Preparation method of butylparaben

A technology of butylparaben and n-butanol, which is applied in the field of food additives to achieve the effects of good catalytic activity, excellent catalytic reaction performance and high selectivity

Inactive Publication Date: 2017-03-22
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the used ammonium ferric sulfate is discharged as waste, which also brings certain pressure to environmental protection.

Method used

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  • Preparation method of butylparaben

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Experimental program
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Effect test

Embodiment

[0020] (1) Catalyst preparation: wash, dry, and grind the ammonium ferric sulfate dodecahydrate used to catalyze the esterification reaction, put it in a crucible, put it into a muffle furnace and roast it at 550°C for 5 hours, and then place it to dry Cool to room temperature in a container, set aside;

[0021] (2) Add a certain amount of p-hydroxybenzoic acid, n-butanol, and the catalyst obtained in step (1) into a three-necked flask equipped with a stirrer, a water separator connected to the upper end of a reflux condenser, and a thermometer, wherein the amount of catalyst It is 5.3% of the total mass of p-hydroxybenzoic acid and n-butanol. The mass ratio of n-butanol and p-hydroxybenzoic acid is 3.5:1. Start stirring, heat to reflux, separate water, and react for 4 hours. After the reaction, separate the catalyst and water Recover n-butanol by steam distillation, pour the distilled residue into distilled water, adjust the pH to 7-8 with 10% sodium carbonate solution under ...

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Abstract

The invention belongs to the field of food additives and particularly relates to a preparation method of butylparaben. With the method, home-made solid super acid is used as a catalyst, p-hydroxybenzoic acid and n-butyl alcohol are used as reaction raw materials, and a product is obtained through an esterification reaction. The home-made catalyst is the solid super acid obtained by roasting ammonium ferric sulfate dodecahydrate. Ammonium ferric sulfate dodecahydrate is ammonium ferric sulfate dodecahydrate waste after catalysis of the esterification reaction. With the method, industrial waste is recycled, the discharge of the solid waste is reduced, and the method has the good environmental protection benefit; and meanwhile, the catalyst prepared with the method has the advantages of being good in catalytic activity, high in selectivity, capable of recycled repeatedly and the like.

Description

technical field [0001] The invention belongs to the field of food additives, in particular to a method for preparing butylparaben, in particular to a method for preparing butylparaben by reacting p-hydroxybenzoic acid and n-butanol under the action of a self-made solid superacid catalyst . Background technique [0002] Due to its high efficiency, broad spectrum, low toxicity, and easy compatibility, paraben is widely used in food, cosmetics, and pharmaceutical industries. It is one of the key development products in my country to replace food preservatives such as sodium benzoate. Among them, the antibacterial effect of butylparaben is due to ethyl and propyl esters, and the antiseptic effect is the best. Most domestic preparation technologies use concentrated sulfuric acid as a catalyst. Although this process has a high esterification rate, concentrated sulfuric acid is highly corrosive, requires high equipment, easily causes side reactions and produces a large amount of w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/84B01J27/053
CPCC07C67/08B01J27/053C07C69/84
Inventor 于龙张宁梁万根张超张永军闫敏敏王晓明张子汉
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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