De-coloring method of benzoic acid heavy by-product benzyl benzoate

A technology of benzyl benzoate and benzoic acid, which is applied in the field of decolorization of benzyl benzoate, a heavy by-product of benzoic acid, can solve the problems of high GC content of benzyl benzoate, low single-pass yield, solvent toxicity recovery, etc., and achieve production The process is simple, the product yield is high, and the production cost is low.

Active Publication Date: 2017-12-22
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest shortcoming of above-mentioned recovery method is that the benzyl benzoate finished product GC content that obtains is high and color number is high, but yield is low, and this greatly limits its scope of application
Although these methods can obtain the finished product of benzyl benzoate with low color number, there are problems such as low single-pass yield, the use of a large amount of reagents, the generation of a large amount of waste water, the use of solvents with certain toxicity and the need to consider recovery, complex operation steps and high energy consumption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The leftovers of benzoic acid produced by liquid-phase air oxidation of toluene in a chemical plant of A are used as raw materials:

[0023] 1) The leftovers of benzoic acid are produced by toluene liquid-phase air oxidation, and 100 g of benzyl benzoate crude product is obtained through vacuum distillation. After testing, the GC content of this benzyl benzoate is 99.38%, and the color number is 180 Hazen, which is added to the reaction vessel;

[0024] 2) Add 50 g of 10% acetic acid aqueous solution and 0.75 g of aluminum powder to the crude product of benzyl benzoate, then put the reaction vessel into a water bath, stir and raise the temperature to 70° C., and keep it warm for 6 hours;

[0025] 3) After the reaction is finished, it is cooled to room temperature, and the unreacted active metal is removed by filtration;

[0026] 4) The filtrate is stratified again to obtain the upper oil layer;

[0027] 5) Distill and dehydrate the oil layer under reduced pressure at 9...

Embodiment 2

[0029] The leftovers of benzoic acid produced by liquid-phase air oxidation of toluene in a certain B chemical plant are used as raw materials:

[0030] 1) The leftovers of benzoic acid are produced by toluene liquid-phase air oxidation, and 100 g of benzyl benzoate crude product is obtained through vacuum distillation. After testing, the GC content of this benzyl benzoate is 99.42%, and the color number is 200 Hazen, which is added to the reaction vessel;

[0031] 2) Add 50 g of 10% hydrochloric acid aqueous solution and 1 g of iron powder to the crude product of benzyl benzoate, then put the reaction vessel into a water bath, stir and raise the temperature to 100° C., and keep it warm for 5 hours;

[0032] 3) After the reaction is finished, it is cooled to room temperature, and the unreacted active metal is removed by filtration;

[0033] 4) The filtrate is stratified again to obtain the upper oil layer;

[0034] 5) Distill and dehydrate the oil layer under reduced pressure...

Embodiment 3

[0036] The leftovers of benzoic acid produced by liquid-phase air oxidation of toluene in a certain C chemical plant are used as raw materials:

[0037] 1) The leftovers of benzoic acid are produced by liquid-phase air oxidation of toluene, and 100 g of crude benzyl benzoate is obtained through vacuum distillation. After testing, the GC content of this benzyl benzoate is 99.54%, and the color number is 170 Hazen, which is added to the reaction vessel;

[0038] 2) Add 50 g of 10% sulfuric acid aqueous solution and 0.6 g of magnesium powder to the crude product of benzyl benzoate, then put the reaction vessel into a water bath, stir and raise the temperature to 50° C., and keep it warm for 8 hours;

[0039] 3) After the reaction is finished, it is cooled to room temperature, and the unreacted active metal is removed by filtration;

[0040] 4) The filtrate is stratified again to obtain the upper oil layer;

[0041] 5) Distill and dehydrate the oil layer under reduced pressure at...

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PUM

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Abstract

The invention discloses a de-coloring method of benzoic acid heavy by-product benzyl benzoate. The de-coloring method comprises the following steps: 1) producing a benzyl benzoate crude product through reduced-pressure distillation of leftovers from production of benzoic acid through methylbenzene liquid phase air oxidation; 2) adding reactive metal and an acidic solution into the benzyl benzoate crude product for thermal insulation reaction; 3) reducing the temperature to a room temperature after the end of reaction, and filtering and removing the unreacted reactive metal; 4) performing layered treatment on a filtrate to obtain an upper oil layer; and 5) performing reduced-pressure distillation and dehydration on the oil layer, wherein an obtained remaining material is a low-color benzyl benzoate finished product. The de-coloring method disclosed by the invention is advanced in process, convenient to operate and high in yield.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a decolorization method of benzyl benzoate, a heavy by-product of benzoic acid. Background technique [0002] Benzyl benzoate is mainly used as a solvent for artificial musk, vanillin and other fragrances, as a fixative for floral fragrances and as a blend of fragrances such as ylang-ylang. At present, benzyl benzoate industrial production method mainly contains the following several: the esterification reaction of sodium benzoate and benzyl chloride; the esterification reaction of benzoic acid and benzyl alcohol; or the transesterification of methyl (b) benzoate and benzyl alcohol reaction. In addition, in the process of producing benzoic acid by liquid-phase air oxidation of toluene, the main heavy by-product is benzyl benzoate, and the output is relatively large. Industrially, the heavy by-product benzyl benzoate recovery method of toluene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/78C07C67/54C07C67/60
CPCC07C67/54C07C67/60C07C69/78
Inventor 聂少春舒振操孙波黄正望毛利民
Owner WUHAN YOUJI IND
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