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Preparation method of nipagin ester

A technology of paraben ester and ethanol, which is applied in the field of preparation of paraben ester, can solve problems such as the yield of paraben ester needs to be improved, easy-to-corrosion equipment, and long reaction time, and achieves catalytic activity that can be recycled and reused. Effects of reducing corrosion and fast synthesis rate

Pending Publication Date: 2022-03-22
无锡江大百泰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But concentrated sulfuric acid is except that reaction time is too long as catalyzer, except the shortcoming such as easy corrosion equipment, the synthetic paraben productive rate still needs to improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0030] Preparation of ethanolamine ionic liquid:

[0031] Dissolve 11kg of N,N-dimethylethanolamine in ethanol solvent, slowly drop into 5.5kg of ethyl chloride in an ice-water bath, heat and reflux at 70°C for 10h, after the reaction is completed, distill off the ethanol to obtain a solid The product was recrystallized three times, and the ethanolamine ionic liquid was obtained after drying.

preparation example 2

[0033] Preparation of diethanolamine ionic liquid:

[0034] Dissolve 11kg of N,N-dimethylethanolamine in ethanol solvent, slowly drop into 11kg of ethyl chloride in an ice-water bath, heat and reflux at 80°C for 11h, after the reaction is completed, distill off the ethanol to obtain a solid product After recrystallization three times, diethanolamine ionic liquid was obtained after drying.

preparation example 3

[0036] Preparation of triethanolamine ionic liquid:

[0037] Dissolve 11kg of N,N-dimethylethanolamine in ethanol solvent, slowly drop into 16.5kg of ethyl chloride in an ice-water bath, heat and reflux at 90°C for 12h, after the reaction is completed, distill off the ethanol to obtain a solid The product was recrystallized three times, and the triethanolamine ionic liquid was obtained after drying.

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PUM

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Abstract

The invention relates to the technical field of preparation methods, and discloses a preparation method of nipagin ester, which comprises the following steps: adding p-hydroxybenzoic acid, methanol, ethanol, propanol, butanol, n-heptanol, an alcamines ionic liquid and a dehydrating agent into a reaction container, stirring for 10-20 minutes at the reaction temperature of 120-150 DEG C for 5-9 hours, and after the reaction is finished, filtering to obtain the nipagin ester. And cooling the reaction mixture, standing, layering, separating out an ester layer, firstly steaming out the dehydrating agent, then steaming out unreacted alcohol, cooling, curing, and recrystallizing to obtain the target product. The method has the effect of improving the yield of the nipagin ester.

Description

technical field [0001] The application relates to the technical field of chemical synthesis, in particular to a preparation method of parabens. Background technique [0002] Paraben is a common name for parabens and is an internationally recognized food preservative. It has broad-spectrum, high efficiency and low toxicity, and is widely used in medicine, food and cosmetics and other industries. [0003] The synthetic method of paraben mostly adopts the concentrated sulfuric acid as catalyst at present, synthesizes paraben by the esterification reaction of p-hydroxybenzoic acid and alcohol. But the concentrated sulfuric acid is except having too long reaction time as catalyzer, except the disadvantages such as easy corrosion equipment, the synthetic paraben productive rate still needs to be improved. Contents of the invention [0004] In order to make the yield of synthetic paraben ester higher, the application provides a kind of preparation method of paraben ester. [00...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/84B01J31/02B01J27/053
CPCC07C67/08B01J31/0279B01J31/0285B01J27/053B01J2231/49C07C69/84
Inventor 陈国安杨盛荣张显久赵樾
Owner 无锡江大百泰科技有限公司