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Method for producing high-purity low-class fatty acid ester

A low-grade fatty acid ester, high-purity technology, applied in the field of preparation of low-grade fatty acid ester, can solve the problems of easy deactivation of catalysts, harsh raw material requirements, and low product purity

Active Publication Date: 2009-04-08
中石化湖南石油化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The purpose of the present invention is to overcome the disadvantages of low product purity, harsh requirements on raw materials, and easy deactivation of catalysts in the existing technology of synthesis of low-grade fatty acid esters by alkene addition, and provide a C 1 -C 5 Fatty carboxylic acid and C 2 -C 6 Method for generating high-purity low-grade fatty acid esters through highly selective addition reaction of olefins

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0032] This example is used to illustrate the adjustment effect of 0.5% water on the addition of butene and acetic acid to synthesize sec-butyl acetate. The catalyst used is silica-supported cesium phosphotungstate (Cs 2.5 h 0.5 PW 12 o 40 / SiO 2 ), the olefin raw material is mixed C 4 , The mass composition is: 38.5% isobutane, 9.4% n-butane, 20.1% trans-butene, 17.5% n-butene, 0.5% isobutene, 13.7% cis-butene, 0.3% butadiene. Acetic acid is industrial grade glacial acetic acid.

[0033] Add water to the glacial acetic acid to make the water content 0.5%. 20g Cs 2.5 h 0.5 PW 12 o 40 / SiO 2 The catalyst is loaded into the reactor. mix C 4 With 40g / h, acetic acid containing 0.5% water is continuously fed into the reaction system at a rate of 28g / h. The process conditions for controlling the reaction are: acid-ene molar ratio 1.2, reaction temperature 80°C, pressure 1.5MPa, for C 4 Feed weight space velocity 2.0h -1 , to react. After the reaction state is stable ...

example 2

[0039] This example is used to illustrate the adjustment effect of adding 1% sec-butanol to butene and acetic acid addition to synthesize sec-butyl acetate. The reaction conditions of this example are except adding 1% sec-butanol in the glacial acetic acid raw material, instead of 0.5% water in example 1, other conditions are completely the same as example 1.

[0040] After the system stabilized, the reactor effluent was analyzed on-line. Calculated according to the analysis results, the conversion rate of butene is 75.2%, the selectivity of converting butene into sec-butyl acetate is 99.3%, and the selectivity of converting into superimposed olefin is 0.7%. After running for 1000 hours, the olefin conversion rate was maintained above 72%. Collect the outlet product of the reactor, remove C4 by flash evaporation, separate acetic acid by azeotropic distillation, and then refine by rectification to finally obtain sec-butyl acetate product, which is carried out by the method spe...

example 3

[0042] This example is used to illustrate the regulating effect of adding 0.25% water and 0.5% sec-butyl alcohol mixture regulator to butene and acetic acid addition to synthesize sec-butyl acetate. The reaction conditions of this example are except adding 0.25% water and 0.5% sec-butanol in the glacial acetic acid raw material, instead of the 0.5% water in example 1, other conditions are exactly the same as example 1.

[0043] After the system stabilized, the reactor effluent was analyzed on-line. According to the analysis results, the conversion rate of olefins is 76.8%, the selectivity of butene into sec-butyl acetate is 99.1%, the selectivity of transforming into superimposed olefins is 0.7%, and the selectivity of transforming into sec-butanol is 0.2% %. After running for 1000 hours, the olefin conversion rate was maintained above 73%. Collect the outlet product of the reactor, remove C4 by flash evaporation, separate acetic acid by azeotropic distillation, and then ref...

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Abstract

The invention provides a method for preparing a high-purity lower fatty acid ester. The method is characterized in that proper amount of water or C1-C6 alcohol is adopted as a reaction conditioner; and C2-C6 olefin and C1-C5 organic carboxylic acid are introduced into a reaction system containing a strong acid catalyst so as to carry out an addition reaction to generate the lower fatty acid ester. The addition of the reaction conditioner of the water or the C1-C6 alcohol can accelerate the acid-olefin addition reaction, inhibit side reactions such as the olefin polymerization, and prevent the coking of diolefin on the surface of the catalyst, thereby generating the lower fatty acid ester through the high-selectivity addition of olefin and carboxylic acid, and greatly prolonging the service life of the catalyst.

Description

technical field [0001] The present invention relates to a kind of preparation method of lower fatty acid ester, relate to a kind of use water and alcoholic substance as reaction regulator, by C 1 -C 5 Carboxylic acid and C 2 -C 6 A method for highly selective synthesis of lower fatty acid esters from olefins under the action of a solid acidic catalyst. technical background [0002] Lower fatty acid esters are an important class of fine chemicals, which can be widely used as solvents for oils, resins, coatings, paints, reaction processes, extraction and separation processes, etc., as well as for the preparation of metal cleaning agents and spices. In recent years, due to increasingly stringent environmental protection requirements, the use of toxic solvents such as benzene, toluene, and chlorinated hydrocarbons is gradually being restricted, and the amount of environmentally friendly solvents such as esters is increasing sharply. Low-grade fatty acid ester products have be...

Claims

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Application Information

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IPC IPC(8): C07C67/04C07C69/02
Inventor 彭鸽威袁红星潘罗其
Owner 中石化湖南石油化工有限公司
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