微波辐射合成L-乳酸铝研究

Study of the Synthesis of Aluminum L-lactate with Microwave Radiation Heating Method

利用正交设计L25(54)安排实验,以L-乳酸铝产率为考察指标,通过极差分析和方差分析优化微波辐射加热合成L-乳酸铝制备工艺。极差分析结论得到以L-乳酸、铝粉为原料,在自制催化剂存在下,合成L-乳酸铝正交实验法优选的最佳反应条件是反应时间12 h,微波功率350 W,wL-乳酸=0.05,nL-乳酸:n铝=2.935。方差分析确定了时间A、微波功率B、乳酸浓度C、乳酸/铝摩尔数比D4个因素对产率影响显著性的相对大小顺序是A>C>D>B,时间是显著影响因素。在优选的条件下合成了L-乳酸铝,产率达77.0%,对合成产品进行了红外光谱、纯度、熔点、旋光度、溶解度测试。相同条件下的对照实验结果表明,微波辐射加热反应产率是传统加热方法的5倍。

Under microwave radiation and catalyst,aluminum L-lactate is synthesized with L-lactic acid and aluminum.To optimize the experimental parameters of the preparation techniques,orthogonal experment L25（54） is designed with yield of aluminum L-lactate as referring index.Considering the results of range analysis,we obtaine that the time of reaction 12h,the microwave power output 350W,the concentration of L-lactic acid 0.05 and n（L-lactic acid）：n（aluminum）=2.935,are the most favorable condition.The yield of aluminum L-lactate is 77.0%. The results of variance analysis indicate that the times of reaction have the remarkable influence to the yield of aluminum L-lactate, and the order of remarkable influence is A 〉 C 〉 D 〉 B. Furthermore, the aluminum L-lactate of sample prepared under the optimized expermental condition is measured by IR, rap. , optical rotation, etc. The results of comparative experiments show： the yield of aluminum L-lactate of microwave radiation heating is fivefold of the conventional heating method.