Synthesis and Application of Tri-n-butyl Citrate and Acetyl Tributyl Citrate
|Keywords||Plasticizer Tributyl citrate Acetyl tributyl citrate Esterification catalyst Acetylation reaction|
In this paper, for the synthesis of non-toxic plasticizer tributyl citrate and acetyl tributyl citrate to citric acid , butanol and acetic acid , and this the two plasticizers synthesis system research . Select ceric sulfate catalyst for the synthesis of tributyl citrate , the synthesis process parameters on the esterification and acetylation of the best influence the amount of catalyst , reaction temperature , reaction time , ratio of raw materials and other factors of esterification and acetylation reaction , using orthogonal experimental design method to filter out the best of the synthesis process . The synthesized products were determined by infrared spectroscopy and chemical analysis methods . The experimental results show that the best reaction conditions for the catalytic synthesis of tributyl citrate ceric sulfate n ( n-butanol ) : n ( citric acid) = 3.5:1 , catalyst amount of 0.9 % of citric acid , the reaction time was 5.0h, the reaction temperature of 120 ℃ ~ 130 ℃, under the reaction conditions , the the products TBC yield up to 96% . Methyl sulfonic acid as a catalyst of the acylation reaction , and the conditions of the acetylation reaction is also optimized . Optimized process conditions : acetic acid with tributyl citrate molar ratio of 1.4 : 1 , with agent accounts for of Tributyl Citrate quality 15.0 % , and the quality of the catalyst as tributyl citrate quality 1.0% , the reaction temperature of 100 ° C to 120 ° C , the reaction time 2.0H , under this condition , the acylation rate of more than 85% . Purified conditions for both products were determined and the optimum conditions of the washing and bleaching : neutralizer with a 5% NaOH solution , and the time in 40min, and temperature 60 ° C , and after the product acid value is less than 0.2 mgKOH · g-1; activated carbon as a bleaching agent, decolorization conditions : the amount of take 7.5% of the crude quality about a bleaching temperature 80 ° C , the time between 30 ~ 60min appropriate .