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The method for reclaiming perfume grade benzyl benzoate from benzoic acid rectification raffinate

A technology for benzyl benzoate and benzoic acid, which is applied in the field of recovering perfume-grade benzyl benzoate, can solve the problems of pungent odor, high cost, low purity, etc., and achieves reduction of residual impurities, energy consumption, and low distillation temperature. Effect

Active Publication Date: 2021-04-13
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for recovering spice-grade benzyl benzoate from the benzoic acid rectification raffinate, which is used to solve the problems of low purity, dark color and pungent smell in extracting benzyl benzoate from the benzoic acid rectification raffinate. Problems, as well as the current situation that perfume grade benzyl benzoate is mainly produced by high-cost alcohol exchange method, greatly improve the resource utilization rate and economic value of benzoic acid distillation raffinate

Method used

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  • The method for reclaiming perfume grade benzyl benzoate from benzoic acid rectification raffinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Get the benzoic acid rectification raffinate that produces when the toluene oxidation production benzoic acid of certain benzoic acid production factory A is raw material, as figure 1 The process flow shown is processed as follows:

[0022] (1) Vacuum rectification: the benzoic acid rectification raffinate is passed in the rectification tower, the rectification tower tower kettle is heated by the falling film reboiler, and the mode rectification of vacuum rectification is used simultaneously to go out benzyl benzoate Ester crude product A, the conditions of vacuum distillation are pressure 50pa, tower bottom temperature 135°C, tower top temperature 123°C, the obtained benzyl benzoate crude product A has a content of 96.41% (mass fraction), a color number of 140HZ, and a pungent smell ;

[0023] (2) Alkali washing: the above-mentioned benzyl benzoate crude product A and mass fraction 20% sodium carbonate solution are mixed and stirred for reaction, the reaction temperat...

Embodiment 2

[0029] Get the benzoic acid rectification raffinate that produces when the toluene oxidation production of benzoic acid of the B factory that certain benzoic acid produces is raw material, as figure 1 The process flow shown is processed as follows:

[0030] (1) Vacuum rectification: the benzoic acid rectification raffinate is passed in the rectification tower, the rectification tower tower kettle is heated by the falling film reboiler, and the mode rectification of vacuum rectification is used simultaneously to go out benzyl benzoate Ester crude product A, the conditions of vacuum distillation are pressure 70pa, tower tank temperature 150°C, tower top temperature 131°C, the obtained benzyl benzoate crude product A has a content of 95.50% (mass fraction), color number 180HZ, and has a pungent smell ;

[0031](2) Alkali washing: the above-mentioned benzyl benzoate crude product A and mass fraction 15% sodium carbonate solution are mixed and stirred for reaction, the reaction te...

Embodiment 3

[0037] Get the benzoic acid rectification raffinate that produces when certain benzoic acid produces C factory toluene oxidation to produce benzoic acid as raw material, as figure 1 The process flow shown is processed as follows:

[0038] (1) Vacuum rectification: the benzoic acid rectification raffinate is passed in the rectification tower, the rectification tower tower kettle is heated by the falling film reboiler, and the mode rectification of vacuum rectification is used simultaneously to go out benzyl benzoate Ester crude product A, the conditions of vacuum distillation are pressure 130pa, column temperature 170°C, tower top temperature 138°C, the content of crude benzyl benzoate A obtained is 94.87% (mass fraction), color number 190HZ, and has a pungent smell ;

[0039] (2) Alkali washing: the above-mentioned benzyl benzoate crude product A and mass fraction 28% sodium carbonate solution are mixed and stirred for reaction, the reaction temperature is controlled at 40° C...

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Abstract

The invention discloses a method for recovering fragrance-grade benzyl benzoate from benzoic acid rectification raffinate. Using benzoic acid rectification raffinate as raw material, the crude product of benzyl benzoate is first extracted by vacuum distillation. Then alkali washing removes benzoic acid and most other impurities, and then using suspension crystallization technology, the above-mentioned crude benzyl ester is refined into colorless and high-purity fragrance-grade benzyl benzoate through steps such as cooling, crystallization, centrifugation, and washing. The raw material used in the present invention is the benzoic acid rectification raffinate treated as hazardous waste in the past, and the whole recovery process does not need other raw materials, and the energy used is only water, electricity, steam and purified benzyl benzoate, and benzyl benzoate falling film The energy consumption of heating rectification and suspension crystallization is relatively small. The purified and refined benzyl benzoate has a content of 99.50-99.99 percent, a color number of 5-15 Hz, a slight aroma, and satisfies the use standard of perfume-grade benzyl benzoate.

Description

technical field [0001] The invention relates to the field of recovery of pharmaceutical and chemical wastes, in particular to a method for recovering perfume-grade benzyl benzoate from benzoic acid rectification raffinate. Background technique [0002] Benzyl benzoate is a transparent, colorless crystal or oily liquid with a faint aroma. It 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, the benzyl benzoate industrial product is mainly synthesized by the reaction of sodium benzoate and benzyl chloride, but benzyl chloride cannot meet the production requirements of perfume grade benzyl benzoate because it has a pungent smell and contains chlorine elements. And when toluene is oxidized to produce benzoic acid, the by-product will contain a certain amount of benzyl benzoate, which has a higher boiling point and will exist in the benzoic acid rectifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/48C07C67/54C07C67/52C07C67/56C07C69/78
CPCC07C67/48C07C67/52C07C67/54C07C67/56C07C69/78
Inventor 黄正望孙波李立周峰李毅聂少春朱辉毛利民
Owner WUHAN YOUJI IND