3-epoxy pinane）:n（ECH） was0.5:1, catalyst dosages ofBF₃·OEt₂are1.0%of the raw material quality, initiator dosages of EG are1.5%of the rawmaterial quality, dosages of CH2Cl2as raw material quality, reaction time of6h at temperature0. Under this technological conditions, pinane-base polyether was heavy molecular weight（MW） of500g.mol-1, pinane-base-ECH polyether of heavy molecular weight （MW） of700g.mol-1.