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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 required in the reaction process. And the conversion rate of the esterification reaction is not high
However, the amount of ionic liquid used in this method is large, the post-treatment time of the catalyst is long, and the energy consumption required to remove the catalyst moisture is relatively large.

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
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Effect test

example 1

[0023] (1) Preparation of ionic liquid

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

[0025] (2) carry out esterification reaction

[0026] 0.015molFeCl 3 With 0.06mol ionic liquid [Hmim] + BF 4 - After mixing evenly, put it into a 500mL three-necked bottle together with 1mol acetic acid and 1mol n-propanol, install a water separator and a temperature sensor, install a reflux condenser on the water separator, and heat until the reactant boils while stirring to start the reaction (reaction temperature 92~105℃). The azeotrope formed during the reaction is distilled from the three-necked flask, conde...

example 2

[0028] Carry out esterification reaction by the method for example 1, difference is (2) step with 0.015molSnCl 4 instead of FeCl 3 With 0.06mol ionic liquid [Hmim] + BF 4 - Mix to make a catalyst, and the results of the esterification reaction are shown in Table 1.

example 3

[0030] Carry out esterification reaction by the method for example 1, difference is (2) in the step with 0.015molFeCl 3 With 0.06mol ionic liquid [Hmim] + BF 4 - After mixing evenly, put 60.0g (1mol) of acetic acid, 130.0g (1mol) of n-octanol and 92.0g (1mol) of toluene into the reaction bottle for esterification reaction. After almost no water is separated from the reflux, use vacuum distillation The method separates toluene, esterification product n-octyl acetate and unreacted raw materials from the catalyst, and 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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