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Synthesis method of acetylsalicylic acid

A technology of acetylsalicylic acid and synthesis method, applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve the problems of industrial application limitation, poor thermal stability, accelerated deactivation speed and the like, Achieve simple preparation process, maintain high activity, and maintain the effect of repeated use

Inactive Publication Date: 2013-02-20
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The synthesis process of acetylsalicylic acid has been applied in recent years. 4 2- / M x o y type solid superacid catalyst reports, but in the liquid-solid reaction system, SO 4 2- / M x o y The sulfate radicals on the surface of the catalyst will dissolve slowly, which will significantly reduce the acid strength, accelerate the deactivation speed, and the thermal stability is not good, so the industrial application is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 10gZrOCl 2 ·8H 2 O solid was dissolved in 150mL of deionized water, 1.80mL of 50.0% (weight) ammonium metatungstate solution was added and heated to boiling, then 6mL of 36.0% (weight) urea solution was added, and the reflux was continued for 3h and then naturally cooled to room temperature. Under full stirring, add ammonia water dropwise, adjust the pH to 8-9, then put it into an ultrasonic generator, undergo ultrasonic treatment at a frequency of 50kHz and a power of 450W for 30min, age for 12h, and then filter and wash until no Cl can be detected. - Ion, dried at 110°C and then calcined at 750°C to obtain the WO patented by the present invention 3 / ZrO 2 Solid superacid catalyst.

[0015] Add 30g of salicylic acid, 62mL of acetic anhydride and 1g of the above self-made WO into the reaction vessel 3 / ZrO 2 The catalyst is heated in a water bath to 75-95°C for reaction. After the reaction is completed, it is suction-filtered while it is hot, and the catalyst is re...

Embodiment 2

[0017] Add 30g of salicylic acid, 41mL of acetic anhydride and 1g of the above self-made WO into the reaction vessel 3 / ZrO 2 Catalyst, water bath is heated to setting temperature and reacts, all the other operations are the same as embodiment 1. The yield is 82.5% based on the pure product after recrystallization.

Embodiment 3

[0019] Add 30g of salicylic acid, 62mL of acetic anhydride and 0.5g of the above self-made WO into the reaction vessel 3 / ZrO 2 Catalyst, water bath is heated to setting temperature and reacts, all the other operations are the same as embodiment 1. The yield is 79.2% based on the pure product after recrystallization.

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PUM

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Abstract

The invention provides a synthesis method of acetylsalicylic acid, relating to the technical field of chemical synthesis. Firstly ZrOCl2. 8H2O solid is dissolved in deionized water, ammonium paratungstate aqueous solution and urea aqueous solution are added, refluxing is carried out, ammonia water is used for regulating pH value, ultrasonic processing, ageing and filtration and washing are carried out, and then drying and roasting are carried out, thus obtaining WO3 / ZrO2 solid super acidic catalyst; then salicylic acid, acetic anhydride and catalyst are added into a reaction vessel, heating is carried out, and filtration is carried out when solution is hot after reaction is finished; filtrate is taken, excessive acetic anhydride is hydrolyzed, standing and cooling are carried out, white crystal is separated out, ice water is used for cooling until crystallization is completely finished; the white crystal is subject to filtration, cold water is used for washing, thus obtaining acetylsalicylic acid crude product, and then mixed solvent of ethanol and water is used for recrystallization, thus obtaining the acetylsalicylic acid. The invention improves the process for preparing WO3 / ZrO2 solid super acid, ultrasonic processing is introduced in, catalyst is easy to recycle, high activity can be maintained, reuse can be realized, and the invention is environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to the technical field of synthesis technology of acetylsalicylic acid. Background technique [0002] Acetylsalicylic acid, also known as aspirin, is one of the most widely used drugs in the world, and its application range is still expanding, and a large number of acetylsalicylic acid derivative drugs have been developed. In industry, acetylsalicylic acid is obtained by using salicylic acid and acetic anhydride in concentrated H 2 SO 4 or H 3 PO 4 It is prepared by acylation reaction under catalysis. Although the process is mature, the product yield is not high, and there are many side reactions, poor product quality, serious equipment corrosion, and a large amount of waste acid polluting the environment. Therefore, it is necessary to seek high catalytic activity and Environmentally-friendly catalysts and the development of green synthesis processes for acetylsalicyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/157C07C67/08B01J23/30
CPCY02P20/584
Inventor 张存刘涛
Owner YANGZHOU UNIV
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