Overdosed esterification production technology for n-octyl gallate

A technology for producing n-octyl gallate, which is applied in the field of preparing n-octyl gallate, can solve the problems of affecting the effect of esterification reaction and difficult separation of water, shorten the time of esterification reaction, cause no environmental pollution, reduce The effect of destruction

Inactive Publication Date: 2010-07-21
JIURUI BIOLOGY & CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult to separate dioxane from the water produced by the esterification reaction, which will affect the effect of the esterification reaction, so how to effectively separate the dehydrating agent from the good solvent is very important

Method used

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  • Overdosed esterification production technology for n-octyl gallate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 100g of industrial gallic acid, 250ml of n-octanol into a beaker, stir, add 7g of methanesulfonic acid catalyst, control the temperature at 80℃ to react for 2 hours, cool to 20℃ and filter, the filtrate is evaporated and concentrated under reduced pressure, recovered and evaporated The n-octanol solvent. After the product was recovered by alcohol, 400ml of cyclohexane solvent (99.0%) was added as a solvent for recrystallization. After filtration and washing with water, the filtrate was recrystallized by adding 400ml of cyclohexane solvent again, and the filtrate was filtered twice to recover the solvent. Filter, wash the filtered material until the pH is 6.0-7.0, take the filtrate and vacuum dry (60°C) to obtain 73.3 g of n-octyl gallate finished product, with a content of 99.2%.

Embodiment 2

[0027] Add 100g of industrial gallic acid, 500ml of n-octanol into a beaker, stir, add 7g of methanesulfonic acid catalyst, control the temperature at 80℃ to react for 2 hours, cool to 20℃ and filter, the filtrate is evaporated and concentrated under reduced pressure, recovered and evaporated The n-octanol solvent. After the product was recovered by alcohol, 400ml of cyclohexane solvent (99.0%) was added as a solvent for recrystallization. After filtration and washing with water, the filtrate was recrystallized by adding 400ml of cyclohexane solvent again, and the filtrate was filtered twice to recover the solvent. Filter, wash the filtered material until the pH is 6.0-7.0, take the filtrate and vacuum dry (60°C) to obtain 87.8 g of n-octyl gallate finished product, with a content of 99.3%.

Embodiment 3

[0029] Add 100g of industrial gallic acid, and 750ml of n-octanol into a beaker, stir, add 7g of methanesulfonic acid catalyst, control the temperature at 80℃ to react for 2 hours, cool to 20℃ and filter, the filtrate is evaporated and concentrated under reduced pressure, recovered and evaporated The n-octanol solvent. After the product is recovered by alcohol, 400ml of cyclohexane (99.0%) is added as a solvent for recrystallization. After filtration and washing with water, the filtrate is recrystallized by adding 400ml of cyclohexane solvent again. The filtrate after twice filtration is concentrated to recover the solvent and filter. , Wash the filtered material until the pH is 6.0-7.0, take the filtered material and vacuum dry (60°C) to obtain 78.1 g of n-octyl gallate finished product with a content of 99.5%.

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Abstract

The invention discloses overdosed esterification production technology for n-octyl gallate, which comprises the following steps: reacting gallic acid raw materials with n-octyl alcohol for an esterification reaction in the presence of an organic sulfonic acid catalyst; vaporizing and concentrating the filtrate under reduced pressure; adding cyclohexane for recrystallization; washing the filtrate by using purified water until the PH is between 6.0 and 7.0; and performing vacuum drying to obtain the end product of n-octyl gallate. The overdosed esterification production technology for the n-octyl gallate has the advantages of obviously shortening the esterification reaction time, having high reaction conversion rate, saving the high temperature distillation process under reduced pressure and reducing the damage to reaction products due to high temperature. The n-octyl alcohol is a reactant and a solvent used for the reaction, and the production cost is reduced.

Description

Technical field [0001] The invention relates to a method for preparing n-octyl gallate, in particular to a method for preparing n-octyl gallate by esterification reaction of excess n-octanol. Background technique [0002] Octyl gallate (English name Octyl gallate, hereinafter referred to as OG), also known as n-octyl 3,4,5-trihydroxybenzoate, is a food antioxidant with excellent performance and is widely used in fats and creams. And in fried foods, it has the functions of improving food quality, extending the shelf life of food, and enhancing preservation and anticorrosion. N-octyl gallate also has anti-platelet aggregation effects and has a therapeutic effect on cardiovascular and cerebrovascular diseases. It is a promising drug. In addition, n-octyl gallate is still producing carbonless copy paper and thermal recording paper as a developer to enhance the color development effect. [0003] The synthesis methods of n-octyl gallate can be divided into three categories: "transester...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/84C07C67/08
Inventor 陈学勇汤先赤汤赫银云峰
Owner JIURUI BIOLOGY & CHEM CO LTD
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