N-乙烯基己内酰胺的合成及放大

Synthesis of N-vinylcaprolactam and its scale-up experiment

以己内酰胺和乙炔为原料,己内酰胺与叔丁醇钾制得的己内酰胺钾盐为催化剂,对叔丁基邻苯二酚为阻聚剂合成N-乙烯基己内酰胺.考察催化剂用量、阻聚剂用量、搅拌速率、反应温度及反应时间对产品收率的影响.用红外光谱仪、核磁共振波谱和质谱对产品结构进行表征.并依据小试条件进行放大实验.结果表明:在催化剂用量为3.5%,阻聚剂用量为0.04%(以己内酰胺质量计),搅拌速率200r/min,温度90℃,反应8h的优化工艺条件下,产品收率为75.4%,质量分数达99.87%.放大40倍后,产品收率为74.6%.

N-vinylcaprolactam （NVCL） was synthesized with caprolactam （CL） and acetylene as raw ma- terials, caprolactam potassium as catalyst, and 4-tert-butyleatechol （TBC） as inhibitor. The effect of cata- lyst dosage, inhibitor dosage, stirring rate, reaction temperature and reaction time on product yield was in- vestigated. The structure of product was characterized with infrared spectroscope （FT-IR）, nuclear mag- netic resonantor （NMR）, and mass spectrometer （MS）. The scale-up experiment on NVCL synthesis was conducted on the basis of the original experiment. The result showed that the optimum reaction conditions would be as follows： the mass-fraction of catalyst was 3. 5% that of inhibitor-0, 04%, stirring rate was 200 r/min, reaction time-8 h and reaction temperature-90 ℃. The yield of NVCL reached 75.4% and its mass- fraction- 99. 87%. Magnified by 40 times, the product yield was 74. 6%.