固体酸催化合成无毒增塑剂柠檬酸三正丁酯

研究了柠檬酸（２－羟基丙烷三羧酸）与丁醇在固体酸催化作用下合成柠檬酸三正丁酯（２－羟 基丙烷三羧酸三正丁酯）的工艺条件，找到了一种工艺简单、反应时间短、酯化率高的合成方法。 实验结果表明：４种固体酸催化剂对反应的催化活性大小依次为ＨＰＷ（磷钨酸）＞ＦｅＣｌ_３·６Ｈ_２Ｏ＞ ＮＨ_４Ｆｅ（ＳＯ_４）_２ １２Ｈ_２Ｏ＞ＳＯ_４~（２－）／ＺｒＯ_２；ＨＰＷ催化合成柠檬酸三正丁酯的的最佳反应条件为：醇酸摩 尔比５０：１，ＨＰＷ用量３％（以酸质量为基准），反应温度１１０～１６０℃，反应时间４～５ｈ，转化率达 ９８％以上，产品纯度＞９９％。

Synthesis of Non-toxic Plasticizer TBC by Solid Acids

The process for synthesis of tri-n-butyl citrate (TBC, i. e. 2-hydroxy-l, 2, 3-propanetricarboxylic acid tributyl ester) using solid acid catalysts is studied, and the older of catalytic activities for catalysts in the reaction of citric acid (2-hydroxy-l, 2, 3-propanetricarboxylic acid) with n-butanol is shown as follows: HPW (tungstophosphoric acid ) > FeCl_3 6H_2O > NH_4Fe(SO_4 )_2,. 12H_2O > SO_4~(2-) /ZrO_2. In the presence of HPW, the Proper technology parameteters for the process are achieved: the molar who of butanol to citric acid is 5: l, the amount of HPW is about 3% upon the mass of citric acid charged in the reaction, the temperature is controlled between 1 10 ~ 16℃ and the reaction time is about 4 ~ 5h, then the conversion of citric acid is above 98%, and the purity of resulting product is over 99%.