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

A technology of ethylene glycol monoethyl ether and tributyl citrate, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of difficult separation and recovery of catalysts, equipment corrosion, and many side reactions, etc. problems, to achieve the effect of shortening the process flow and production cycle, less usage, and no environmental pollution

Inactive Publication Date: 2009-09-02
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 1g of zirconium sulfate tetrahydrate, dissolve it in water, add 9g of pretreated activated carbon (see "Summary of the Invention" for the pretreatment method) into the solution, stir at room temperature for 24 hours, heat at 80°C to evaporate the water, and wet The sample was dried at 80°C for 3-5 hours to obtain a supported zirconium sulfate catalyst.

[0034] Reaction material composition:

[0035] Acetic acid 15.6g

[0036] Ethylene glycol monoethyl ether 18g

[0037] Toluene 5g

[0038] Catalyst 0.9g

[0039] Add the above materials into the esterification reactor, heat to 120°C, and react at this temperature for 4 hours, then filter the reaction liquid, recover the catalyst, and rectify the filtrate to obtain the product ethylene glycol monoethyl ether acetic acid ester. The conversion rate of ethylene glycol monoethyl ether is 94.2%, and the selectivity of the target product is 100%.

[0040] The above-mentioned supported zirconium sulfate catalyst is ...

Embodiment 2

[0045]Basically the same as Example 1, but with the following changes: the amount of zirconium sulfate tetrahydrate and activated carbon in the catalyst preparation were 2g and 8g respectively. The conversion rate of ethylene glycol monoethyl ether was 94.9%, and the selectivity of the target product was 100%.

[0046] In the synthetic process step of ethylene glycol monoethyl ether acetate, the mass ratio of ethylene glycol monoethyl ether and acetic acid is 1:1.13 (mol ratio is 1:1.7), and the mass ratio of ethylene glycol monoethyl ether and catalyst is 1: 0.05.

Embodiment 3

[0048] Basically the same as Example 1, but with the following changes: the amount of zirconium sulfate tetrahydrate and activated carbon in the preparation of the catalyst were 3g and 7g respectively. The conversion rate of ethylene glycol monoethyl ether was 95.7%, and the selectivity of the target product was 100%.

[0049] Synthetic process for tributyl citrate:

[0050] Esterification reaction conditions: the mass ratio of citric acid to n-butanol is 1:1.76 (molar ratio is 1:5), and the catalyst is 3% of the total mass of reactants.

[0051] Reaction process:

[0052] Add the prepared catalyst and reaction materials into the esterification reactor at one time according to the above material ratio, heat to the reaction temperature of 110-140°C, and react for 4 hours. After the reaction, filter the mixture in the reactor, recover the catalyst, and react Liquid filtration, neutralize the filtrate with anhydrous sodium carbonate solution, then wash the organic layer with wa...

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PUM

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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, ...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07C67/08C07C69/16C07C69/12C07C69/704C08K5/11
CPCY02P20/584
Inventor 杨春傅鹏远
Owner NANJING NORMAL UNIVERSITY
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