Method for synthesis of high-concentration anhydrous peracetic acid solution and co-production of acetylurea

A technology of anhydrous peroxyacetic acid and acetic acid solution, which is applied to the preparation of peroxygen compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of high explosion risk factor, complicated production equipment, and reduced yield. The effect of simple process flow, low equipment investment and high added value

Active Publication Date: 2016-05-04
LIMING RES INST OF CHEM IND
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Problems solved by technology

The aqueous solution of high-concentration peracetic acid is also used as organic synthesis, but because the presence of water will cause the hydrolysis of the target product to reduce the yield, and the by-products produced by hydrolysis will increase the difficulty of purification and post-treatment of the target product, so in organic synthesis. The anhydrous organic solution of peracetic acid in the field of synthesis is often used as an oxidizing agent
However, the anhydrous organic solution of peracetic acid is mainly prepared by oxidation of acetaldehyde, the process and production equipment are complex, the explosion risk factor is high, and the equipment investment is huge. Therefore, it is important to develop a new method with simpler technology, high safety and low investment. the meaning of

Method used

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  • Method for synthesis of high-concentration anhydrous peracetic acid solution and co-production of acetylurea

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 98.65 g of percarbamide with an active oxygen content of 16.2% into a glass reactor, add 1 g of boric acid, and then inject 51.5 g of acetic anhydride; heat the reactor to 50° C. and stir the reaction mixture until the percarbamide is completely dissolved; The remaining 154.5g of acetic anhydride was slowly dropped into the reaction solution through a constant flow device, and the reaction solution was controlled to reflux slightly during the dropping process; after the dropwise addition of acetic anhydride, the reaction solution was maintained at 50°C and stirred for 1.5h. After the reaction is over, send the mixed solution into a vacuum distillation device, first turn on the decompression device to control the absolute pressure in the device to 31.33kPa, then heat the mixed solution to 90°C, collect the distillate at 65°C, and obtain a colorless and transparent high The concentration of the acetic acid solution of anhydrous peracetic acid is about 164ml, the densit...

Embodiment 2

[0020] Add 193.75 g of percarbamide with an active oxygen content of 16.5% into a glass reactor, then add 2.85 g of sodium borate, and then inject 102.86 g of acetic anhydride; raise the temperature of the reactor to 50° C. and stir the reaction mixture until the percarbamide is completely dissolved; The remaining 309.20 g of acetic anhydride was slowly dropped into the reaction solution through a constant flow device, and the reaction solution was slightly refluxed during the dropping process; after the dropwise addition of acetic anhydride, the reaction solution was maintained at 50° C. and stirred for 1 hour. After the reaction is over, send the mixed solution into a vacuum distillation device, first turn on the decompression device to control the absolute pressure in the device to 11.33kPa, then heat the mixed solution to 70°C, collect the distillate at 60°C, and obtain a colorless and transparent high The concentration of the acetic acid solution of anhydrous peracetic aci...

Embodiment 3

[0022] Add 300.12 g of percarbamide with an active oxygen content of 16.0% into a glass reactor, then add 5.94 g of sodium perborate tetrahydrate, and then inject 155.20 g of acetic anhydride; heat the reactor to 50° C. and stir the reaction mixture to reach percarbamide All dissolved; then the remaining 465.50g of acetic anhydride was slowly dropped into the reaction solution through a constant flow device, and the dropping process was controlled to slightly reflux the reaction solution; after the dropwise addition of acetic anhydride, the reaction solution was maintained at 50°C and stirred for 0.5h. After the reaction is over, send the mixed solution into a vacuum distillation device, first open the decompression device to control the absolute pressure in the device to 6.33kPa, then heat the mixed solution to 60°C, collect the distillate at 55°C, and obtain a colorless and transparent high The concentration of the acetic acid solution of anhydrous peracetic acid is about 456...

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Abstract

The invention discloses a method for synthesis of a high-concentration anhydrous peracetic acid solution and co-production of acetylurea. According to the method, peracetic acid and acetylurea are generated via a reaction between percarbamide and acetic anhydride under the action of a catalyst; and then the high-concentration anhydrous peracetic acid solution is separated out via vacuum distillation, the residual distillate is frozen, and the frozen residual distillate is recrystallized for preparation of acetylurea, wherein the catalyst is selected from boric acid, metaboric acid, sodium borate, sodium metaborate, sodium perborate or a corresponding hydrate. As the raw materials, percarbamide and acetic anhydride are cheap and easy to obtain; compared with a method for preparing the anhydrous peracetic acid solution via acetaldehyde oxidation, the method provided by the invention is simpler, less in equipment investment and safer; and by adoption of the method provided by the invention, both the anhydrous peracetic acid solution and acetylurea are prepared, so that the application range is broad and the added value is high.

Description

technical field [0001] The invention belongs to the technical field of peracetic acid, in particular to a method for co-producing acetylurea from a high-concentration anhydrous peracetic acid solution. Background technique [0002] Peracetic acid is an important industrial oxidant and high-efficiency medical fungicide. It is widely used in material synthesis in the chemical industry, diesel desulfurization in the petroleum industry, fabric bleaching in the textile industry, and sterilization and disinfection in the medical and health field. There are two main preparation methods of peracetic acid: one is to use acetic acid or acetic anhydride and H 2 o 2 The aqueous solution is reacted under the catalysis of concentrated sulfuric acid, and then distilled to prepare a certain concentration of peracetic acid aqueous solution; the other is to use acetaldehyde and oxygen to prepare peracetic acid ethyl acetate through gas phase or liquid phase reaction under the action of catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/26C07C273/18C07C275/50
CPCC07C273/18C07C407/00C07C409/26C07C275/50
Inventor 李韶峰何红振程磊于文杰王宏伟
Owner LIMING RES INST OF CHEM IND
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