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Method for preparing benzyl acetate by using waste reaction liquid generated in acetate production

A technology of benzyl acetate and acetate, which is applied in the field of synthesis of benzyl acetate, can solve the problems of poor product fragrance, high production cost, and large impact on equipment and the environment, so as to reduce energy consumption, ensure product quality, and reduce environmental pollution Effect

Inactive Publication Date: 2014-07-02
ZHUHAI FEIYANG NOVEL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are currently three main types of industrial production of benzyl acetate. The first one is prepared by using benzyl alcohol and acetic acid or acetic anhydride. The product of this method has an excellent fragrance, but because acetic acid or anhydride is used as the reaction raw material, it has a greater impact on equipment and the environment. , the production cost is also higher; the second is to adopt benzyl alcohol by-product benzyl ether and acetic anhydride to prepare benzyl acetate. ; The third is the benzyl chloride and sodium acetate method, which is the most economical production route, but the product fragrance is slightly worse

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Atmospheric pressure distillation produces reaction waste liquid of ethylene glycol diacetic acid, collects the distillate of 99.5-118.5 ℃, namely the acetic acid aqueous solution component, the mass percentage of acetic acid in the obtained acetic acid aqueous solution is 25%. Put more than 1000g of acetic acid aqueous solution into the reaction kettle, and slowly add 170g of sodium hydroxide until the pH of the solution is 13 at a stirring speed of 600r / s to obtain a sodium acetate solution, and then heat the sodium acetate solution to 80°C, at 0.6atm Carry out underpressure distillation to remove part of water, and stop the underpressure distillation when the water content of the sodium acetate solution in the reactor is 50%.

[0016] Add 70g of sec-butyl acetate, 468g of benzyl chloride and 10.8g of tetrabutylammonium bromide to the reaction kettle in sequence, and immediately raise the temperature to 110°C, and continue stirring for 8h. It is detected that there is ...

Embodiment 2

[0020] Atmospheric pressure distillation produces reaction waste liquid of ethylene glycol diacetic acid, collects the distillate of 99.5-118.5 ℃, namely the acetic acid aqueous solution component, the mass percentage of acetic acid in the obtained acetic acid aqueous solution is 25%. Put more than 1000g of acetic acid aqueous solution into the reaction kettle, and slowly add 170g of sodium hydroxide until the pH of the solution is 13 at a stirring speed of 600r / s to obtain a sodium acetate solution, and then heat the sodium acetate solution to 80°C, at 0.6atm Carry out underpressure distillation to remove part water, stop underpressure distillation when the water content to the sodium acetate solution in the reactor is 45%.

[0021] Add 70g of butyl acetate, 440g of benzyl chloride and 13.8g of tetrabutylammonium bromide to the reaction kettle in sequence, and immediately raise the temperature to 110°C, and continue to stir for 7h. It is detected that there is no benzyl chlori...

Embodiment 3

[0025] Atmospheric pressure distillation produces reaction waste liquid of ethylene glycol diacetic acid, collects the distillate of 99.5-118.5 ℃, namely the acetic acid aqueous solution component, and the mass percentage of acetic acid in the obtained acetic acid aqueous solution is 20%. Put more than 1000g of acetic acid aqueous solution into the reaction kettle, and slowly add 135g of sodium hydroxide until the pH of the solution is 12 at a stirring speed of 800r / s to obtain a sodium acetate solution, and then heat the sodium acetate solution to 75°C, at 0.5atm Carry out underpressure distillation to remove part water, stop underpressure distillation when the water content to the sodium acetate solution in the reactor is 45%.

[0026] Add 50 g of benzyl acetate, 380 g of benzyl chloride and 5.1 g of tetrabutylammonium bromide to the reaction kettle in sequence, and immediately raise the temperature to 110° C., and continue stirring for 8 hours. It is detected that there is n...

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Abstract

The invention relates to the technical field of benzyl acetate synthesis and in particular relates to a method for preparing benzyl acetate by using waste reaction liquid generated in acetate production. Benzyl acetate is prepared by steps of treating the waste reaction liquid, performing acid-base reaction, performing esterification reaction, desalting and rectifying. According to the method, benzyl acetate is prepared from acetic acid in the waste reaction liquid during the acetate production, so that the waste resources can be fully utilized, the resource waste can be reduced, and the environmental pollution caused by the acetate production can be alleviated; in addition, as a raw material is the waste reaction liquid generated in the acetate production, the production cost of benzyl acetate can be greatly reduced and the development requirements of environment-friendly and low-cost synthetic routes can be met; in a process of converting the waste reaction liquid into a reactant, heat emitted in the reaction between acetic acid and sodium hydroxide is fully utilized, the energy consumed for heating a sodium acetate solution is reduced, and the purposes of energy conservation and environmental protection are reached; benzyl acetate with the purity higher than 98% still can be prepared from the waste reaction liquid, and the product quality is ensured.

Description

technical field [0001] The invention relates to the technical field of synthesis of benzyl acetate, in particular to a method for preparing benzyl acetate from the reaction waste liquid of acetate production. Background technique [0002] Benzyl acetate is an ingredient used in flavors, which has a floral aroma and can be used in both cosmetics and food additives. In addition, benzyl acetate is also an excellent solvent for alkyd resins, nitrocellulose, dyes, greases and printing inks. Benzyl acetate has broad market prospects at home and abroad, and it is a synthetic fragrance with a large amount of consumption. In 2010, the annual sales volume in the international market has reached tens of thousands of tons, and the demand is still on the rise. There are currently three main types of industrial production of benzyl acetate. The first one is prepared by using benzyl alcohol and acetic acid or acetic anhydride. The product of this method has an excellent fragrance, but bec...

Claims

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Application Information

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IPC IPC(8): C07C69/157C07C67/10
CPCC07C67/11C07C67/48
Inventor 张余英谢成张宇博傅兵
Owner ZHUHAI FEIYANG NOVEL MATERIALS
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