Dissertation > Industrial Technology > Chemical Industry > Production of solvents and plasticizers > Plasticizer

Synthesis and Application of Tri-n-butyl Citrate and Acetyl Tributyl Citrate

Author DuXiaoZuo
Tutor JiangPingPing
School Jiangnan University
Course Chemical processes
Keywords Plasticizer Tributyl citrate Acetyl tributyl citrate Esterification catalyst Acetylation reaction
Type Master's thesis
Year 2007
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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 .

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