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Unsaturated acid esterification method

A technology of esterification and unsaturation, applied in chemical instruments and methods, preparation of carboxylic acid esters, organic chemistry, etc., can solve the problems of large usage and unfavorable industrial production, and achieve short reaction time, low vapor pressure, and catalytic efficiency high effect

Inactive Publication Date: 2007-08-01
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But above-mentioned patents all only relate to the esterification of saturated acid and ester, all do not relate to the esterification of unsaturated acid; CN1405140 uses ionic liquid [Hmim] BF4 as catalyst and solvent, although also can be used for the esterification of crotonic acid and alcohol Esterification, but the amount of ionic liquid used is too large, almost reaching the reagent amount, and the use of fluorine-containing ionic liquid will generate HF, which is not conducive to industrial production

Method used

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  • Unsaturated acid esterification method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Weigh respectively n-butanol 9.25g (0.125mol), acrylic acid 9.00g (0.125mol), ionic liquid N-methylpyrrolidone bisulfate 0.0025mol; ionic liquid, butanol, acrylic acid, water-carrying agent Add successively in the round-bottomed flask that has agitator, thermometer, water trap, reflux condenser, magnetically stir, and react 2 hours under reflux temperature; Gained crude product is carried out vacuum distillation, conversion rate is 87.8%, 100% selectivity. The ionic liquid is reused after simple dehydration.

Embodiment 2

[0023] Embodiment two: take by weighing ethanol 5.75g (0.125mol), methacrylic acid 10.50g (0.125mol), ionic liquid N-methylpyrrolidone sulfate 0.0005mol; Add successively in the round-bottomed flask that has agitator, thermometer, water trap, reflux condenser, magnetically stir, and react at reflux temperature for 0.5 hour; Gained thick product is carried out vacuum distillation, conversion rate is 78.5%, 100% selectivity. The ionic liquid is reused after simple dehydration.

Embodiment 3

[0024] Embodiment three: take by weighing ethanol 5.75g (0.125mol), cinnamic acid 18.50g (0.125mol), ionic liquid N-methylpyrrolidone bisulfate 0.00125mol; Add in a round bottom flask with a stirrer, thermometer, water separator, reflux condenser, magnetically stir, and react at reflux temperature for 2 hours; cooling, static, liquid separation, water washing, alkali washing, the yield is 89.2% , selectivity 100%. The ionic liquid is reused after simple dehydration.

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Abstract

The invention discloses an esterifying method of unsaturated acid ester, which comprises the following steps: adopting 0.01%-50% ionic liquid A+B- as catalyst and solvent; stirring; heating; stewing; laminating; separating; or distilling directly to obtain the ester; making the ionic liquid as catalyst of alcohol and insaturated phased ester, inhibitor and reacting accelerator without polluting.

Description

technical field [0001] The invention belongs to an organic chemical reaction method, in particular to a clean method for carrying out unsaturated esterification in an ionic liquid. technical background [0002] Unsaturated ester compounds, especially acrylate compounds, have a wide range of industrial applications and are extremely important monomers for polymer synthesis. Traditional unsaturated esterification reactions usually use strong corrosive protonic acids such as concentrated sulfuric acid as catalysts , there are problems such as waste acid polluting the environment, difficult to separate products from catalysts, colored products and corroding equipment. Obviously, the society has an urgent demand for new alkyd esterification methods that are environmentally friendly and economically beneficial. Ionic liquids are new materials that have attracted much attention in recent years. They have the advantages of good stability, non-volatility, solubility and adjustable a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54B01J31/02
CPCY02P20/54
Inventor 方岩雄周蓓蕾陈晓刚黄宝华张焜
Owner GUANGDONG UNIV OF TECH