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A kind of preparation method of ethyl benzoate

A technology of ethyl benzoate and sodium benzoate, applied in the field of organic synthesis, can solve problems such as large amount of waste water, equipment corrosion, pollution, etc., and achieve the effects of improving conversion rate, no serious corrosion, and improving selectivity

Active Publication Date: 2021-08-31
HUAIAN WAN BANG SPICE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method mainly include: ① large amount of waste water, serious pollution; ② serious corrosion of equipment; ③ product yield is not too high, generally 90%-93%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 100g of sodium benzoate, 500g of toluene, and 5g of benzyltriethylammonium chloride into the autoclave, seal the autoclave, start stirring, replace the air in the autoclave with nitrogen, raise the temperature to 40°C, and slowly pass in the preheated (preheated The temperature is 60°C, the gasification pressure is 0.6Mpa) of ethyl chloride gas to react, and the reaction temperature is controlled at 50°C-70°C and the pressure is 0.4Mpa-0.6Mpa by controlling the amount of ethyl chloride. Reaction temperature was maintained by jacket heating. When the still pressure no longer drops, stop feeding the ethyl chloride gas, keep the pressure at 0.6Mpa for 1 hour, and finish the reaction. Lower the temperature to 30°C-40°C, release the pressure, replace with nitrogen, filter off the catalyst and sodium chloride produced by the reaction, and obtain a crude product containing toluene solvent.

[0022] After recovering the toluene solvent by distillation under normal pressure...

Embodiment 2

[0025] Put 100g of sodium benzoate, 400g of toluene recovered from Example 1, and 3g of tetrabutylammonium bromide into the autoclave, seal the autoclave, start stirring, replace the air in the autoclave with nitrogen, raise the temperature to 40°C, and slowly feed the preheated ( The preheating temperature is 50°C, the gasification pressure is 0.5Mpa) to react with ethyl chloride, and the reaction temperature is controlled at 50°C-70°C and the pressure is 0.4Mpa-0.6Mpa by controlling the amount of ethyl chloride introduced. Reaction temperature is maintained by jacket heating. When the still pressure no longer drops, stop feeding the ethyl chloride gas, keep the pressure at 0.6Mpa for 1 hour, and finish the reaction. Lower the temperature to 30°C-40°C, release the pressure, replace with nitrogen, filter off the catalyst and sodium chloride produced by the reaction, and obtain a crude product containing toluene solvent.

[0026] After recovering the toluene solvent by distill...

Embodiment 3

[0029] Put 100g of sodium benzoate, 600g of toluene recovered from Example 1, and 4g of benzyltriethylammonium bromide into the autoclave, seal the autoclave, start stirring, replace the air in the autoclave with nitrogen, raise the temperature to 40°C, and slowly introduce the preheating Then (the preheating temperature is 70°C, the gasification pressure is 0.7Mpa) to react with ethyl chloride, and the reaction temperature is controlled at 50°C-70°C and the pressure is 0.4Mpa-0.6Mpa by controlling the amount of ethyl chloride introduced. In the later stage of the reaction, the reaction temperature needs to be maintained by jacket heating. When the still pressure no longer drops, stop feeding the ethyl chloride gas, keep the pressure at 0.6Mpa for 1 hour, and finish the reaction. Lower the temperature to 30°C-40°C, release the pressure, replace with nitrogen, filter off the catalyst and sodium chloride produced by the reaction, and obtain a crude product containing toluene sol...

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Abstract

The invention discloses a preparation method of ethyl benzoate, comprising the following steps: putting sodium benzoate, toluene, and a phase transfer catalyst into a pressure kettle, replacing the air in the kettle with nitrogen, and feeding ethyl chloride at a certain temperature and pressure. After the reaction, the catalyst and the sodium chloride produced by the reaction are filtered off, the solvent toluene is recovered, and the finished product is obtained by rectification under reduced pressure. Compared with the current esterification process, the present invention has the advantages of high product yield, no serious corrosion of equipment, zero discharge of "waste water", and the like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, relates to a preparation method of perfume products, in particular to a preparation method of ethyl benzoate. Background technique [0002] Ethyl benzoate, Chinese alias ethyl benzoate. Appearance is colorless transparent liquid with sweet, fruity and medicinal aroma. Molecular formula is C 9 h 10 o 2 , molecular weight 150.18, melting point -34.6°C, boiling point 212.6°C, almost insoluble in water, soluble in organic solvents such as alcohol and ether. It is mainly used for blending daily flavors such as ylang-ylang, carnation, tuberose, and fern, as well as food flavors such as bananas, cherries, strawberries, peaches, grapes, vanilla, walnuts, wine, and tobacco. [0003] The existing industrial production method of ethyl benzoate is mainly formed by the esterification of benzoic acid and ethanol under strong acid catalysis. The disadvantages of this method mainly include: ① large amount ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/11C07C69/78
CPCC07C67/11C07C69/78
Inventor 陈文抗杨丽谢雨
Owner HUAIAN WAN BANG SPICE IND CO LTD
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