Preparation method of butyl p-hydroxybenzoate

A technology of butyl hydroxybenzoate and p-hydroxybenzoic acid, which is applied in the field of preparation of butyl p-hydroxybenzoate, can solve problems such as equipment corrosion, dark product color, troublesome operation, etc., and achieve the effect of no corrosive damage

Inactive Publication Date: 2010-07-28
李松伦
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, its synthesis method usually uses p-hydroxybenzoic acid and n-butanol, and is directly prepared under the action of concentrated sulfuric acid, but this method has problems such as serious equipment corrosion and easy dehydration side reactions.
In recent years, it has been reported to use heteropolyacids, super solid acids, etc. as catalysts. Although the effect is good, the price is rel...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Catalyst preparation:

[0014] First, wash the 4A zeolite with distilled water and activate it at 120°C for 2 hours. After cooling, weigh 20g of zeolite and soak it in 100ml of p-toluenesulfonic acid solution with a mass fraction of 20% for 24 hours. Dry for 4 hours, put into a desiccator and cool to obtain a solid catalyst;

[0015] Preparation of butyl p-hydroxybenzoate:

[0016] Add 100g of p-hydroxybenzoic acid, 100g of butanol, 100ml of toluene, 1g of benzyltriethylamine chloride and 8g of solid catalyst into the flask, and react under reflux for 4 hours while removing water. After the reaction, remove the catalyst by filtration, steam the unreacted butanol and toluene, add the residue into cold water and stir vigorously, and white crystals will precipitate out, then neutralize the unreacted acid with 5% sodium carbonate solution until the solution is weakly alkaline, suction filtered, and dried to obtain 134 g of the product butyl p-hydroxybenzoate, with a yield...

Embodiment 2

[0018] Catalyst preparation:

[0019] First, wash the 4A zeolite with distilled water and activate it at 120°C for 2 hours. After cooling, weigh 20g of zeolite and soak it in 100ml of p-toluenesulfonic acid solution with a mass fraction of 20% for 24 hours. Dry for 4 hours, put into a desiccator and cool to obtain a solid catalyst;

[0020] Preparation of butyl p-hydroxybenzoate:

[0021] Add 100 g of p-hydroxybenzoic acid, 150 g of butanol, 100 ml of toluene, 2 g of benzyltriethylamine chloride and 15 g of solid catalyst into the flask, and react under reflux for 8 hours while removing water. After the reaction, remove the catalyst by filtration, steam the unreacted butanol and toluene, add the residue into cold water and stir vigorously, and white crystals will precipitate out, then neutralize the unreacted acid with 5% sodium carbonate solution until the solution is weakly alkaline, suction filtered, and dried to obtain 136 g of the product butyl p-hydroxybenzoate, with a...

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PUM

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Abstract

The invention discloses a preparation method of butyl p-hydroxybenzoate, comprising the following steps of: firstly cleaning a 4A zeolite by distilled water, and controlling activation temperature; activating for a period of time, cooling, and then weighing a certain amount of the 4A zeolite; soaking in a toluenesulfonic acid solution; removing a water solution, and then drying to obtain a needed catalyst; adding p-hydroxybenzoic acid, butanol, toluene, benzyltriethylammonium chloride and the catalyst to a flask together, reacting in a reflux state, and also separating water; after the reaction is finished, filtering to remove the catalyst, and steaming unreacted and toluene; adding residues to cold water for intensely stirring so as to separate out white crystals; then neutralizing unreacted acid by a sodium carbonate solution till the sodium carbonate solution becomes alkalescent; filtering, and drying to obtain a product of the butyl p-hydroxybenzoate. The invention has low cost, easy storage, no side reaction in the production process, and corrosive damage on equipment.

Description

technical field [0001] The invention relates to a preparation method of butyl p-hydroxybenzoate. Background technique [0002] The trade name of butyl paraben is butylparaben, which is one of the safe and effective preservatives used in the world, and can be widely used in the manufacture of food, cosmetics, daily chemicals and pharmaceuticals. At present, its synthesis method usually adopts p-hydroxybenzoic acid and n-butanol, and directly prepares it under the action of concentrated sulfuric acid, but this method has problems such as serious equipment corrosion and prone to dehydration side reactions. In recent years, it has been reported to use heteropolyacids, super solid acids, etc. as catalysts. Although the effect is good, the price is relatively expensive, and there is a certain gap with the actual application. There is also the use of ferric chloride as a catalyst. The disadvantage is that it is easy to absorb moisture, is difficult to preserve, and is soluble in t...

Claims

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Application Information

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IPC IPC(8): C07C69/84C07C67/08B01J31/02
Inventor 李松伦
Owner 李松伦
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