Method for preparing tributyl citrate by taking macroporous strong-acid cation exchange resin as catalyst

A technology of strongly acidic cation, tributyl citrate, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of difficult industrialization, inconvenient operation, high investment cost, and the like, Achieve the effect of being conducive to large-scale industrial production, short reaction time and low production cost

Active Publication Date: 2014-03-05
XUZHOU NAILI MACROMOLECULE TECH CO LTD
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Problems solved by technology

[0004] At present, there have been reports in China on the preparation of tributyl citrate from organic acids, solid super acids, phosphotungstic acid, loaded phosphotungstic acid, silicotungstic acid, ionic liquids, mesoporous molecular sieves, mic

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  • Method for preparing tributyl citrate by taking macroporous strong-acid cation exchange resin as catalyst
  • Method for preparing tributyl citrate by taking macroporous strong-acid cation exchange resin as catalyst

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[0021] The scheme and effect of the present invention will be further explained below in conjunction with the implementation case.

[0022] Add 126g of citric acid and 247.5mL of n-butanol to a four-necked flask equipped with electric stirring, thermometer, reflux condenser, and water separator. Heat and stir below 70℃. After the citric acid is completely dissolved, add the above-mentioned macroporous strong acid Cation exchange resin (NKC-9) is used as catalyst 18.9g, heated at 108~140℃ under reflux and stirred to separate the water produced by the reaction from the water separator, and then enter the water separator to stop the reaction until there is no water; after the reaction, add it Stirring 5% NaOH aqueous solution to neutralize unreacted citric acid. After the neutralization reaction is completed, wash with hot water at 60~70℃ until it is neutral. The separated organic phase is at a vacuum degree of -0.08~0.1mpa and temperature Distill off water and excess n-butanol unde...

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Abstract

The invention discloses a method for preparing tributyl citrate by taking macroporous strong-acid cation exchange resin as a catalyst, belonging to a preparation method of tributyl citrate. The method comprises the steps of: reacting citric acid with n-butanol in the presence of macroporous strong-acid cation exchange resin (NKC-9) serving as a catalyst; filtering to remove the catalyst after the reaction reaches the end point; and neutralizing, rinsing, distilling and purifying the product to obtain the tributyl citrate. The separated catalyst can be recycled, and the activity is basically unchanged. By taking the reactant n-butanol as a water-carrying agent, the environmental pollution due to the use of organic solvents such as toxic benzene, methylbenzene and the like can be avoided, and the aftertreatment is convenient; the method has the advantages of mild reaction conditions, short reaction time, no environment pollution and the like.

Description

Technical field [0001] The invention relates to a method for preparing tributyl citrate, in particular to a method for preparing tributyl citrate by using a macroporous strong acid cation exchange resin as a catalyst. Background technique [0002] Tributyl citrate has excellent characteristics such as non-toxic and odorless, cold resistance, light resistance, water resistance, flame retardancy, low volatility, good biodegradability, and high plasticizing efficiency. It is considered by the FDA to be the safest plasticizer One of them, and was approved by the FDA as a green plasticizer, making it widely used in food packaging, beverage bottle stoppers, medical supplies, children's toys, personal hygiene products, and national defense projects. It is also an important chemical intermediate . [0003] Tributyl citrate is usually synthesized from citric acid and n-butanol under certain process conditions under the action of a catalyst. The traditional catalyst is mostly concentrated ...

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Application Information

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IPC IPC(8): C07C69/704C07C67/08
CPCY02P20/584C07C67/08C07C69/704
Inventor 李敢王德堂季剑波
Owner XUZHOU NAILI MACROMOLECULE TECH CO LTD
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