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Method for synthesizing ethyl p-hydroxybenzoate through catalysis of modified metal oxide type solid super acid

A technology of ethyl hydroxybenzoate and p-hydroxybenzoic acid, which is applied in the field of catalytic synthesis of ethyl p-hydroxybenzoate by modified metal oxide solid superacids, and can solve the problems of lack of green synthesis technology of ethyl p-hydroxybenzoate , achieve the effect of maintaining high activity for repeated use, high economic and social benefits, and remarkable catalytic effect

Inactive Publication Date: 2015-02-04
YANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0006] At present, there is a lack of an environmentally friendly green synthetic process for ethyl p-hydroxybenzoate with industrial application prospects

Method used

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  • Method for synthesizing ethyl p-hydroxybenzoate through catalysis of modified metal oxide type solid super acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Preparation of modified metal oxide solid superacid:

[0018] ZrOCl 2 ·8H 2 O is dissolved in deionized water to prepare a solution with a certain concentration. First, add quantitatively calculated boric acid, stir and dissolve, then add a certain proportion of ammonium metatungstate, stir and dissolve, and mix the prepared solution with 6mol / l ammonia water gradually under stirring conditions. Add dropwise to a certain amount of ammonia solution with pH=9, control the pH value of the whole dropping process to be constant at 9, continue to stir for a certain period of time after the dropwise addition, leave it to age at room temperature, filter and wash with deionized water until it cannot be detected Cl - ion, dried at 120°C for 12h, and then roasted at 700°C for 3h in an atmosphere-protected box furnace to obtain a modified metal oxide solid superacid WO 3 / B 2 o 3 -ZrO 2 ,stand-by.

[0019] Synthesis of ethyl p-hydroxybenzoate:

[0020] Add 3.45g p-hydroxybe...

Embodiment 2

[0025] The difference between embodiment 2 and embodiment 1 is: add 3.45g p-hydroxybenzoic acid, 10.5ml dehydrated alcohol and 0.58g modified metal oxide type solid superacid WO in the reaction vessel 3 / B 2 o 3 -ZrO 2 , heating to raise the temperature, and carry out the esterification reaction under the condition of reflux temperature. After the reaction, the solid superacid catalyst was separated and recovered by filtration, and the excess ethanol was removed from the filtrate by rotary evaporation to obtain the product ethyl p-hydroxybenzoate with a yield of 91.8%.

[0026] The recovered solid superacid catalyst can be recycled after being regenerated and vacuum-dried.

Embodiment 3

[0028] The difference between embodiment 3 and embodiment 1 is: add 3.45g p-hydroxybenzoic acid, 12.0ml dehydrated alcohol and 0.49g modified metal oxide type solid superacid WO in the reaction vessel 3 / B 2 o 3 -ZrO 2 , heating to raise the temperature, and carry out the esterification reaction under the condition of reflux temperature. After the reaction, the solid superacid catalyst was separated and recovered by filtration, and excess ethanol was removed from the filtrate by rotary evaporation to obtain the product ethyl p-hydroxybenzoate with a yield of 91.0%.

[0029] The recovered solid superacid catalyst can be recycled after being regenerated and vacuum-dried.

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Abstract

The present invention discloses a method for synthesizing ethyl p-hydroxybenzoate through catalysis of a modified metal oxide type solid super acid. The method comprises: (1) adopting a modified metal oxide type solid super acid as a catalyst, heating p-hydroxybenzoic acid and excess ethanol, carrying out an esterification reaction at a reflux temperature of 75-85 DEG C, and co-boiling part of the ethanol and the water produced by the reaction so as to take away the ethanol; and (2) after reacting for 3-4 h, filtering to separate and recover the solid super acid catalyst, wherein the filtrate presents the yellow oil state; and carrying out rotary evaporation to remove the excess ethanol to obtain the ethyl p-hydroxybenzoate. According to the present invention, the modified metal oxide type solid super acid is adopted as the catalyst for the ethyl p-hydroxybenzoate synthesis reaction, such that the catalysis effect is significant, the environment protection effect is provided, the solid super acid is easily recovered and regenerated, can maintain the high activity and can be reused.

Description

technical field [0001] The invention relates to a chemical synthesis process, in particular to a method for catalytically synthesizing ethyl p-hydroxybenzoate with a modified metal oxide type solid superacid. Background technique [0002] Parabens, namely parabens, are usually esters formed from p-hydroxybenzoic acid and C1-C7 lower fatty alcohols. It is a safe, efficient and broad-spectrum preservative currently used internationally. As an intermediate of organic synthesis, it is widely used in food, cosmetics and pharmaceutical industries due to its advantages of low toxicity, non-irritation and wide pH range. One of the products of the agent. In addition, paraben ester is also an intermediate of new ester organic liquid crystals and a dye intermediate in thermal recording materials. Therefore, the research and development of such products has broad prospects. [0003] In recent years, the research on the synthetic method of parabens at home and abroad is quite active, m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/08
CPCC07C67/08C07C69/84
Inventor 张存杜蒙吴过高维丹张骏超赵永庚孙晶芸
Owner YANGZHOU UNIV
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