Study On The Synthetic Technology Of Hydroxybutyl Vinyl Ether

Hydroxybutyl vinyl ether (HBVE) is a very important intermediate in organic synthesis and polymer monomer. It is widely used in many fields such as coating, adhesive, printing ink, lubricant, plasticizer, elastomer, foam, pesticide and surface protection material etc.The key of the paper is to choose the best catalyst, while in this situation, the optimum process for synthesis of HBVE used by acetylene in atmospheric pressure has been researched. Then the crude product of HBVE was refined and the high purity sample was obtained.In the process for researching the effect of single catalysts, it was found that the catalytic effect of KOH and potassium tert-butoxide were the best. Then some catalysts were mixed, and it was found that the conversion rate of BDO was 31.9% and the yield of HBVE was 58.8% while the potassium alcoholate prepared by KOH and raw alcohol was mixed with P(Ph) 3 and ZnO. The catalytic effect of some supported catalysts was not well. KOH/Al2O3 that wasn't calcined had the best catalytic effect.The optimum process for synthesis of HBVE was confirmed from single factor experiment and orthogonal experiment:m(KOH)/m(BDO)=13.5%; m(P(Ph)3)/m(Zn0)=1;m(P(Ph)3+Zn0) /m(BDO)=3%; m(DMPE-300)/m(BDO)=1.5; Reaction temperature was 140℃; Reaction time was 9 h. KOH, BDO and polyethylene glycol dimetyl ether(DMPE-300) were firstly mixed heated,vacuumed distillated and dehydrated under the vacuum≥0.090 MPa, which kept the temperature of 100 to 120℃for 1 to 2 hours. Then P(Ph)3 and ZnO were added in this reaction solution before which was heated. And N2 was through into the system firstly and then acetylene was in slowly by bubbling. Observe the tail gas bubbles so that a slight excess. Under the optimum process condition, three times repeated experiments were done and the average yield of HBVE was 42.5%.The reaction solution was vacuumed distillated under the pressure of 2 kPa, collecting fractions with the temperature of residue below 180℃. Reducing substances NaBH4 was added before the vacuum distillation of this crude product of HBVE. Specifications of distillation column:Φ2.4×100 cm. The packing was stainless steel ofσring. And the height of packing was 85 cm. Under the pressure between 0.5 and 0.7 kPa, the purity of the distillate HBVE which collected from 58 to 60℃was up to 97.0%, and the yield was 77.2%.Synthesis of DBVE and vinylation of different diols have also been researched exporingly. It was concluded that the best yield of DBVE was in which the product was continued to bring out in the reaction with the reaction temperature of 150℃. In addition, diols with more carbon atoms and farther away from two hydroxyl groups had easier ability of vinylation.