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Catalytic alcohol acid esterizing method

A technology for catalyzing alkyd esters and catalysts, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, catalysts for physical/chemical processes, etc., and can solve the problems of environmental friendliness, large usage of ionic liquids, poor stability of ionic liquids, etc. problem, to achieve the effect of stable properties, simple synthesis method and low cost

Active Publication Date: 2004-12-15
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • 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 esterizing method
  • Catalytic alcohol acid esterizing method
  • Catalytic alcohol acid esterizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment one: 0.02 mole ionic liquid [P 666，14 LABS] and 0.25 mole of acetic acid and 0.25 mole of n-butanol are put into a reaction flask, stirred, heated, and controlled at a temperature of 100-130° C. for 2 hours, the reaction is left standing, and the esterification product n-butyl acetate is 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] name is: trihexyl (tetradecyl) phosphonium dodecylbenzenesulfonates molecular formula is:

[0015]

Embodiment 2

[0016] Embodiment two: 0.04 mole ionic liquid [P 666，14 LABS] and 0.25 mole of acetic acid and 0.25 mole of n-butanol are put into a reaction flask, stirred, heated, and controlled at a temperature of 100-130° C. for 2 hours, the reaction is left standing, and the esterification product n-butyl acetate is 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] name is: trihexyl (tetradecyl) phosphonium dodecylbenzenesulfonates molecular formula is:

[0017]

Embodiment 3

[0018] Example 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 and heat, and control the temperature at 100-130°C for 2 hours, let the reaction stand, and pass liquid separation Separate the esterification product n-butyl acetate, the conversion rate is 96%, and the selectivity is 99%. The ionic liquid in the lower layer is simply distilled to remove water and then recycled. [BmimCl] molecular formula is:

[0019]

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Abstract

The catalytic alcohol acid esterizing process features that ionic liquid in the form of A+B- is used as catalyst, where A is alkyl pyridine, imidazole and other nitrous compound; and B is TA (CF3COO), HB (C3F7COO), TfO (CF3SO3), etc. and A may be in the form shown in expression (1) and B may be in the form shown in expression (2). The present invention features that the ionic liquid has simple synthesis process and low cost, and the catalytic esterizing reaction has high selectivity, simple process, simple separation of final product from the catalyst, easy recovering, high product purity, reuse of the catalyst and easy industrial application.

Description

technical field [0001] The invention relates to a method for catalytic alkyd esterification, which is characterized in that an ionic liquid is used as a catalyst, and the form of the ionic liquid is: A + B - , where A is a nitrogen-containing heterocyclic compound, including alkylpyridine or 1,3 alkylimidazole, and the chain length of the alkyl group is C 1 to C 15 ; B is a simple halogen element fluorine, chlorine, bromine or TA - (CF 3 COO - ), HB - (C 3 f 7 COO - ), TfO - (CF 3 SO 3 - ), NfO - (C 4 f 9 SO 3 - ), Tf 2 N - ((CF 3 SO 2 ) 2 N) - 、Beti - ((C 2 f 3 SO 2 ) 2 N - ), Tf 3 C - ((CF 3 SO 2 - ) 3 C - ), CB 11 h 12 - (and its substitutes), CH 3 COO - , NO 3 - , SO 4 - , NO 2 - 、HSO 3 - etc.; A can also be 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; meanwhile, B is in the form shown in (2), and R is a branc...

Claims

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Application Information

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Patent Type & Authority Applications(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
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