Integrated process for synthesizing acetyl tributyl citrate (ATBC) from active carbon solid-carried sulphuric acid catalyst

Abstract

The invention relates to an integrated process for synthesizing acetyl tributyl citrate (ATBC) from an active carbon solid-carried sulphuric acid catalyst. The integrated process comprises the following steps of: (1) preparing the catalyst: immersing wooden active carbon in a 5-20 times of sulphuric acid solution, stirring and solid-carrying at normal temperature, and obtaining the active carbon solid-carried sulphuric acid catalyst after filtering and drying; (2) preparing TBC (Tributyl Citrate): reacting (hydrate) citric acid, n-butyl alcohol and the catalyst at 130-160 DEG C for 3.0-6.0 h, and dealcoholizing; and (3) preparing the ATBC: adding acetic anhydride into the TBC, reacting at 70-90 DEG C for 0.5-1.5 h, filtering a reaction solution after cooling, adding water, recycling acetic acid, and post-processing to obtain the ATBC finished product. According to the method disclosed by the invention, the catalyst is low in use amount and easy for being separated and recycled and also has decolourization function; after being dealcoholized, the TBC is unnecessary to be separated and the acylation reaction is directly carried out; the steps of refining the TBC, decolourizing and the like are saved; the three wastes (waste gas, waste water and industrial residue) are reduced obviously; the cost is reduced; the product yield is increased; and the integrated process is applied to industrial application.

Description

technical field [0001] The invention relates to a method for synthesizing plasticizer acetyl tributyl citrate (ATBC), in particular to an integrated synthesis process for synthesizing acetyl tributyl citrate with an activated carbon immobilized sulfuric acid catalyst, which belongs to the field of chemical synthesis and technology . 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 gap in the ATBC domestic market. The traditional method of ATBC synthesis is a homogeneous system using concentrated...

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to propose an integrated process for the synthesis of acetyl tributyl citrate under the catalysis of a solid acid, which overcomes the complex process, long production cycle and product loss in the existing preparation method of acetyl tributyl citrate Large, many "three wastes", environmental pollution and other shortcomings, the method TBC of the present invention does not undergo separation and water washing, and directly carries out acylation reaction after dealcoholization, the catalyst is simple to prepare, easy to separate and recycle, the reaction conditions are mild, and the product quality is good