Method for producing trimethylcyclododecatriene
A technology of trimethylcyclododecatriene and isoprene, which is applied in the field of preparing trimethylcyclododecatriene, and can solve the problems such as the decrease of CDT yield
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Embodiment 1
[0043] Embodiment 1 (comparative example)
[0044] 0.5 liter of benzene with a water content of 15 ppm was filled into a 1.5 liter glass autoclave with a nitrogen atmosphere. Then add 42.5 ml ethyl aluminum sesquichloride (20% solution in benzene) and 13.2 ml TiCl 4 (5% solution in benzene). The autoclave was closed and the reaction mixture was warmed to 40 °C. At this temperature, 343 g of isoprene were added within 4 hours. During the addition of isoprene, the temperature inside the autoclave was kept constant at 40°C. Stirring of the reaction mixture was continued at 40° C. for 1 hour after the end of the addition, and finally the catalyst was decomposed by adding 25% aqueous sodium hydroxide solution. The organic reaction mixture contained 48.81% TMCDT, and 3.48% cyclic and linear C 10 Dimer and 4.85% linear trimer and 29.4% polymer component.
Embodiment 2
[0045] Embodiment 2 (according to the present invention)
[0046] 0.5 liter of benzene with a water content of 15 ppm was filled into a 1.5 liter glass autoclave with a nitrogen atmosphere. Then add 84.9 ml ethyl aluminum sesquichloride (20% solution in benzene) and 13.2 ml TiCl 4 (5% solution in benzene). The autoclave was closed and 201 mg of ammonia gas was added through a septum with stirring at room temperature. The reaction mixture was warmed to 40 °C. At this temperature, 170.5 g of isoprene were added within 4 hours. During the addition of isoprene, the temperature inside the autoclave was kept constant at 40°C. Stirring of the reaction mixture was continued at 40° C. for 1 hour after the end of the addition, and finally the catalyst was decomposed by adding 25% aqueous sodium hydroxide solution. The organic reaction mixture contained 60.27% TMCDT, and 14.07% cyclic and linear C 10 Dimer and 4.14% linear trimer and 13.35% polymer component.
Embodiment 3
[0047] Embodiment 3 (according to the present invention)
[0048] 4 liters of benzene having a water content of 15 ppm was filled into a 10 liter stainless steel autoclave with a nitrogen atmosphere. Then add 76.8 ml ethyl aluminum sesquichloride (20% solution in benzene) and 16.3 ml TiCl 4 (5% solution in benzene). The autoclave was closed and 296 mg of ammonia gas was added through a septum with stirring at room temperature. The reaction mixture was warmed to 40 °C. At this temperature, 2716 g of isoprene was added at a flow rate of 7 g / min. During the addition of isoprene, the temperature inside the autoclave was kept constant at 40°C. Stirring of the reaction mixture was continued at 40° C. for 2 hours after the end of the addition, and finally the catalyst was decomposed by adding 25% aqueous sodium hydroxide solution. The organic reaction mixture contained 53.12% TMCDT, and 9.85% cyclic and linear C 10 Dimers and 2.29% linear trimers.
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