A kind of aftertreatment method of the tert-butanol containing tert-butyl hydroperoxide

A technology of tert-butyl hydroperoxide and tert-butanol, which is applied in the separation/purification of hydroxy compounds, organic chemistry and other directions, can solve problems such as high energy consumption, and achieve low energy consumption, wide application range and mild reaction conditions. Effect

Active Publication Date: 2019-10-25
北京水木滨华科技有限公司
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  • Abstract
  • Description
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Problems solved by technology

Above-mentioned two kinds of methods all are to operate under high temperature, and energy consumption is big

Method used

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  • A kind of aftertreatment method of the tert-butanol containing tert-butyl hydroperoxide

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[0032] The preparation method of the present invention will be further described in detail below in conjunction with specific examples. It should be understood that the following embodiments are only illustrative and explaining the present invention, and should not be construed as limiting the protection scope of the present invention. All technologies implemented based on the foregoing contents of the present invention are covered by the scope of the present invention.

[0033] The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents and materials used in the following examples, unless otherwise specified, can be obtained from commercial sources.

Embodiment 1

[0035] Into a 1000ml four-necked flask equipped with a thermometer, constant pressure dropping funnel and condenser tube (water bath temperature control), add 190g of sodium sulfite aqueous solution with a concentration of 18.7%, stir, add 39.5g of TBA-TBHP solution into the dropping funnel ( TBHP content 61.8wt%), slowly drip into the sodium sulfite aqueous solution, control the temperature at 50°C, after 30 minutes of dripping, continue to stir for 10 minutes. The temperature was lowered to 30° C., the layering was allowed to stand, and 32 g of tert-butanol was obtained after separation. Gas chromatography showed that neither TBA nor the aqueous phase contained TBHP, and the TBA contained 32% water, and contained no sodium sulfate and sodium sulfite.

Embodiment 2

[0037] Into a 1000ml four-necked flask equipped with a thermometer, constant pressure dropping funnel and condenser tube (water bath temperature control), add 190g of sodium sulfite aqueous solution with a concentration of 18.7%, stir, add TBA-TBHP solution 40g (TBHP) to the dropping funnel Content 50wt%), slowly drip into the sodium sulfite aqueous solution, control the temperature at 50°C, after 30 minutes of dripping, continue to stir for 10 minutes. The temperature was lowered to 30°C, the layering was allowed to stand, and 33.5 g of tert-butanol was obtained after separation. Gas chromatography showed that the TBA and the water phase contained no TBHP, and the TBA contained 31.5% water, and contained no sodium sulfate and sodium sulfite.

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Abstract

The invention belongs to the technical field of butyl alcohol purification, and particularly relates to a post-treatment method of tert butyl alcohol containing tert-butyl hydroperoxide. The method includes the steps: reducing the tert-butyl hydroperoxide into the tert butyl alcohol by sodium sulfite and / or sodium thiosulfate in the reaction process; oxidizing the sodium sulfite and / or sodium thiosulfate into sodium sulfate; rapidly layering the tert butyl alcohol, the sodium sulfate and water solution of optionally-selected and unreacted sodium sulfite and / or sodium thiosulfate at normal temperature. A mixed system containing the tert butyl alcohol and water is positioned on the upper layer, and a mixed system containing the sodium sulfate, water and the optionally-selected and unreactedsodium sulfite and / or sodium thiosulfate is positioned at the lower layer. By the aid of a reaction principle, a mixed system of the tert-butyl hydroperoxide and the tert butyl alcohol is treated, thetert-butyl hydroperoxide in the mixed system can be effectively removed, and refined tert butyl alcohol can be acquired on the premise of ensuring subsequent safety of a reaction system.

Description

Technical field [0001] The invention belongs to the technical field of tert-butanol purification, and specifically relates to a post-treatment method for tert-butanol containing tert-butyl hydroperoxide. Background technique [0002] The production of propylene oxide (PO) began in 1931 with the chlorohydrin method of UCC Company using chlorine gas as the raw material, and then successively developed and industrialized methods are as follows: In 1969, the US Arco Company’s PO with isobutane as raw material / TBA co-oxidation method, PO / SM co-oxidation method with ethylbenzene as raw material in 1977, CHP co-oxidation method with cumene as raw material in 2003, etc. At present, the global production capacity of the chlorohydrin method, PO / TBA co-oxidation method, and PO / SM co-oxidation method totals 90%, which is the mainstream production technology of PO. [0003] Among them, the PO / TBA co-oxidation method using isobutane as a raw material is disclosed in US patent documents US44080...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/12C07C29/74
CPCC07C29/74C07C31/12
Inventor 马敏解淑民郑虓姚春海
Owner 北京水木滨华科技有限公司
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