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Efficient synthesis method of acetyl tributyl citrate

A technology for acetyl tributyl citrate and tributyl citrate, which is applied in the field of efficient synthesis of acetyl tributyl citrate, can solve the problems of harsh catalyst synthesis conditions and low yield, and achieves high selectivity and yield. High, high catalytic activity effect

Inactive Publication Date: 2017-07-07
FOSHAN FEISHIDA NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst synthesis conditions used in it are harsh, the yield is not high, and the yield of the product needs to be further improved

Method used

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  • Efficient synthesis method of acetyl tributyl citrate

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Embodiment 1

[0025] A kind of efficient synthetic method of acetyl tributyl citrate, comprises the following steps:

[0026] (1) mixing and stirring trifluoroacetic acid and concentrated sulfuric acid evenly to obtain a mixed acid catalyst; wherein, the content of fluoroacetic acid in the mixed acid catalyst is 10wt%;

[0027] (2) Stir tributyl citrate, n-butanol and acetic anhydride at room temperature for 10 minutes, then transfer to a three-necked flask, add the mixed acid catalyst prepared above, and react for 3 hours at 55° C. After the reaction, cool to At room temperature, remove the catalyst by filtration, cool the filtrate to room temperature after vacuum distillation, and wash with 8% sodium bicarbonate solution to neutrality, separate the organic phase, dry the organic phase with anhydrous copper sulfate, filter, and decompress the filtrate Distillation to obtain acetyl tributyl citrate; wherein, the mass ratio of tributyl citrate, n-butanol and acetic anhydride is: 1:2:1; the a...

Embodiment 2

[0029] A kind of efficient synthetic method of acetyl tributyl citrate, comprises the following steps:

[0030] (1) Trichloroacetic acid and concentrated sulfuric acid are mixed and stirred uniformly to obtain a mixed acid catalyst; wherein, the content of trichloroacetic acid in the mixed acid catalyst is 33wt%;

[0031] (2) Stir tributyl citrate, n-butanol and acetic anhydride at room temperature for 20 minutes, then transfer to a three-necked flask, add the mixed acid catalyst prepared above, and react for 1.5 hours at 95°C. After the reaction, cool to room temperature, remove the catalyst by filtration, cool to room temperature after the filtrate is distilled under reduced pressure, and wash to neutrality with a sodium bicarbonate solution with a mass fraction of 8%, separate the organic phase, dry the organic phase with anhydrous copper sulfate, filter, and the filtrate reduces Press distillation to obtain acetyl tributyl citrate; wherein, the mass ratio of tributyl citra...

Embodiment 3

[0033] A kind of efficient synthetic method of acetyl tributyl citrate, comprises the following steps:

[0034] (1) Mix and stir trifluoroacetic acid, trichloroacetic acid and concentrated sulfuric acid evenly to obtain a mixed acid catalyst; wherein, the content of trifluoroacetic acid and trichloroacetic acid in the mixed acid catalyst is 7wt%, 8wt%;

[0035] (2) Stir tributyl citrate, n-butanol and acetic anhydride at room temperature for 10 minutes, then transfer to a three-necked flask, add the mixed acid catalyst prepared above, and react at 60°C for 2.7 hours. After the reaction, cool to room temperature, remove the catalyst by filtration, cool to room temperature after the filtrate is distilled under reduced pressure, and wash to neutrality with a sodium bicarbonate solution with a mass fraction of 8%, separate the organic phase, dry the organic phase with anhydrous copper sulfate, filter, and the filtrate reduces Press distillation to obtain acetyl tributyl citrate; w...

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Abstract

The invention discloses a high-efficiency synthesis method of acetyl tributyl citrate, which specifically comprises the following steps: first, mix an organic acid and concentrated sulfuric acid to prepare a mixed acid catalyst; then use tributyl citrate, n-butanol, acetic anhydride As a raw material, under the catalysis of the mixed acid catalyst prepared above, react, after the reaction, cool to room temperature, remove the catalyst by filtration, cool to room temperature after the filtrate is distilled under reduced pressure, and wash with sodium bicarbonate solution until neutral, separate The organic phase was dried with anhydrous copper sulfate, filtered, and the filtrate was distilled under reduced pressure to obtain acetyl tributyl citrate. The catalyst adopted in the method has good catalytic effect, low acid consumption, low cost and high product yield.

Description

[0001] Technical field: [0002] The invention relates to the field of organic synthesis, in particular to a high-efficiency synthesis method of acetyl tributyl citrate. [0003] Background technique: [0004] Acetyl tributyl citrate (ATBC), molecular formula C 20 h 34 o 8 , molecular weight 402.8. The substance is a colorless, odorless oily liquid, insoluble in water, highly resistant to hydrolysis, even boiled in boiling water for 6 hours without hydrolysis, soluble in most organic solvents, compatible with ethyl cellulose, polyvinyl chloride, polystyrene, polyacetic acid Compatible with vinyl esters, chlorinated rubber, etc. The relative density is 1.046 (20°C), the refractive index is 1.4410 (25°C), the boiling point is 343°C (0.1MPa), 173°C (133Pa), the flash point is 204°C, and the viscosity is 0.0427Pa·s (25°C). It is safe and biodegradable, and can be used as food packaging materials, medical appliances, and children's toys. [0005] Traditional plasticizers can i...

Claims

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Application Information

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IPC IPC(8): C07C69/67C07C67/31C07C67/54
CPCC07C67/31C07C67/54
Inventor 陈兴建
Owner FOSHAN FEISHIDA NEW MATERIAL TECH CO LTD
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