Integrated process for catalytically synthesizing acetyl tributyl citrate by sodium bisulfate monohydrate

Abstract

The invention discloses a method for synthesizing acetyl tributyl citrate by taking sodium bisulfate monohydrate as a catalyst. The method comprises the following steps of: step (1), adding citric acid (hydrate), n-butyl alcohol and catalyst sodium bisulfate monohydrate into a reactor and reacting at a temperature in a range of 130-160 DEG C for 3.0-6.0 hours; carrying out dealcholization to obtain crude TBC tributyl citrate; step (2) adding acetic anhydride and active carbon into the prepared TBC of the step (1) and reacting at a temperature in a range of 70-80 DEG C for 0.5-1.5 hours; cooling and filtering the catalyst and active carbon; adding water into the filtering solution to recycle acetic acid and treating to obtain the finished product of ATBC acetyl tributyl citrate. In integrated process for synthesizing the ATBC provided by the invention, the TBC is not separated from the catalyst and then is directly acylated after the process of dealcholization, and the processes of acetylation and decoloration are simultaneously carried out; the method provided by the invention has the advantages of simple process, short production cycle and less 'three wastes'; the processes of esterification and acetylation utilize the same catalyst, the catalyst is cheap and easy to obtain, and the catalyst is easy to separate and recycle; the quality of the product is good and the cost is low, so that the method is suitable for the industrial application.

Description

technical field [0001] The present invention relates to a synthetic method of plasticizer acetyl tributyl citrate (ATBC), in particular to an integrated synthetic process for synthesizing acetyl tributyl citrate with sodium bisulfate monohydrate as a catalyst, which belongs to chemical synthesis and technology fields. Background technique [0002] Traditional plasticizers, phthalates, may cause cancer, and foreign countries have legislated to restrict their use. Acetyl tributyl citrate (ATBC), as a "green" environmental plasticizer, has been approved by the US Food and Drug Administration (FDA). With the advantages of water resistance and low volatility, it is widely used in food packaging, medical products, children's toys and other fields, and has become the first choice to replace phthalate plasticizers. [0003] At present, there is a huge vacancy in the ATBC domestic market. The traditional method of ATBC synthesis uses concentrated sulfuric acid as a catalyst. The di...

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Problems solved by technology

[0007] The object of the present invention is to provide a kind of integrated synthetic technique that takes sodium bisulfate monohydrate as catalyzer to synthesize acetyl tributyl citrate, and this catalyzer is easy to separate and reclaim, and reaction condition is milder than the concentrated sulfuric acid, and product index is better than the concentrated sulfuric acid; Simultaneously In the integrated process for the synthesis of acetyl tributyl citrate of the present invention, TBC does not separate the catalyst, and directly acylates after dealcoholization, which overcomes the complex process and long production cycle in the preparation method of acetyl tributyl citrate in the prior art. , large product loss, many "three wastes", environmental pollution and other shortcomings

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