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Method for purifying alkyl hydroperoxide by extraction with water and separation of the aqueous phase

An alkyl hydroperoxide, alkyl peroxide technology, applied in separation methods, peroxy compound preparation, chemical instruments and methods, etc., can solve the problems of low productivity, difficulty in purifying alkyl hydroperoxides, and the like, Minimize risks, avoid side effects, and reduce safety issues

Pending Publication Date: 2021-02-26
ARKEMA FRANCE SA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this technology originate on the one hand from its low productivity (if one considers that the same reactor implements several stages (salt formation / separation by settling, re-acidification / extraction)) and on the other hand from the large amount of brine effluent Formation
[0022] For reasons of quality and safety of the product to be purified, it is therefore important to limit the processing temperature as much as possible, which makes the purification of alkyl hydroperoxides increasingly difficult

Method used

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  • Method for purifying alkyl hydroperoxide by extraction with water and separation of the aqueous phase

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0077] Preparation of hydroperoxide

[0078] As indicated above, the process according to the invention involves the purification of a mixture comprising at least one alkyl hydroperoxide and at least one dialkyl peroxide.

[0079] Preferably, said mixture is obtained after the preparation of the alkyl hydroperoxide in question.

[0080] In other words, the process according to the invention is aimed at purifying the alkyl hydroperoxides obtained by synthesis.

[0081] Preferably, the alkyl hydroperoxides can be prepared in acidic media.

[0082] In other words, the process according to the invention may comprise, prior to stage a), a stage a') of synthesis of said alkyl hydroperoxide in an acidic medium.

[0083] In this case, the process for the preparation of alkyl hydroperoxides consists in particular in reacting aqueous hydrogen peroxide in an acidic medium in the presence of at least one alcohol or at least one olefin.

[0084] Preferably, the process for the prepara...

Embodiment 1

[0199] starting mixture

[0200] In the examples below, the mixture treated was a mixture containing 84.6% tert-amyl hydroperoxide, 4% di(tert-amyl)peroxide (DTA), 0.8% acetone, 0.8% tert-amyl alcohol and 0.9% by weight The peroxide 2,2-bis(tert-amylperoxy)propane in tert-amyl hydroperoxide (TAHP) solution.

[0201] Extraction stage a)

[0202] In a closed flask, 500 ml of demineralized water was added to 41.2 g of the above tert-amyl hydroperoxide solution.

[0203] The combined product was mixed for 30 minutes using a magnetic stir bar and then allowed to separate by settling at ambient temperature for a period of 30 minutes.

[0204] After this separation by settling, about 12.5 g of a supernatant organic phase (with interface) and about 528 g of a slightly cloudy lower phase formed.

[0205] Concentration stage b)

[0206] The lower phase was introduced into a rotary evaporator flask.

[0207] The distillation was carried out at a bath temperature of 50° C. at a...

Embodiment 2

[0211] starting mixture

[0212] In the examples below, the treated mixture was a mixture containing 84.6% tert-amyl hydroperoxide, 4% di(tert-amyl)peroxide (DTA), 0.8% acetone, 0.8% tert-amyl alcohol, and 0.9 % by weight peroxide 2,2-bis(tert-amylperoxy)propane in tert-amyl hydroperoxide (TAHP) solution.

[0213] The starting mixture is the same as that of Example 1.

[0214] Extraction stage a)

[0215] In a closed flask, 500 ml of demineralized water was added to 41.2 g of the above tert-amyl hydroperoxide solution.

[0216] The combined product was mixed for 30 minutes using a magnetic stir bar and then allowed to separate by settling at ambient temperature for a period of 60 hours.

[0217] After this separation by settling, about 11.5 g of a supernatant liquid phase and about 526 g of a lower phase were formed.

[0218] Concentration stage b)

[0219] A quantity of 428 g of the lower phase was introduced into the rotary evaporator flask.

[0220] The distilla...

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Abstract

The present invention relates to a method for purifying a mixture containing at least one alkyl hydroperoxide, preferably tert-butyl hydroperoxide or tert-amyl hydroperoxide, and at least one corresponding dialkyl hydroperoxide, said method comprising at least one step of extraction with water and at least one separation step which is carried out within the aqueous phase, obtained following the extraction step, in order to recover an aqueous solution which is rich in alkyl hydroperoxide. The invention also relates to an aqueous composition which is rich in alkyl hydroperoxide and contains at least 0.1% by weight of dialkyl peroxide in relation to the total weight of the composition.

Description

technical field [0001] The present invention relates to a process for purifying a mixture comprising at least one alkyl hydroperoxide, preferably tert-butyl hydroperoxide or tert-amyl hydroperoxide, and at least one dialkyl peroxide, comprising At least one stage of extraction with water and at least one stage of separation carried out on the aqueous phase obtained after said extraction stage, in order to recover an aqueous solution rich in alkyl hydroperoxides. [0002] The present invention also relates to an aqueous composition rich in alkyl hydroperoxides comprising less than 0.1% by weight of dialkyl peroxides relative to the total weight of said composition. Background technique [0003] Alkyl hydroperoxides are usually produced as raw materials: intended for blending with polymers such as polyesters, copolymers of ethylene and vinyl acetate (EVA) and terpolymers of ethylene / propylene / diene monomers (EPDM) or free radical polymerization initiators such as peroxyesters...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/04
CPCC07C407/003C07C409/04B01D3/143B01D11/0492C08K5/14
Inventor P.梅杰A.布卢姆S.哈布B.范赫梅尔里克
Owner ARKEMA FRANCE SA
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