Method for utilizing molecular sieve supported catalyst to prepare acetic ether

A technology of immobilized catalysts and ethyl acetate, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of non-targeted product uses, low purity of ethyl acetate products, and incomplete product reactions and other problems, to achieve the effects of large void ratio and specific surface area, reduced pressure, and improved mass and heat transfer efficiency

Inactive Publication Date: 2016-07-13
GUANGXI XINTIANDE ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to overcome the strong corrosiveness brought by the existing catalyst, serious environmental pollution, complicated preparation process, non-targeted product use, and the current production method of ethyl acetate product to obtain low product conversion rate and low product reaction. Incomplete, the purity of the obtained ethyl acetate product is not high, etc., providing a simple and easy-to-implement method for preparing ethyl acetate using a molecular sieve immobilized catalyst. The immobilized catalyst uses molecular sieve as a carrier and heteropolyacid as a catalytic active layer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation process of the molecular sieve immobilized catalyst used in the present invention is as follows: dissolve 2 mol of water glass and 0.01 mol of aluminum sulfate in 250 mol of deionized water, stir vigorously for 10 minutes to fully dissolve it, add 0.4 mol of n-butylamine, and stir for 20 minutes , use sulfuric acid to adjust the pH of the solution to 10, then add lanthanum nitrate with a mass fraction of 2%, put the resulting mixed solution into an oven and evaporate it at 100°C for 5 hours to obtain a concentrated gel substance, seal the concentrated gel substance, and crystallize the kettle at 150°C After internal crystallization for 10 hours, the samples were filtered, washed and dried, and then calcined at 550°C for 5 hours. Take 5g of dodecaphosphotungstic acid, put it into 400g of water and stir to dissolve it completely, then add 40g of carrier, stir for 1-2 hours, soak for 24 hours, then dry the water, activate at 250°C for 3.5h, so as to obtain s...

Embodiment 2

[0025] The preparation process of the molecular sieve immobilized catalyst used in the present invention is as follows: 3 mol of water glass and 0.03 mol of sodium metaaluminate are dissolved in 250 mol of deionized water, vigorously stirred for 10 min to fully dissolve it, and 0.6 mol of ethylenediamine is added, Stir for 30 minutes, adjust the pH of the solution to 11 with sulfuric acid, then add lanthanum nitrate with a mass fraction of 2%, put the resulting mixed solution in an oven and evaporate at 100°C for 5 hours to obtain a concentrated gel substance, seal the concentrated gel substance, and crystallize at 150°C Crystallize in the kettle for 10h, filter, wash and dry the sample, and roast at 600°C for 6h. Take 5g of dodecaphosphotungstic acid and put it into 500g of water and stir to dissolve it completely, then add 50g of carrier, stir for 1 hour, impregnate for 24 hours, then dry the water, activate at 200°C for 4 hours, so as to prepare the immobilized catalyst MCM ...

Embodiment 3

[0029]The preparation process of the molecular sieve immobilized catalyst used in the present invention is as follows: 4 mol of water glass and 0.05 mol of sodium metaaluminate are dissolved in 250 mol of deionized water, vigorously stirred for 20 minutes to fully dissolve, and 0.6 mol of n-butylamine and Ethylenediamine (mole number 1:1), stirred for 30 minutes, adjusted the pH of the solution to 11 with sulfuric acid, then added lanthanum nitrate with a mass fraction of 2%, put the resulting mixed solution into an oven and evaporated at 100°C for 5 hours to obtain a concentrated gel substance. Seal the concentrated gel substance, crystallize in a crystallization kettle at 150°C for 10h, filter, wash and dry the sample, and bake at 600°C for 6h. Take 5g of dodecaphosphotungstic acid and put it into 600g of water and stir to dissolve it completely, then add 60g of carrier, stir for 1 hour, impregnate for 24 hours, then dry the water and activate at 200°C for 3 hours to prepare ...

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Abstract

The invention belongs to the field of chemical synthesis processes and particularly relates to a method for utilizing a molecular sieve supported catalyst to prepare acetic ether.Ethanol, acetic acid and water are vaporized according to the volume ratio of 3-8 L to 2-3 L to 3 L, then a vaporization product is led into an esterification reaction kettle, the molecular sieve supported catalyst accounting for 5-30% of the total volume percentage of a reaction system is added, reaction is performed at the temperature of 110-115 DEG C for 15-30 minutes, condensation is performed, and the acetic ether is obtained through distillation recovery.The method utilizes the catalytic action of the molecular sieve supported catalyst to prepare the acetic ether, the acetic acid conversion rate is up to 98% or above, the acetic ether yield is 99.5% or above, an obtained esterification product is high in purity, the molecular sieve supported catalyst can be repeatedly used for 6-8 times, and the production costs are greatly reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis technology, and specifically relates to a method for preparing ethyl acetate by using a molecular sieve immobilized catalyst. The immobilized catalyst uses molecular sieve as a carrier and heteropolyacid as a catalytic active layer. Background technique [0002] Ethyl acetate is an excellent organic solvent, which has good solubility properties for ethyl cellulose, cellulose acetate butyrate, polystyrene, methacrylic resin, chlorinated rubber and various natural gums. [0003] In the traditional process, ethyl acetate is obtained by esterification of acetic acid and n-ethanol in the presence of sulfuric acid. Ethanol, acetic acid and sulfuric acid are put into the distillation pot according to the proportion, and the esterification is carried out at 120 degrees Celsius. After reflux dehydration, the time of esterification is controlled. The acid value of the crude ester is below 0.5, and the obta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/14B01J29/48B01J29/78
CPCB01J29/48B01J29/7876B01J2229/186C07C67/08C07C69/14Y02P20/50
Inventor 徐大鹏冯英
Owner GUANGXI XINTIANDE ENERGY
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