Method for preparing benzyl benzoate by oxidizing dibenzyl ether

A technology of benzyl benzoate and oxidized dibenzyl ether, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve the problems of rarely used, high cost, and limited application fields, and achieves the goal of preparing Low cost and good product quality

Inactive Publication Date: 2012-11-07
HUBEI GREENHOME MATERIALS TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The products prepared by the catalytic synthesis method of benzyl chloride and sodium benzoate are very limited in use because of chlorine, and the cost is also high; the ester conversion method is rarely used due to cost reasons

Method used

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  • Method for preparing benzyl benzoate by oxidizing dibenzyl ether
  • Method for preparing benzyl benzoate by oxidizing dibenzyl ether
  • Method for preparing benzyl benzoate by oxidizing dibenzyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 445g of dibenzyl ether (purity: 89.54%) into the oxidation kettle equipped with a separation tower, heat it, and when the temperature of the kettle rises to about 200°C, start to introduce air, and the air flow rate is 0.15m 3 / h. When the temperature of the kettle rises to about 230°C and there is almost no output from the top of the fractionation tower, close the air inlet valve, and take a kettle sample for analysis. The kettle sample contains 4.56% benzoic acid, 2.72% dibenzyl ether, and benzyl benzoate. Esters 84.42%. Transfer all the liquid from the still to a rectifying still, heat it, and collect fractions at 145-160°C to obtain 186 g of crude benzyl ester, which contains 2.36% benzoic acid, 0.86% dibenzyl ether, and 95.33% benzyl ester. The crude product was neutralized, cooled and crystallized, and separated to obtain 244 g of crystals. The composition was as follows: benzoic acid 0.089ml / 0.1N NaOH / g, dibenzyl ether 0.32%, and benzyl ester 99.58%.

Embodiment 2

[0027] According to the same dibenzyl ether consumption and temperature of reaction of embodiment 1, investigate the impact of different air consumptions on the ratio of gained benzaldehyde and benzyl benzoate, as shown in table 1:

[0028] Table 1

[0029]

Embodiment 3

[0031] According to the same raw material consumption of embodiment 1, investigate the impact of different oxidation temperatures on the ratio of gained benzaldehyde and benzyl benzoate, as shown in table 2:

[0032] Table 2

[0033]

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Abstract

The invention discloses a method for preparing benzyl benzoate by oxidizing dibenzyl ether, which comprises steps as follows: A, oxidization; B, rectification and refining; C, acid-alkali neutralization; D, freezing crystallization; and E, centrifugal separation. According to the method disclosed by the invention, by-product dibenzyl ether produced by benzyl alcohol preparation is used as a raw material, so that the defects of other benzyl benzoate preparation methods are well solved; the preparation cost is low, the product quality is good, and no pollution is caused; and therefore, the preparation method disclosed by the invention is the method of preparing high-quality benzyl benzoate by low cost.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a method for preparing benzyl benzoate by oxidizing dibenzyl ether, which has low preparation cost, good product quality and no pollution. Background technique [0002] Benzyl benzoate is a colorless or light yellow oily liquid, insoluble in water but soluble in most organic solvents, with a melting point of 17°C, a boiling point of 323.5°C and a flash point of 148°C. It is mainly used in medicine, spices, textiles and other industries. [0003] According to published bibliographical reports, the preparation of benzyl benzoate mainly adopts methods such as benzyl chloride and sodium benzoate catalytic synthesis, ester transformation at present. The products prepared by the catalytic synthesis method of benzyl chloride and sodium benzoate are very limited in use because of containing chlorine, and the cost is also high; the ester conversion method is seldom used because ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/78C07C67/39
Inventor 杨华肖华青黄圣
Owner HUBEI GREENHOME MATERIALS TECH INC
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