CN108440246A - A kind of separation method of the tert-butyl alcohol - Google Patents

A kind of separation method of the tert-butyl alcohol Download PDF

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Publication number
CN108440246A
CN108440246A CN201810154538.6A CN201810154538A CN108440246A CN 108440246 A CN108440246 A CN 108440246A CN 201810154538 A CN201810154538 A CN 201810154538A CN 108440246 A CN108440246 A CN 108440246A
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China
Prior art keywords
tert
butyl alcohol
butyl
butyl peroxide
extractant
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CN201810154538.6A
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Chinese (zh)
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CN108440246B (en
Inventor
纪红兵
周贤太
刘明
王结祥
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Huizhou Research Institute of Sun Yat Sen University
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Huizhou Research Institute of Sun Yat Sen University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation

Abstract

The invention discloses a kind of separation methods of the tert-butyl alcohol.The tert-butyl alcohol present in synthesis technology of this method for the tert-butyl alcohol forms the problem of azeotropic mixture is difficult to detach with di-tert-butyl peroxide, by the way that extractant is added, realizes efficiently separating for the tert-butyl alcohol.After separating-purifying, the purity of the tert-butyl alcohol is up to 95% or more, and di-tert-butyl peroxide purity is up to 99% or more.It is an advantage of the invention that using continuous extraction rectificating method separating tert-butanol and di-tert-butyl peroxide, separative efficiency is high, and high income is simple for process.

Description

A kind of separation method of the tert-butyl alcohol
Technical field
The invention belongs to the processes of chemical separation process, specifically, being the isolation technics for being related to the tert-butyl alcohol.
Background technology
The tert-butyl alcohol also known as 2- methyl-2-propanols are a kind of very important chemicals.Its chemical industry purposes is extremely extensive, It is used frequently as fuel oil additive, anti-knock agent, organic solvent, synthetic drug or fragrance and prepares the raw material of isobutene.Patent CN 104402675A disclose a kind of method that bionic catalysis iso-butane selective oxidation prepares the tert-butyl alcohol, in the synthesis technology Main by-product is di-tert-butyl peroxide.Di-tert-butyl peroxide easily forms azeotropic mixture with the tert-butyl alcohol, such as straight Row rectifying separation is tapped into, necessarily causes separating effect bad, tert-butyl alcohol yield is low.
Since the tert-butyl alcohol is water-miscible, when carrying out tert-butyl alcohol separation, mostly selection water by the tert-butyl alcohol from mixed It closes and is extracted in object, then carry out separation of extractive distillation.CN 1621399A, CN 1887834A, CN 104383711A etc. are open For the extraction rectification technique for the azeotropic mixture that the tert-butyl alcohol is formed with water, but these separating technologies are not all suitable for tertiary fourth The separation of alcohol and di-tert-butyl peroxide.
To realize being kept completely separate for the tert-butyl alcohol and di-tert-butyl peroxide in tert-butyl alcohol synthesis technology, a kind of separation is developed The continuous extraction rectificating method of the tert-butyl alcohol and di-tert-butyl peroxide, for realizing that tert-butyl alcohol industrialization has important meaning Justice.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of separative efficiency height, the high tert-butyl alcohols of purity Separation method.
To achieve the above object, the technical solution adopted by the present invention is:
Extractant is added in the mixed liquor of the tert-butyl alcohol and di-tert-butyl peroxide, the extraction in a kind of separation method of the tert-butyl alcohol The azeotropic mixture that ring is formed between the two can be broken by taking agent, then realize dividing completely for the tert-butyl alcohol and di-tert-butyl peroxide by rectifying From.
In above-mentioned separation method, preferably, the extractant is one in ethylbenzene, n-butyl ether, n-amylether Kind.
In above-mentioned separation method, preferably, the mass ratio of the extractant and mixture is 0.5 ~ 10:1.
Compared with prior art, the present invention has the advantages that:The method separating tert-butanol and two tertiary fourths of the present invention Base peroxide, after separating-purifying, the purity of the tert-butyl alcohol up to 95% or more, di-tert-butyl peroxide purity up to 99% with On.It is an advantage of the invention that using continuous extraction rectificating method separating tert-butanol and di-tert-butyl peroxide, separative efficiency is high, High income, it is simple for process.
Specific implementation mode
The present invention is illustrated with following embodiment, but the present invention is not limited to the following embodiments.By three embodiments, to this The there is provided method of invention is further described.
Embodiment 1
The method of the present invention is used for the separation process of the tert-butyl alcohol and di-tert-butyl peroxide.The tert-butyl alcohol and di-tert-butyl peroxide The treating capacity of object mixed liquor is 150 kg/h, and wherein the mass fraction of the tert-butyl alcohol is 80%, the quality point of di-tert-butyl peroxide Number is 20%;Extractant is n-butyl ether, mixed liquor and extractant it is preheated after obtained after rectifying detaches into extractive distillation column The tert-butyl alcohol product purity arrived is 97.21 wt%, and di-tert-butyl peroxide product purity is 99.51 wt%.
Embodiment 2
The method of the present invention is used for the separation process of the tert-butyl alcohol and di-tert-butyl peroxide.The tert-butyl alcohol and di-tert-butyl peroxide The treating capacity of object mixed liquor is 150 kg/h, and wherein the mass fraction of the tert-butyl alcohol is 70%, the quality point of di-tert-butyl peroxide Number is 30%.Extractant is n-butyl ether, mixed liquor and extractant it is preheated after obtained after rectifying detaches into extractive distillation column The tert-butyl alcohol product purity arrived is 95.45 wt%, and di-tert-butyl peroxide product purity is 99.03 wt%.
Embodiment 3
The method of the present invention is used for the separation process of the tert-butyl alcohol and di-tert-butyl peroxide.The tert-butyl alcohol and di-tert-butyl peroxide The treating capacity of object mixed liquor is 150 kg/h, and wherein the mass fraction of the tert-butyl alcohol is 75%, the quality point of di-tert-butyl peroxide Number is 25%.Extractant is n-butyl ether, mixed liquor and extractant it is preheated after obtained after rectifying detaches into extractive distillation column The tert-butyl alcohol product purity arrived is 96.26wt%, and di-tert-butyl peroxide product purity is 99.03wt%.

