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Method for preparing benzyl acetate by using butyl benzyl phthalate rectified low-boiling-point substances

A technology of butyl benzyl phthalate and benzyl acetate, which is applied in the field of preparing benzyl acetate, can solve problems such as inability to separate, waste resources, and large economic losses, and achieve the effects of contributing to environmental protection, saving resources, and low cost

Active Publication Date: 2014-08-27
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the boiling points of benzyl alcohol and benzyl butyl ether are very close, the two components cannot be separated by rectification. At present, the low-boiling mixture can only be treated as a waste product, which leads to serious waste of resources and huge economic losses.

Method used

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  • Method for preparing benzyl acetate by using butyl benzyl phthalate rectified low-boiling-point substances
  • Method for preparing benzyl acetate by using butyl benzyl phthalate rectified low-boiling-point substances

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A kind of method that utilizes butyl benzyl phthalate rectification low boiler to prepare benzyl acetate comprises the following steps:

[0026] 1) In a 100mL three-necked flask, add 300g of butyl benzyl phthalate rectification low boiler, 200g of acetic acid (98% purity), 30mL toluene (98% purity) and 1.5g sulfamic acid (95% purity) After testing, benzyl alcohol content is 80% (GC, area %), benzyl butyl ether content is 20% (GC) in this phthalate butyl benzyl ester rectification low boiler, heat up to 110°C azeotropic reflux reaction and water separation;

[0027] 2) When there is no obvious water in the phase separator, add 73g acetic anhydride (98% purity) and 1.5g sulfamic acid (95% purity) to the reactor, and heat up to 140-150°C to continue the reaction. Use gas chromatography to monitor the reaction process. When the residual benzyl butyl ether component content in the system is lower than 0.2% (GC, area %), you can stop heating and cool down;

[0028] 3) The p...

Embodiment 2

[0030] A kind of method that utilizes butyl benzyl phthalate rectification low boiler to prepare benzyl acetate comprises the following steps:

[0031] 1) Add 120kg butyl benzyl phthalate rectification low boiler (component is the same as embodiment 1), 72kg glacial acetic acid, 1.5kg p-toluenesulfonic acid (purity 95%), 30kg butyl acetate in 300L reactor (purity 98%), heating the reactor to 110°C for azeotropic reflux and water separation;

[0032] 2) When there is no obvious water in the phase separator, add 35kg of acetic anhydride and 1.5kg of p-toluenesulfonic acid to the reactor, and heat up to 150°C to continue the reaction. During the reaction, use gas chromatography to monitor the reaction process. When the system When the remaining benzyl butyl ether component content is lower than 0.2% (GC), the heating can be stopped and cooled;

[0033] 3) The product obtained by the reaction is distilled under reduced pressure to remove remaining acetic acid, acetic anhydride an...

Embodiment 3

[0035] A kind of method that utilizes butyl benzyl phthalate rectification low boiler to prepare benzyl acetate comprises the following steps:

[0036] 1) Add 120kg butyl benzyl phthalate rectification low boiler (component is the same as embodiment 1), 70kg glacial acetic acid, 1.5kg sulfamic acid, 30kg butyl acetate in the 300L reactor, heat up the reactor Azeotropic reflux at 110°C for water separation;

[0037] 2) When there is no obvious water in the phase separator, add 35kg of acetic anhydride and 1.5kg of p-toluenesulfonic acid to the reactor, and heat up to 160°C for reaction. During the reaction, use gas chromatography to monitor the reaction process. When the benzyl butyl ether component content is lower than 0.2% (GC), the heating can be stopped and cooled;

[0038] 3) The product obtained by the reaction is distilled under reduced pressure to remove low boilers such as acetic acid, acetic anhydride and butyl acetate remaining in the crude product, and the resulti...

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Abstract

The invention discloses a method for preparing benzyl acetate by using butyl benzyl phthalate rectified low-boiling-point substances. The method comprises the following steps: (1) adding the butyl benzyl phthalate rectified low-boiling-point substances, acetic acid, a first catalyst and a water-carrying agent into a reactor, heating to 90-130 DEG C for performing reflux reaction, and separating water until no water is separated out from a phase splitter; (2) adding acetic anhydride and a second catalyst into the reactor, continuously heating to 130-160 DEC for performing reflux reaction, tracking by gas chromatography, and stopping heating when the content of residual benzyl butyl ether in reaction materials is less than 0.2%; (3) performing reduced-pressure distillation on a reaction product to remove impurities, washing to be neutral by using 15wt%-25wt% of a sodium carbonate solution, and washing with water and rectifying to obtain a finished product of benzyl acetate. The practice proves that the method is simple and convenient to operate, high in efficiency, low in production cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical spices, and specifically refers to a method for preparing benzyl acetate by using butyl benzyl phthalate to rectify low boilers. Background technique [0002] Butylbenzyl phthalate is a plasticizer, mainly used in the processing of plastic products to improve the plasticity and fluidity of the resin, and when combined with other plasticizers, it can make the product have excellent transparency and smooth surface. [0003] At present, the main method of industrial production of butyl benzyl phthalate is generally to generate monobutyl phthalate through the esterification reaction of phthalic anhydride and butanol, and then neutralize with liquid caustic soda to generate sodium monobutyl phthalate Salt, and then undergo condensation reaction with benzyl chloride under the catalysis of triethylamine to produce butyl benzyl phthalate. [0004] Generate butyl benzyl phthalate reaction...

Claims

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Application Information

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IPC IPC(8): C07C69/157C07C67/08C07C67/24
CPCC07C67/08C07C67/24C07C69/157C07C69/14
Inventor 舒振操孙波林士海陈乐张龙基肖翔黄正望毛利民
Owner WUHAN YOUJI IND
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