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Production method of glycerin tribenzoate

A technology of glycerol tribenzoate and its production method, which is applied in the chemical field, can solve the problems of deep color of the reaction system, low atom economy, and many side reactions, and achieve stable color, short process flow, and low solvent unit consumption Effect

Inactive Publication Date: 2016-02-24
浙江合糖科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new technology solves problems associated with current methods that use strong bases or long periods at elevated temperatures during chemical processes used to make certain products. These techniques have resulted in fewer unwanted compounds being formed due to lower reactivity towards other molecules involved in these reactions compared to older methods. Additionally, this technique allows for efficient separation between desired components without causing excessively large amounts of waste materials produced from previous steps. Overall, it provides technical benefits over traditional methods while minimizing harmful side rereactions caused by acid/alkal interactions.

Problems solved by technology

This patent describes different ways to make certain substances that have specific properties like resistance against bacteria, harmfulness towards humans, and high melting point (Tmax) compared to existing methods. However, these techniques involve expensive starting material sources, complex processes, use of hazardous compounds, long production times, and potential negative health effects associated therewith.

Method used

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  • Production method of glycerin tribenzoate
  • Production method of glycerin tribenzoate

Examples

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Embodiment 1

[0022] In a 1000L reactor, add 184Kg of glycerin, 0.3Kg of sodium hydroxide, 732Kg of benzoic acid, and 50Kg of toluene, stir and raise the temperature until it dissolves and becomes clear, and then continue to raise the temperature to 220°C. Heat preservation and reflux dehydration reaction until almost no water evaporates, and continue heat preservation reaction for 1 hour. After the reaction is complete, toluene and benzoic acid are reclaimed by distillation, and the residual benzoic acid is steamed out by nitrogen distillation. After the material in the kettle is put into a square pan to cool, 800.5Kg of white solid is obtained, with a content of 98.3%. The distilled benzoic acid and toluene can be directly applied to the next batch after water separation.

Embodiment 2

[0024] In a 1000L reaction kettle, add 184Kg of glycerin, 2Kg of potassium carbonate, 750Kg of benzoic acid, and 80Kg of xylene, stir and raise the temperature until dissolved and clear, and continue to raise the temperature to 220°C. Heat preservation and reflux dehydration reaction until almost no water evaporates, and continue heat preservation reaction for 1 hour. After the reaction is completed, xylene and benzoic acid are recovered by distillation. Nitrogen distillation was carried out to distill the residual benzoic acid, and the material in the still was put into a square pan to cool to obtain 806.1 Kg of white solid with a content of 99.1%. The distilled benzoic acid and xylene can be directly applied to the next batch after water separation.

Embodiment 3

[0026] In a 1000L reactor, add 184Kg of glycerin, 0.8Kg of sodium benzoate, 750Kg of benzoic acid, and 60Kg of n-octane, stir and raise the temperature until dissolved and clarified, and continue to raise the temperature to 220°C. Heat preservation and reflux dehydration reaction until almost no water evaporates, and continue heat preservation reaction for 1 hour. After the reaction is completed, n-octane and benzoic acid are recovered by distillation. The residual benzoic acid was steamed out by nitrogen distillation, and the material in the still was put into a square pan to cool to obtain 805.3 Kg of white solid with a content of 98.5%. The distilled benzoic acid and n-octane can be directly applied to the next batch after water separation.

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Abstract

The invention discloses a production method of glycerin tribenzoate. The production method comprises the following steps: carrying out heating reflux for water distribution on glycerol and benzoic acid under the existence of an alkaline substance and a dehydrating agent, carrying out a dehydration esterification reaction, carrying out reaction liquid post-treatment after the reaction is finished, to prepare the glycerin tribenzoate. A ratio of the amount of substance of the glycerol to the benzoic acid is 1: (3.0-3.3); and the alkaline substance is carbonate, bicarbonate, hydroxide or benzoate of alkali metals or alkaline-earth metals. In the invention, a dehydration esterification reaction is carried out under the existence of alkaline, so that side reactions such as glycerol polymerization and glycerol dehydration to generate acraldehyde and the like are greatly inhibited, production of corresponding by-products is reduced, and the yield of the principal product and the content of the product are improved. The operation is simple, the process stability is high, the corrosion and material requirements for equipment are greatly reduced, and meanwhile, the product is low and stable in chromaticity, being suitable for industrial production.

Description

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Claims

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Application Information

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Owner 浙江合糖科技有限公司
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