Catylatic synthesizing method of acetyl tri-in-butyl citrate

A technology for the synthesis of acetyl tri-n-butyl citrate, which is applied in chemical recovery, organic chemistry, etc., can solve the problems of complex product refining, many side reactions, and high price, achieve excellent catalytic performance, avoid separation difficulties, and prepare simple effect

Inactive Publication Date: 2005-12-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

P-toluenesulfonic acid, sulfamic acid, pyridine, etc. are used as catalysts to synthesize acetyl tri-n-butyl citrate. The refining of the product is more complicated, the catalyst and the product are not easy to separate, the product quality is difficult to guarantee, and the catalyst cannot be recycled, and the production cost is obvious. Improve; There is also the use of loaded solid superacid as a catalyst to synthesize acetyl tri-n-butyl citrate, the preparation of the catalyst is complicated, the price is expensive, and the conversion rate of tributyl citrate is not high, which brings difficulties for product refining; there is also the use of Inorganic strong acids such as concentrated sulfuric acid and concentrated hydrochloric acid are used as catalysts to synthesize tri-n-butyl acetyl citrate, but the above-mentioned catalysts severely corrode equipment, have many side reactions, and the refining of products is more complicated. recycle and re-use

Method used

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  • Catylatic synthesizing method of acetyl tri-in-butyl citrate

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Experimental program
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Effect test

Embodiment 1

[0016] According to the molar ratio of tri-n-butyl citrate and acetic anhydride as 1:1.8, weigh 18.02 g of tri-n-butyl citrate, 9.18 g of acetic anhydride, and 0.54 g of catalyst sodium bisulfate, put them into a three-necked flask, and place them in a water bath. Keep the temperature of the reaction solution at 60°C, stir and react for 90 minutes, and the yield of acetyl tributyl citrate is 99.3%. There is no peak of tri-n-butyl citrate on the gas chromatogram, indicating that tri-n-butyl citrate has been completely converted . After the crude product obtained by the reaction is suction filtered to recover the catalyst, acetic anhydride and acetic acid are recovered by distillation under reduced pressure, and then washed with deionized water, 5% sodium carbonate aqueous solution, and then washed with water until the water phase is neutral, and the water is removed by distillation under reduced pressure , That is, tri-n-butyl acetyl citrate. According to gas chromatography an...

Embodiment 2

[0018] According to the molar ratio of tri-n-butyl citrate and acetic anhydride as 1:1.5, weigh 18.02 g of tri-n-butyl citrate, 7.65 g of acetic anhydride, and 0.90 g of catalyst potassium bisulfate, put them into a three-necked flask, and place them in a water bath. Keep the temperature of the reaction solution at 70°C, stir and react for 60min, the yield of acetyl tri-n-butyl citrate is 99.5%, and there is no peak of tri-n-butyl citrate on the gas chromatogram, indicating that tri-n-butyl citrate has been Totally converted. After the crude product obtained by the reaction is suction filtered to recover the catalyst, acetic anhydride and acetic acid are recovered by distillation under reduced pressure, and then washed with deionized water, 10% aqueous sodium hydroxide solution, and then washed with water until the water phase is neutral, and then removed by distillation under reduced pressure. water, that is, acetyl tri-n-butyl citrate. According to gas chromatography analys...

Embodiment 3

[0020] According to the molar ratio of tri-n-butyl citrate and acetic anhydride as 1:1.8, weigh 18.02 g of tri-n-butyl citrate, 9.18 g of acetic anhydride, and 0.54 g of catalyst H-type macroporous strong acid cation exchange resin, and add them to a three-necked flask , placed in a water bath, keeping the temperature of the reaction solution at 50°C, stirring and reacting for 45 minutes, the yield of acetyl tri-n-butyl citrate was 99.4%, and there was no peak of tri-n-butyl citrate on the gas chromatogram, indicating that citric acid Tri-n-butyl ester has been completely converted. After the crude product obtained by the reaction is suction filtered to recover the catalyst, acetic anhydride and acetic acid are recovered by distillation under reduced pressure, and then washed with deionized water, 10% aqueous sodium bicarbonate solution, and then washed with water until the water phase is neutral, and then removed by distillation under reduced pressure. water, that is, acetyl ...

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Abstract

This invention has disclosed a kind of catalyzed synthesis method for acetyl tri-n-butyl citrate; its step is as follows: -Join tri-n-butyl citrate and acetic anhydride, catalyst in three-necked flask, which is in water bath, mix and react, gain acetyl tri-n-butyl citrate; -Recover catalyst from above-mentioned coarse product, distill acetic anhydride and acetic by pressure reduction, wash by deionized water and alkaline solution, then bath to water-phase to neutrality, distill water off by pressure reduction. This method is simple and the catalyst used is choiceness recyclable, and easy to gain. In agreeable condition, this method can make tri-n-butyl citrate complete liquefaction basically, have prevented tributyl citrate and acetyl tri-n-butyl citrate from separating problem, the purity of acetyl tri-n-butyl citrate is above 99% analysed by gas chromatography.

Description

technical field [0001] The invention relates to a catalytic synthesis method of acetyl tri-n-butyl citrate. Background technique [0002] Acetyl tri-n-butyl citrate is a new type of non-toxic additive and plasticizer that can be used in plastic processing industries such as food packaging, medical appliances, children's toys, and personal hygiene products. It has good compatibility, and the plasticized plastic has good low-temperature flexibility, and is heat-stable, light-resistant, water-resistant, and cold-resistant when it is melt-sealed. [0003] In the catalytic synthesis method of acetyl tri-n-butyl citrate given in the literature, it mainly lies in the difference of catalyzer, and different catalysts have different effects of synthesizing acetyl tri-n-butyl citrate, and the process of refining is also not the same. P-toluenesulfonic acid, sulfamic acid, pyridine, etc. are used as catalysts to synthesize acetyl tri-n-butyl citrate. The refining of the product is more...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716
CPCY02P20/584
Inventor 何潮洪谢春和金伟光
Owner ZHEJIANG UNIV
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