催化氧化合成邻苯二甲醛工艺的响应面优化的研究
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摘要
以制备的Co/Mo/γ-Al_2O_3为催化剂,采用过氧化氢催化氧化工艺合成邻苯二甲醛,在前期实验基础上,通过响应面法对邻苯二甲醛的合成工艺参数进行了优化,选用Box-Behnken对实验进行设计,研究了对反应有较大影响的反应时间、反应温度及过氧化氢加量三个因素对邻苯二甲醛收率的影响,得到最佳工艺条件并进行模型的建立。实验表明:过氧化氢催化氧化合成邻苯二甲醛的优化工艺条件为:邻苯二甲醇的加量为5g,30%过氧化氢加量15g,反应温度为81℃,反应时间为3h,催化剂为0. 3g,邻苯二甲醛收率可达51. 4%。使用傅里叶红外光谱、核磁共振氢谱、气相色谱对产品结构进行了分析表征。
Phthalaldehyde was synthesized from the catalytic oxidation process with hydrogen peroxide,using the prepared Co/Mo/γ-Al_2O_3 as the catalyst.Response surface methodology was used to optimize the synthesis process for phthalaldehyde on the basis of previous experiments.Box-Behnken composite design was adopted to investigate the influences of reaction time,reaction temperature and hydrogen peroxide dosage on the yield. The optimal conditions were obtained by response surface methodology,and a quadric polynomial regression model was established. The results showed that the optimal conditions were as follows: amount of 1,2-benzenedimethanol 5 g,amount of 30%hydrogen peroxide 15 g,temperature of 81℃,reaction time of 3 h and dosage of catalyst 0. 3 g.Under the optimal condition,the average yield was 51. 4%. The structure and composition of the products were analyzed and identified by infrared spectroscopy,nuclear magnetic resonance and gas chromatography.
Phthalaldehyde was synthesized from the catalytic oxidation process with hydrogen peroxide,using the prepared Co/Mo/γ-Al_2O_3 as the catalyst.Response surface methodology was used to optimize the synthesis process for phthalaldehyde on the basis of previous experiments.Box-Behnken composite design was adopted to investigate the influences of reaction time,reaction temperature and hydrogen peroxide dosage on the yield. The optimal conditions were obtained by response surface methodology,and a quadric polynomial regression model was established. The results showed that the optimal conditions were as follows: amount of 1,2-benzenedimethanol 5 g,amount of 30%hydrogen peroxide 15 g,temperature of 81℃,reaction time of 3 h and dosage of catalyst 0. 3 g.Under the optimal condition,the average yield was 51. 4%. The structure and composition of the products were analyzed and identified by infrared spectroscopy,nuclear magnetic resonance and gas chromatography.
引文
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[2]欧燕妮,梁祖兰,叶婉华,等.邻苯二甲醛对内镜消毒效果的观察[J].现代临床护理,2012,11(1):31-32.
[3]周晓亮,李雯.邻苯二甲醛与戊二醛消毒消化内镜的比较研究[J].中国微生态学杂志,2013,25(4):454-456.
[4]林江,高珊,徐海莉,等.邻苯二甲醛、戊二醛、含氯消毒剂内镜消毒效果及耐用性比较[J].护士进修杂志,2013,28(15):1414-1415.
[5]栾丽.邻苯二甲醛与戊二醛用于内镜消毒的对比研究[J].医疗装备,2016,29(14):96-97.
[6]王孝友,曾秀,孔路军,等.邻苯二甲醛杀菌作用研究[J].四川畜牧兽医,2003,30(1):28-29.
[7]Cabrera Martinez RM,Setlow B,Setlow P. Studies on the mechanisms of the sporicidal action of ortho-phthalaldehyde[J].Appl Microbiol,2002,92(4):675-680.
[8]徐克勋.精细有机化工原料及中间体手册[M].北京:化学工业出版社,2004:157-158.
[9]刘鸿.邻苯二甲醛合成新工艺[J].精细化工中间体,2004,34(4):45-47.
[10]成西涛,唐璇,王思晨,等.邻苯二甲醛合成新工艺研究[J].应用化工,2007,36(8):767-769.
[11]Gosteli Jacques. Multiple substituted o-phthalaldehyde[P]:EP:19793230,1979-04-12.
[12]Hiral Naruhisa,Himeji Shi.Process for producing dialdehyde[P]:EP:1078908,2001-02-28.
[13]Ronald R Ramos,Carmelo Bolivar,Jimmy Castillo,et al.Ultrasound assisted synthesis of nanometric Ni,Co,Ni Mo and Co Mo HDS catalysts[J]. Catalysis Today,2008:277-281.
[14]VALDéS H,ZAROR C.A.Ozonation of benzothiazole saturated-activated carbons:influence of carbon chemical surface properties[J]. J Hazard Mater,2006,137(2):1042-1048.
[15]Peris Vicente J,Gimeno Adelantado J V.Characterization of proteinaceous glues in old paintings by separation of the o-phtalaldehyde derivatives of their amino acids by liquid chromatography with fluorescence detection[J].Talanta,2006,68(5):1 648-1 654.
[16]成西涛,李稳宏,黄方方,等.响应面法优化双羟丙基封端聚硅氧烷的微波合成工艺研究[J].化学研究与应用,2015,27(12):1 849-1 855.