Preparation of benzyl acetate

A technology of benzyl acetate and a manufacturing method, applied in the field of preparing benzyl acetate, can solve the problems of high equipment cost, many equipment, expensive titanium metal, etc., and achieves the effects of safe transportation and storage, simple and convenient operation process, and less pollution of three wastes

Active Publication Date: 2009-05-20
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Dibenzyl ether is the main by-product in benzyl alcohol production (benzyl chloride hydrolysis method), and its amount reaches 13% (mass ratio) of benzyl alcohol final output, and it has occupied a considerable part in benzyl alcohol production cost; Benzyl ether is mostly underutilized except for a small part as a solvent
[0008] 1. The preparation of the catalyst itself requires more equipment, even more equipment than the production of ethyl benzyl ester, and the equipment cost is relatively large
[0009] 2. There are many operation steps in catalyst preparation, and there are many uncertain factors in the production process, so the quality is not easy to control
[0010] 3. Because the catalyst material titanium metal is relatively expensive, it needs to be recycled and reused, and the activity effect of the catalyst after regeneration is not easy to maintain stability
[0011] 4. The most difficult thing is that after industrial scale production, the corresponding equipment required for the roasting and activation operation in the preparation of catalysts in batches (such as 50-100 kg) is currently difficult to obtain
[0012] The above points have greatly limited the industrial application of the synthetic benzyl acetate process route with dibenzyl ether as raw material

Method used

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  • Preparation of benzyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 308g dibenzyl ether (industrial crude product, 91.43%, 1.420mol), 176g acetic anhydride (chemically pure, 99.0%, 1.706mol) and 7g (2.27%) solid acid catalyst p-toluenesulfonate respectively in a 1000ml three-necked flask acid, heated up to 130°C to 150°C, and reacted for 3 to 6 hours; after the reaction, about 483g of crude product was obtained, and sampling analysis showed that the content of benzyl acetate was 81.10% (GC), acetic anhydride 3.57% (GC), and dibenzyl ether 0.09% ( GC).

[0033] Put the above crude product in N 2 Distillation under reduced pressure under protection (the number of trays is about 1), the vacuum degree is -0.097~-0.098Mpa (the same below), and the material starts to discharge when the temperature of the material liquid rises to 45°C until the temperature of the material rises to about 220°C. When the material is not obvious, stop the distillation. A total of 399.3 g of distillates were received, with a benzyl acetate content of 91.24% ...

Embodiment 2

[0035] Feeding amount and reaction operation are the same as in Example 1, and the crude product obtained by the reaction is used with about 400ml of 20%Na 2 CO 3 The solution was neutralized to a pH value of 7, the brine layer was separated, and the obtained crude ester was subjected to vacuum distillation to obtain a total of 343.5 g of finished product, with a content of 99.61% (GC), a one-way yield of 79.86%, and a total yield of 83.9%.

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Abstract

The invention discloses a method for producing jasmal, which mainly adopts dibenzyl ether which is a high boiling waste produced by benzoic alcohol, as a raw material. The dibenzyl ether reacts with acetic anhydride in the presence of solid acid catalysts to obtain a crude product, and then the crude product is refined and purified to obtain an end product. The technology has simple operation process, stability, high efficiency, less pollution of the three wastes and applicability to the industrialized production.

Description

technical field [0001] The present invention relates to the manufacture method of chemical product, particularly a kind of method for preparing benzyl acetate. Background technique [0002] Benzyl acetate is a mature and widely used spice, mainly used in the preparation of jasmine-flavored essence and soap essence; in addition, it is also a widely used fine organic chemical product, used as resin, dye, oil, Solvents for inks, etc. [0003] At present, the preparation of benzyl acetate is mainly prepared by the following three methods: ① take benzyl chloride as raw material and synthesize it with sodium acetate in the presence of a phase transfer catalyst. ② It is obtained by reacting benzyl alcohol with acetic acid under the catalysis of strong ester (such as sulfuric acid). ③ Obtained by reacting dibenzyl ether with acetic anhydride under the catalysis of a superacid catalyst. [0004] Among the above-mentioned methods, the first two methods have been studied the most, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/157C07C67/10
Inventor 毛利民周宇邹晓虹聂少春郭涛王雷娟
Owner WUHAN YOUJI IND
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