1-丁烯高效氢甲酰化制戊醛的工艺条件探索

Identification of the optimum conditions for highly active hydroformylation of 1-butene to produce pentanal

以WHF-0.5自控高压釜为反应器,以质量分数为97%的正戊醛作为反应溶剂,采用乙酰丙酮三苯基膦羰基铑(Cat)和配体三苯基膦(PPh3)作为催化剂体系,探讨能够同时达到高转化率和高正异比的1-丁烯氢甲酰化制戊醛的最优工艺条件。本文对能够影响1-丁烯氢甲酰化制戊醛反应的8个单因素进行了实验考评并对部分重要因素进行了正交实验,结果表明:在反应温度100℃、反应压力2.5 MPa、搅拌速率200 r/min、反应时间3.5 h、溶剂用量125 m L(25%)、膦铑(P/Rh)物质的量之比600、1-丁烯用量10 m L(0.2393 mol/L)和催化剂浓度1.25 mmol/L的条件下,1-丁烯的转化率达86.84%,产物正异比(mN/mI)达10.98,催化剂的转化频率237.48 h-1。

The optimum conditions for simultaneously achieving high conversion and high n / iso ratio in 1-butene hydroformylation to produce pentanal have been investigated using a WHF-0. 5 autoclave as the reactor,97% n-valeraldehyde as the reaction solvent and Rh( C5H7O2)( PPh3)3( CO) and triphenyl phosphine as the catalyst system.Eight factors influencing the reaction were examined and orthogonal experiments were carried out. The results showed that under the conditions of a temperature of 100 ℃,pressure of 2. 5 MPa,stirring rate of 200 r / min,reaction time of 3. 5 h,solvent amount of 125 m L( 25%),molar ratio [PPh3]/[Rh]= 600,l-butene amount 10 m L( 0. 2393 mol/L) and [Cat]= 1. 25 mmol/L,the 1-butene conversion,the n /iso ratio of the products,and the turnover frequency could respectively reach 86. 84%,10. 98,and 237. 48 h-1.