Esterification catalysts and esterification process of organic acid

An esterification catalyst and catalyst technology, applied in physical/chemical process catalysts, organic chemistry, chemical instruments and methods, etc., can solve the problems of large amount of ionic liquid, large amount of organic solvents, high energy consumption, etc., to simplify the esterification reaction Process, high yield of esterified product, effect of prolonging service life

Active Publication Date: 2008-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2002, J.Fraga Dubreuil et al. reported on "Catalysis Communications" the method of using ionic liquids to catalyze the esterification of organic acids and alcohols. The synthesis steps of ionic liquids used in this method are complicated, and a large amount of organic solvents are still require

Method used

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  • Esterification catalysts and esterification process of organic acid
  • Esterification catalysts and esterification process of organic acid

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0022] Example 1

[0023] (1) Preparation of ionic liquid

[0024]Put 1 mol of 1-methylimidazole into a three-necked round bottom flask, add tetrafluoroboric acid (concentration of 40wt%) while stirring at an equimolar ratio, and control the reaction temperature not to be higher than 40°C, and continue to stir for 1 hour to prepare light Yellow liquid. Remove excess water by distillation under reduced pressure at 70°C to obtain ionic liquid 1-methylimidazole tetrafluoroborate [Hmim] + BF 4 - .

[0025] (2) Carry out esterification reaction

[0026] 0.015molFeCl 3 With 0.06mol ionic liquid [Hmim] + BF 4 - After mixing uniformly, put 1mol acetic acid and 1mol n-propanol into a 500mL three-necked flask, install a water separator and a temperature sensor, and install a reflux condenser on the water separator. Heat until the reactants boil and start the reaction (reaction temperature). 92~105℃). The azeotrope formed during the reaction is distilled out from the three-necked flask, co...

Example Embodiment

[0027] Example 2

[0028] The esterification reaction was carried out according to the method of Example 1, except that 0.015mol SnCl was used in step (2) 4 Instead of FeCl 3 With 0.06mol ionic liquid [Hmim] + BF 4 - The mixture is made into a catalyst, and the results of the esterification reaction are shown in Table 1.

Example Embodiment

[0029] Example 3

[0030] The esterification reaction was carried out according to the method of Example 1, except that in step (2), 0.015molFeCl 3 With 0.06mol ionic liquid [Hmim] + BF 4 - After mixing uniformly, put 60.0g (1mol) acetic acid, 130.0g (1mol) n-octanol and 92.0g (1mol) toluene into the reaction flask for esterification reaction. After almost no water in the refluxed material, use vacuum distillation Toluene, esterification product n-octyl acetate and unreacted raw materials were separated from the catalyst by the method. The results of the esterification reaction are shown in Table 1.

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Abstract

The invention relates to esterification catalyst, which is inorganic compound including ionic liquid and inorganic compound with Lewis acid. The cation of the ionic liquid is imidazole or pyridine taken place by C1C15 alkyl, wherein, the substituting group number is one or more, and the anion is BF4<-> or PF6<->; the inorganic compound with Lewis acid is selected from FeCl3, SnCl4, ZnCl2 or Zn (NO32) and so on, and the mol ratio of the inorganic compound with Lewis acid and the ionic liquid is 0.01 to 1.0:1. The catalyst is used for esterification reaction, the selectivity is good, the yield rate of the esterified ester is high, and the service life is long.

Description

technical field [0001] The invention relates to an organic esterification catalyst and an esterification method, in particular to an esterification catalyst containing an ionic liquid and a method for esterifying organic acids using the catalyst. Background technique [0002] The main uses of organic acid esters are fragrances, flavors, plasticizers, solvents and intermediates in organic synthesis. Low-level esters have an aromatic smell and are commonly used spices; paraben esters (paraben esters) are a class of low-toxicity, non-irritating, and can be used in industries such as food, cosmetics, and medicine in a wide pH range. Preservatives; Dioctyl phthalate (DOP) is an excellent plasticizer and occupies a very important position in the plastics industry; Tri-n-butyl citrate (TBC) is a non-toxic, odorless, weather-resistant One of the excellent plasticizer varieties. [0003] The traditional ester synthesis process mostly uses inorganic acids such as concentrated sulfur...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J31/26C07C67/08C07C69/02
Inventor 葸雷董忠杰王建伟谢红霞果卉
Owner CHINA PETROLEUM & CHEM CORP
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