Claims (3)

1. a kind of separation method of the tert-butyl alcohol, it is characterised in that:Add in the mixture of the tert-butyl alcohol and di-tert-butyl peroxide Enter extractant, which can destroy the azeotropic mixture formed between the two, to realize the tert-butyl alcohol and two by the method for rectifying Tert-butyl peroxide is kept completely separate.
2. separation method as described in claim 1, which is characterized in that the extractant is in ethylbenzene, n-butyl ether, n-amylether One kind.
3. separation method as described in claim 1, which is characterized in that the mass ratio of the extractant and mixture be 0.5 ~ 10:1.
CN201810154538.6A 2018-02-23 2018-02-23 Separation method of tert-butyl alcohol Active CN108440246B (en)

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CN201810154538.6A CN108440246B (en) 2018-02-23 2018-02-23 Separation method of tert-butyl alcohol

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CN201810154538.6A CN108440246B (en) 2018-02-23 2018-02-23 Separation method of tert-butyl alcohol

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CN108440246B CN108440246B (en) 2021-06-25

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114763333A (en) * 2021-01-15 2022-07-19 万华化学集团股份有限公司 Separation and recovery method of peroxide TBHP and byproduct TBA in styrene oxide mother liquor

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4810809A (en) * 1986-12-23 1989-03-07 Texaco Inc. Ditertiary butyl peroxide recovery
US5312998A (en) * 1993-06-10 1994-05-17 Arco Chemical Technology, L.P. Integrated process for the production of ditertiary butyl peroxide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4810809A (en) * 1986-12-23 1989-03-07 Texaco Inc. Ditertiary butyl peroxide recovery
US5312998A (en) * 1993-06-10 1994-05-17 Arco Chemical Technology, L.P. Integrated process for the production of ditertiary butyl peroxide

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114763333A (en) * 2021-01-15 2022-07-19 万华化学集团股份有限公司 Separation and recovery method of peroxide TBHP and byproduct TBA in styrene oxide mother liquor
CN114763333B (en) * 2021-01-15 2023-05-26 万华化学集团股份有限公司 Separation and recovery method of peroxide TBHP and byproduct TBA in epoxy phenylethane mother liquor

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