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Process for the production of diacyl peroxides

A technology for producing diacyl peroxide and diacyl peroxide, which is applied in the preparation of peroxy compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of expensive acid anhydride, high salt concentration in wastewater, expensive acid chloride, etc.

Active Publication Date: 2022-01-28
诺力昂化学品国际有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Acid chlorides are relatively expensive and produce a chloride-containing water layer, which results in high salt concentrations in the wastewater
[0013] On the other hand, acid anhydrides are even more expensive than acid chlorides and, due to the carboxylates formed, the waste stream of the process contains a high organic load, i.e. has a high chemical oxygen demand (COD) value and is therefore economically and environmentally unattractive force

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] An empty reactor equipped with a thermometer and a turbine impellor was loaded with 79 g of n-butyric anhydride and 16.9 g of D60 (ex-Total). While cooling the mixture at 15-17 °C, 194 g of 10.8 wt% NaOH solution and 12.4 g of 70 wt% H 2 o 2 solution.

[0082] After post-reaction for 5 minutes at 10° C., the aqueous phase was separated by gravity and subsequently removed. The organic layer containing 62.6% by weight of di-n-butyryl peroxide was treated with MgSO 4 2H 2 O was dried and filtered through a G3 glass filter.

[0083] The aqueous phase (241g) was mixed with 18.3g at 0-5°C The D60 were stirred together to extract residual peroxide and the layers were separated. followed by H 2 SO 4 (26.8 g, 96 wt%) was added to the aqueous layer causing the temperature to rise to 27°C. 215.4 g of an aqueous layer and 51.6 g of an organic layer were obtained, and these layers were separated. The organic compound in the organic layer consists of greater than 99% by ...

Embodiment 2

[0086] Load 45.6 g at 0°C into an empty reactor equipped with a thermometer and a turbo stirrer D60 (ex-Total) and 288g water. While cooling the mixture at 5 °C, 211 g of 25 wt% NaOH solution, 32.4 g of 70 wt% H 2 o 2 solution and 211 g isobutyric anhydride.

[0087] After post-reaction for 10 minutes at 5°C, the aqueous layer was allowed to settle by gravity and then removed. The organic layer contained 70.9% by weight of diisobutyryl peroxide, corresponding to a yield of 94%, calculated on the basis of anhydride. The aqueous layer contained about 24% by weight sodium isobutyrate.

[0088] Add 10.4g to the aqueous layer D60 and the resulting mixture was mixed at 0-5 °C. separate After D60 layer, 32.5g 96%H 2 SO 4 Add to aqueous layer. The resulting 270.1 g aqueous layer and 60.6 g organic isobutyric acid layer were separated. The organic compound in the organic layer consists of greater than 99.5% by weight of isobutyric acid.

[0089] After azeotropic removal ...

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PUM

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Abstract

Process for the production of a diacyl peroxide involving the reaction of an anhydride with hydrogen peroxide, removal of the formed carboxylic acid, production of an anhydride from said carboxylic acid, and recycling of the anhydride within the process.

Description

technical field [0001] The present invention relates to a process for the production of diacyl peroxide. Background technique [0002] Diacyl peroxide has the general formula [0003] R-C(=O)-O-O-C(=O)-R [0004] wherein the R groups are independently selected from aryl, arylalkyl, and linear, branched, and cyclic alkyl, optionally substituted with heteroatom-containing substituents. [0005] Such diacyl peroxides can be prepared by reacting an excess of acid anhydride or acid chloride with a basic solution of hydrogen peroxide as shown in the following formula: [0006] 2R-C(=O)-O-C(=O)-R+Na 2 o 2 →R-C(=O)-O-O-C(=O)-R+2NaOC(=O)R [0007] 2R-C(=O)Cl+Na 2 o 2 → R-C(=O)-O-O-C(=O)-R+2NaCl. [0008] In this reaction scheme, Na 2 o 2 does not refer to the independent product Na 2 o 2 , but refers to the inclusion of H 2 o 2 And the balance of NaOOH. [0009] US 3,956,396 discloses a process for the preparation of diacyl peroxide comprising reacting an anhydride wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/34C07C51/083C07C53/122C07C53/124C07C53/126C07C53/128C07C51/41C07C51/56
CPCC07C407/00C07C407/003C07C51/412C07C409/34C07C51/56C07C51/083C07C53/122C07C53/124C07C53/126C07C53/128
Inventor M·C·塔默A·德恩·巴博尔C·A·M·C·狄利克斯
Owner 诺力昂化学品国际有限公司