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Method for synthesizing sec-butyl acetate from acetic acid and linear butylene

A technology of sec-butyl acetate and butene, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of side reaction waste liquid, increased energy consumption, difficult to handle, etc., and achieves easy Regeneration, good stability, and the effect of reducing production costs

Inactive Publication Date: 2008-02-13
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] The object of the present invention is to provide a kind of method that is practical by acetic acid and linear butene synthetic sec-butyl acetate in industrial production, and the solid catalyst that can be applicable to this method, overcomes the equipment corrosion that traditional method exists, side reaction And the problem that the reaction waste liquid is difficult to deal with; it also overcomes the problem of increased energy consumption caused by the difficulty of water separation in the traditional method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Put 2ml of modified resin catalyst into the above-mentioned reaction tube, adjust the reaction temperature to 125°C, pass nitrogen gas for 8 hours to activate the catalyst, turn on the micro-feed pump to make the acetic acid feed space velocity reach 1.0h -1 , After 15 minutes, the mixed butenes containing butene-154% were introduced. After the air was replaced under normal pressure, the pressure was gradually increased to 1.0 MPa. To promote the reaction, the tail butene flow rate was kept at 30 ml / min. After 5 hours, the reaction product was collected for one hour and analyzed by gas chromatography. After a period of time (6-8 hours) after the reaction, the reaction product could be sampled and analyzed. The product is analyzed by HP6580 gas chromatograph, and the conversion rate of acetic acid can reach 71%, and the selectivity of generating sec-butyl acetate is 98.1%.

Embodiment 2

[0044] According to the conditions described in Example 1, the life test of the modified resin catalyst was carried out. After 1000 hours of continuous operation, the catalyst activity dropped from 70% to about 56%. The selectivity to sec-butyl acetate was 98%.

Embodiment 3

[0046] Except that the reaction temperature was changed to 90°C and the feed rate of acetic acid was 0.1h -1 Outside, other is the same as embodiment 1, and the result is: the conversion rate of acetic acid can reach 78%, and the selectivity of isopropyl acetate is 98.2%.

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PUM

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Abstract

The invention relates to a synthetic method of the sec-butyl acetate with the acetic acid and linear butylene. The invention is characterized in that a fixed-bed reactor is used; the solid catalyst is used; when the butylenes pressure is between 2 and 15 kilograms per square centimeters and the reaction temperature is between 90 and 160 Celsius system, the acetic acid and olefin react and compose the sec-butyl acetate under the gas-liquid-solid reaction condition; therein, the ratio between the cetic acid and olefin is from 1 to 1.15 to 1 to 1.80; the material feeding airspeed of the acetic acid is 1.0 to 1.8 liters per hour; the solid catalyst is the modified resin catalyst, silica gel loading heteropoly acid catalyst, silica gel loading phosphoric acid catalyst or super acid catalyst. The invention overcomes the erosion of the equipment, the side reaction, the difficult treatment of the waste liquid of the reaction, and the difficult separation of water in the traditional process, which may cause the increase of the energy consumption; the invention can greatly lower the production cost of the product.

Description

technical field [0001] The invention relates to a method for synthesizing sec-butyl acetate from acetic acid and linear butenes (including butene-1 and butene-2) through direct addition esterification. Background technique [0002] Secondary butyl acetate is a colorless, flammable, fruity liquid, insoluble in water, miscible with ethanol and ether. It can be widely used in fruit flavor essence; it can be used as a solvent for nitrocellulose paint, acrylic paint, polyurethane paint, etc.; it can be used in the manufacture of celluloid products, coated paper, patent leather, etc.; it can be used as a volatile solvent in printing ink; It can be used as a quick-drying agent for photosensitive materials; it can be used as a drug absorption promoting component; as a reaction medium; it can be used as azeotropic distillation solvent component and partially replace the occasions where toluene, xylene and methyl isobutyl ketone were used as solvents in the past ; It can also be used...

Claims

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Application Information

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IPC IPC(8): C07C67/04C07C69/14
Inventor 廖世军宋慧宇刘仕文
Owner SOUTH CHINA UNIV OF TECH
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