用于邻苯二甲酸二丁酯(DBP)合成的TiO_2-SO_4^(2-)型固体超强酸催化剂的研究

The Study of Solid Super Acid TiO_2-SO_4^(2-)-Catalyst Applied for the Synthesis of DBP

对用于邻苯二甲酸二丁酯(DBP)合成的TiO_2—SO_4^(2-)型固体超强酸催化剂进行了研究。考察了H_2SO_4浓度、与H_2SO_4接触时间、焙烧温度和时间等制备条件对催化剂活性的影响,并考察了催化剂用量、原料醇酐摩尔比、酯化温度对产品DBP收率的影响。结果表明,制备TiO_2—SO_4^(2-)固体超强酸催化剂的最佳工艺为,采用1N H_2SO_4淋洗TiO_2·nH_2O粉末,并在500℃焙烧3小时。醇酐酯化反应随催化剂用量、醇酐摩尔比和酯化温度的增加,DBP收率随之增加,但催化剂用量3.0～3.5%、醇酐摩尔比2.5、酯化温度155℃,回流5小时,DBP收率可达100%。以TiO_2—SO_4^(2-)固体超强酸替代H_2SO_4用于DBP合成,具有工业推广价值。

The solid super acid TiO_2-SO_4^(2-)catalyst applied for the synthesis of DBP was studied in this paper. The influence ofpreparing conditions such as the concentration and contacting time with H_2SO_4 , calcing temperature and time on the activity ofthe catalyst was investigated, and the best preparing process was selected. The influence of the adding amount of the catalyst, ofthe mole ratio of the reactants and the esterifying temperature on the conversion of DBP were also investigated, and the resultswere given in this paper. By infra-red and DSC-TG analysis, the contraction of the catalyst and the reason for the loss of ac-tivity were studied. The replacement of H_2SO_4 with solid super acid in the synthesis of DPB is worth to popularize inindustry.