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Method for preparing butyl acetate by using molecular sieve immobilized catalyst

A technology of immobilized catalyst and butyl acetate, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of organic compounds. and other issues, to achieve the effect of increasing anti-virus performance, prolonging life, and increasing geometric surface area

Active Publication Date: 2019-02-19
GUANGXI XINTIANDE ENERGY +2
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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, tedious preparation process, non-targeted product use, and the current production method of butyl acetate product to obtain low product conversion rate and low product reaction. Incomplete, the purity of the obtained butyl acetate product is not high, and a simple and easy-to-implement method for preparing butyl acetate using a molecular sieve immobilized catalyst is provided. 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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PUM

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Abstract

The invention belongs to the field of chemical synthesis processes, and particularly relates to a method for preparing n-butyl acetate from a molecular sieve immobilized catalyst. Butanol, acetic acid and water are added to an esterification reaction still according to the proportion of (2-5 L):1L:3L, the molecular sieve immobilized catalyst accounting for 5% to 30% of the total proportion of the volume of the reaction system is added, reacting is carried out for 15 min to 30 min at the temperature of 80 DEG C to 115 DEG C, then condensation is carried out, and n-butyl acetate is obtained through rectification and recovery. N-butyl acetate is prepared through the catalytic action of the molecular sieve immobilized catalyst, the acetic acid conversion rate reaches 98% or above, the yield of n-butyl acetate is 99.5% or above, and the obtained esterification product is high in purity; the molecular sieve immobilized catalyst can be reused 6-8 times, so that the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis technology, and in particular relates to a method for preparing butyl 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] Butyl acetate is an excellent organic solvent, and it has good solubility properties for ethyl cellulose, cellulose acetate butyrate, polystyrene, methacrylic resin, chlorinated rubber and various natural gums. [0003] In the traditional process, butyl acetate is obtained by esterification of acetic acid and n-butanol in the presence of sulfuric acid. Butanol, acetic acid and sulfuric acid are put into the distillation pot in proportion, and esterified at 120 degrees Celsius. After reflux dehydration, the esterification is controlled. The acid value at the time of melting is below 0.5, and the obtained crude ester is neutralized and put...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/08B01J31/16B01J31/18B01J27/188
CPCB01J27/188B01J29/48B01J29/7876B01J2229/18C07C67/08C07C69/14Y02P20/50
Inventor 徐大鹏冯英
Owner GUANGXI XINTIANDE ENERGY
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