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Composite catalyst for preparing sec-butyl acetate with direct esterification of ethyl ester and butylene

A composite catalyst, sec-butyl acetate technology, applied in physical/chemical process catalysts, catalyst carriers, carboxylate preparation and other directions, can solve problems such as reduced catalytic efficiency

Inactive Publication Date: 2008-10-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of this invention is to provide a kind of composite catalyst for producing sec-butyl acetate, to solve the problem that heteropolyacid is separated out from reaction system and cause the problem that catalytic efficiency reduces

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 30g of 98% industrial acetic acid, 30g of 1-butene (98% content), 0.6g of phosphotungstic acid, and 1.2g of SBA-15 were loaded into a 100ml autoclave, and reacted at 120°C for 2 hours. After the reaction, the autoclave was cooled to room temperature and vented. The liquid phase material was analyzed by gas chromatography. The conversion rate of acetic acid is 78.5%, the selectivity of sec-butyl acetate is 98.6%, and the others are butene dimers.

Embodiment 2

[0019] No carrier is added in Example 2, and the carriers of 3 to 5 are respectively white carbon black, kaolin, porous amorphous Al 2 o 3 , others are identical with embodiment 1. The results are shown in Table 1.

[0020] Table 1:

[0021] Example

[0022] After the reaction, a brown-black viscous liquid was precipitated from the solution of Example 2, adhering to the inner wall of the reactor and the stirring bar. The viscous liquid was soluble in water and acetic acid, and it was a heteropolyacid according to XRD analysis. However, the viscous liquid did not appear in Examples 3-5, indicating that the precipitated heteropolyacid was adsorbed on the porous carrier.

Embodiment 6-10

[0024] Reaction operation is identical with embodiment 1. The reaction time is 0, 0.5, 1, 1.5 and 2 hours respectively. After the reaction is over, the reaction solution is clarified, and the SBA-15 adsorbed with the heteropoly acid is filtered out. The mass of residual heteropolyacid in the liquid phase. The results are shown in Table 2.

[0025] Table 2:

[0026] Example

[0027] As can be seen from the results of Examples 6-10, when there is no reaction (Example 6), the heteropolyacid is basically dissolved in the liquid phase, and as the reaction proceeds, the heteropolyacid separated out gradually increases and is adsorbed on the carrier, The reaction gradually changed from homogeneous to heterogeneous.

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Abstract

The present invention relates to a composite catalyst for preparing sec-butyl acetate by direct esterification of ethyl ester and butylene, which takes heteropoly acid as the catalyst active component and porous carrier as the dispersant; the weight proportion of the heteropoly acid and the porous carrier is 0.01:1 to 10:1. The heteropoly acid is one with Keggin structure, which consists of phosphotungstic acid, silicotungstic acid, germanium tungstic acid, arsenowolframic acid, phosphomolybdate, germanomolybdate or arsenicomolybdate. The porous carrier comprises porous SiO2, Al2O3, SBA-15, MCM-41, white carbon black, porous SiC, corallite, andalusite, cordierite, meerschaum, Attapulgite or kaolin. The composite catalyst of the present invention solves the problem that the catalysis efficiency is low if the heteropoly acid is separated out from the reaction system.

Description

technical field [0001] The invention relates to a composite catalyst for preparing sec-butyl acetate, in particular to a composite catalyst for preparing sec-butyl acetate by direct reaction of acetic acid and butene. [0002] The present invention also relates to the application of the catalyst in the direct esterification of ethyl ester and butene to prepare sec-butyl acetate. Background technique [0003] Butyl acetate is a good organic solvent, which is widely used in nitrocellulose, paint, artificial leather, medicine, ink and plastic industries. The traditional method of producing butyl acetate both at home and abroad is to adopt a batch-type tank reaction, and use sulfuric acid as a catalyst to catalyze the esterification reaction of acetic acid and butanol. Chinese patent CN1844076A reports a method for large-scale production of butyl acetate using sulfuric acid as a catalyst reactive distillation method. This method uses sulfuric acid as a catalyst, which will inev...

Claims

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Application Information

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IPC IPC(8): B01J27/188B01J32/00C07C67/08C07C69/14
Inventor 王华张今令谢文勇刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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