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Production method of isoamyl salicylate

A technology of isoamyl salicylate and a production method, which are applied in chemical instruments and methods, reaction preparation of ester groups and hydroxyl groups, organic chemistry, etc., can solve the problem of reducing the yield of isoamyl salicylate, reducing the reaction selectivity, Easy to corrode equipment and other problems, to achieve the effect of reducing production costs, improving selectivity, and convenient recycling

Inactive Publication Date: 2019-06-21
天津大加化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation method of this isoamyl salicylate adopts concentrated sulfuric acid as a catalyst to esterify salicylic acid and isoamyl alcohol to obtain isoamyl salicylate, but the use of concentrated sulfuric acid as a catalyst is not only easy to corrode equipment, but also There are many reactions, thereby reducing the selectivity of the reaction and reducing the productive rate of isoamyl salicylate

Method used

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  • Production method of isoamyl salicylate
  • Production method of isoamyl salicylate
  • Production method of isoamyl salicylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A kind of production method of isoamyl salicylate, comprises the steps:

[0042] (1) preparation of isoamyl salicylate: 0.5Kg methyl salicylate, 1Kg isoamyl alcohol, 4.5g solid superacid catalyst are mixed homogeneously, at this moment, the weight of solid superacid catalyst accounts for methyl salicylate and 0.3wt% of the total weight of isoamyl alcohol, under the condition of microwave radiation power of 200W and constant stirring, irradiate for 80 minutes to obtain crude ester-catalyst mixture and methanol gas, and the methanol gas is condensed and recycled;

[0043] (2) Crude ester separation and washing: filter the crude ester-catalyst mixture, separate the crude ester and solid superacid catalyst, recover and recycle the solid superacid catalyst, then add water to the crude ester, wash the crude ester with water, and separate The crude ester organic layer and washing water are removed, and the washing water is recovered and recycled;

[0044] (3) Crude ester vacu...

Embodiment 2

[0048] A production method of isoamyl salicylate, comprising the steps:

[0049] (1) isoamyl salicylate preparation: 0.8Kg methyl salicylate, 1Kg isoamyl alcohol, 10.8g solid superacid catalyst are mixed, at this moment, the weight of solid superacid catalyst accounts for methyl salicylate and 0.6wt% of the total weight of isoamyl alcohol, under the condition of microwave radiation power of 225W and constant stirring, radiate for 60min to obtain crude ester-catalyst mixture and methanol gas, and the methanol gas is condensed and recycled;

[0050] (2) crude ester separation and washing: the crude ester-catalyst mixture is filtered, the crude ester and the solid superacid catalyst are separated, and the solid superacid catalyst is recovered and recycled, and then water is added to the crude ester, and the crude ester is washed with water and separated The crude ester organic layer and washing water are taken out, and the washing water is recovered and recycled;

[0051] (3) un...

Embodiment 3

[0055] A production method of isoamyl salicylate, comprising the steps:

[0056] (1) isoamyl salicylate preparation: 1.2Kg methyl salicylate, 1Kg isoamyl alcohol, 19.8g solid superacid catalyst are mixed, at this moment, the weight of solid superacid catalyst accounts for methyl salicylate and 0.9wt% of the total weight of isoamyl alcohol, under the condition of microwave radiation power of 220W and constant stirring, radiate for 55min to obtain crude ester-catalyst mixture and methanol gas, and the methanol gas is condensed and recycled;

[0057] (2) crude ester separation and washing: the crude ester-catalyst mixture is filtered, the crude ester and the solid superacid catalyst are separated, and the solid superacid catalyst is recovered and recycled, and then water is added to the crude ester, and the crude ester is washed with water and separated The crude ester organic layer and washing water are taken out, and the washing water is recovered and recycled;

[0058] (3) un...

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Abstract

The invention relates to a production method of isoamyl salicylate, and belongs to the technical field of isoamyl salicylate. The production method comprises the following steps: preparing the isoamylsalicylate, separating crude ester, washing the crude ester with water, and distilling the crude ester under reduced pressure, wherein under the conditions of a solid superstrong acid catalyst and microwave irradiation, a reaction is performed on methyl salicylate and isoamyl alcohol to produce the isoamyl salicylate; the solid superstrong acid catalyst comprises an active component and a carrier; the active component comprises lanthanum sulfate, molybdenum sulfate and cesium sulfate; the carrier is titanium dioxide. By the production method of the isoamyl salicylate, corrosion of equipment during production is reduced, so that the service life of the equipment is prolonged; in addition, the advantages of simple technology and relatively high selectivity are achieved; meanwhile, the solidsuperstrong acid catalyst is easy to separate and recycle.

Description

technical field [0001] The present invention relates to the technical field of isoamyl salicylate, more specifically, it relates to a kind of production method of isoamyl salicylate. Background technique [0002] Isoamyl Salicylate is a colorless or light yellow liquid with strong floral scent and long-lasting fragrance. Isoamyl salicylate can be added to grass orchid essence, xiangwei, Su Xinlan, and can also be used in medicine and food to play a role in fixing fragrance. [0003] At present, the patent application literature with the application publication number CN102249926A discloses a preparation method of isoamyl salicylate. The raw materials include 65-75 g of salicylic acid, 440-460 g of isoamyl alcohol, and 18-25 g of concentrated sulfuric acid. , neutralization, water washing and distillation to prepare isoamyl salicylate. The preparation method of this isoamyl salicylate adopts concentrated sulfuric acid as a catalyst to esterify salicylic acid and isoamyl alc...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/84B01J27/053
CPCY02P20/584
Inventor 游云深赵旭阳游乃生易于伟
Owner 天津大加化工有限公司
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