Supported zirconium sulfate catalyst, preparation method thereof and application thereof in synthesizing ethylene glycol monoethylether acetate or tributyl citrate

Abstract

The invention discloses a supported zirconium sulfate catalyst, a preparation method thereof and application thereof in synthesizing ethylene glycol monoethylether acetate or tributyl citrate. The catalyst comprises the following components in proportion by weight: 10 to 40 percent of zirconium sulfate tetrahydrate and 60 to 90 percent of carrier, wherein the carrier is mesoporous molecular sieve SBA-15 or active carbon. The preparation method comprises the following steps: (1) preparation of an active carbon carrier, wherein the active carbon is soaked by sodium hydroxide and hydrochloric acid respectively, the solution is filtered, the active carbon is placed into a nitric acid solution for reflux, the solution is filtered, and the active carbon is washed to neutrality and dried; (2) preparation of a mesoporous molecular sieve carrier, wherein a template agent is dissolved in dilute HCl, ethyl orthosilicate is added dropwise into the mixture, the mixture is stirred at a constant temperature, the mixture is subjected to ageing and filtering to obtain a solid, and the solid is baked to remove the template agent to obtain the mesoporous molecular sieve carrier; and (3) preparation of the catalyst, wherein the zirconium sulfate tetrahydrate is dissolved in water, the carrier is added into a water solution for stirring and impregnating, the mixture is heated to remove the water, and the mixture is dried to obtain the catalyst. The method overcomes the defects of difficult separation, incapacity of recycling the catalyst, long process flow, corrosion of equipment and environmental pollution of the conventional catalyst.

Description

technical field [0001] The present invention relates to a catalyst and its preparation method and application, in particular to a supported zirconium sulfate catalyst for synthesizing ethylene glycol monoethyl ether acetate or tributyl citrate, and the present invention also relates to the supported zirconium sulfate catalyst The preparation method, and the application of the supported zirconium sulfate catalyst in the synthesis process of ethylene glycol monoethyl ether acetate or tributyl citrate. Background technique [0002] Ethylene glycol monoethyl ether acetate (EGEEA), also known as 2-ethoxyethanol acetate and 2-ethoxyethyl acetate, is generally produced by esterification of acetic acid and ethylene glycol monoethyl ether. Ethylene glycol monoethyl ether acetate is a multifunctional excellent solvent with multifunctional groups. There are ether bonds, carbonyl groups, and alkyl groups in the solvent molecule, so it can dissolve organic molecules, polymer compounds, ...

AI Technical Summary

Problems solved by technology

[0004] The synthesis of ethylene glycol monoethyl ether acetate and tributyl citrate is a typical esterification reaction. At present, sulfuric acid is mostly used as a catalyst in industry. Although sulfuric acid has the advantages of high catalytic activity and short reaction time, it also has side effects. There are many reactions, the catalyst is not easy to separate and recover, the product needs to be neutralized by alkali, and can be purified by distillation after washing, and the problems of equipment corrosion and environmental pollution are serious. It is urgent to replace it with a new catalyst that is non-corrosive, pollution-free and easy to separate. Of