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Catalytic alcohol acid esterifying method

A technology for catalyzing alkyd esters and catalysts, which is applied in chemical instruments and methods, preparation of carboxylate esters, catalysts for physical/chemical processes, etc. The problem is to achieve the effect of simple synthesis method, environmentally friendly catalytic process and low cost.

Active Publication Date: 2005-12-21
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN 1247856A reports the method of utilizing ionic liquids to catalyze esterification, but what this patent uses is ionic liquids composed of metal or non-metal halides. The ionic liquids composed of metal halides have poor stability and are easy to decompose when encountering water. It is reflected in the fact that there must be certain restrictions on the feeding method
Patent CN 1405140A has reported the use of ionic liquid [Hmim] + BF 4 The method of catalyzing esterification, but the report (Richard P.Swatloski, Greem Cheistry, 2003 (5): 361-363.) that the ionic liquid containing F is easy to decompose and generate HF when encountering water has proved that this type of ionic liquid does not have environmental friendliness property, and during the implementation of this patent, the amount of ionic liquid used is too large (essentially equal to the reactant), which is not suitable as a catalyst

Method used

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  • Catalytic alcohol acid esterifying method
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  • Catalytic alcohol acid esterifying method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: 0.02 moles of ionic liquid [P 666，14 LABS] and 0.25 moles of acetic acid and 0.25 moles of n-butanol were put into a reaction flask, stirred, heated, and reacted at a temperature of 100-130 ° C for 2 hours, the reaction was allowed to stand, and the esterification product n-butyl acetate was separated by liquid separation, The conversion was 94% and the selectivity was 99%. The ionic liquid in the lower layer is simply distilled to remove water and then recycled. [P 666，14 LABS] The name is: trihexyl(tetradecyl)phosphonium dodecylbenzenesulfonates The molecular formula is:

[0016]

Embodiment 2

[0017] Example 2: 0.04 moles of ionic liquid [P 666，14 LABS] and 0.25 moles of acetic acid and 0.25 moles of n-butanol were put into a reaction flask, stirred, heated, and reacted at a temperature of 100-130 ° C for 2 hours, the reaction was allowed to stand, and the esterification product n-butyl acetate was separated by liquid separation, The conversion was 97% and the selectivity was 99%. The ionic liquid in the lower layer is simply distilled to remove water and then recycled. [P 666，14 LABS] The name is: trihexyl(tetradecyl)phosphonium dodecylbenzenesulfonates The molecular formula is:

[0018]

Embodiment 3

[0019] Embodiment 3: put 0.04 moles of ionic liquid [BmimCl], 0.25 moles of acetic acid and 0.25 moles of n-butanol into a reaction flask, stir, heat, and react at a temperature of 100-130 °C for 2 hours, the reaction is allowed to stand, and the liquid separation is carried out. The esterification product n-butyl acetate was separated, the conversion rate was 96%, and the selectivity was 99%. The ionic liquid in the lower layer is simply distilled to remove water and then recycled. The molecular formula of [BmimCl] is:

[0020]

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PUM

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Abstract

The invention relates to a catalytic alkyd esterification method. It is characterized in that ionic liquid is used as catalyst, and the form of ionic liquid is: A + B - , where A is alkylpyridine or 1,3 alkylimidazole, and the chain length of the alkyl group is C 1 to C 15 , while B is chlorine, bromine, SO 4 - 、HSO 3 - ; or A is in the form shown in (1), abbreviated as: [PR 1 R 2 R 3 R 4 ] + , where R 1 R 2 R 3 R 4 is a branched or straight-chain alkyl group of any chain length, while B is in the form shown in (2), and R is a branched or straight-chain alkyl group of any chain length. ∴∴The main features of this method are that the ionic liquid used in the present invention is simple to synthesize, cheap, and the catalyzed esterification reaction has high conversion rate and high selectivity, and the process is simple, and the separation of the final product and the catalyst is simple and easy to recycle. High purity. The catalyst can be used repeatedly and is easy to realize industrialization.

Description

technical field [0001] The present invention relates to a kind of catalytic alcohol esterification method, it is characterized in that ionic liquid is used as catalyst, and the form of ionic liquid is: A + B - , where A is an alkyl pyridine or 1,3 alkyl imidazole, and the chain length of the alkyl group is C 1 to C 15 , while B is chlorine, bromine, SO4 - , HSO 3 - ; or A is in the form shown in (1), abbreviated as: [PR 1 R 2 R 3 R 4 ] + , where R 1 R 2 R 3 R 4 is a branched or straight-chain alkyl group of any chain length, while B is in the form shown in (2), and R is a branched or straight-chain alkyl group of any chain length. [0002] Background technique [0003] Esters can be used as spices, food additives, plasticizers, defoaming agents and good organic solvents, and are very important organic compounds. Most of the esterification methods in the background art are realized by using protonic acid, solid acid, ion ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07C67/08
Inventor 张锁江李春山张香平徐全清王蕾
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI