Post-treatment method of tert butyl alcohol containing tert-butyl hydroperoxide

A technology of tert-butyl hydroperoxide and tert-butanol, which is applied in the separation/purification of hydroxyl compounds, organic chemistry, etc., can solve the problems of high energy consumption, achieve low energy consumption, mild reaction conditions, and a wide range of applications Effect

Active Publication Date: 2019-04-05
北京水木滨华科技有限公司
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  • Abstract
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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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  • Post-treatment method of tert butyl alcohol containing tert-butyl hydroperoxide

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[0032] The preparation method of the present invention will be further described in detail in conjunction with specific examples below. It should be understood that the following examples are only for illustrating and explaining the present invention, and should not be construed as limiting the protection scope of the present invention. All technologies realized based on the above contents of the present invention are covered within the scope of protection intended by 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 can be obtained from commercial sources unless otherwise specified.

Embodiment 1

[0035] In the four-neck flask (water bath temperature control) that is equipped with thermometer, constant pressure dropping funnel and condensing tube 1000ml, add 190g concentration and be the sodium sulfite aqueous solution of 18.7%, stir, add TBA-TBHP solution 39.5g in dropping funnel ( TBHP content 61.8wt%), slowly add dropwise to the sodium sulfite aqueous solution, control the temperature at 50° C., and continue stirring for 10 minutes after the dropwise addition is completed in 30 minutes. The temperature was lowered to 30° C., and the layers were left to stand. After separation, 32 g of tert-butanol was obtained. Gas chromatographic detection showed that TBA and the water phase did not contain TBHP, and TBA contained 32% water, and did not contain sodium sulfate and sodium sulfite.

Embodiment 2

[0037] In the four-neck flask (water bath temperature control) that is equipped with thermometer, constant pressure dropping funnel and condenser tube 1000ml, add 190g concentration and be the sodium sulfite aqueous solution of 18.7%, stir, add TBA-TBHP solution 40g (TBHP in dropping funnel) Content 50wt%), slowly added dropwise to the sodium sulfite aqueous solution, the temperature was controlled at 50° C., and after 30 minutes the dropwise addition was completed, the stirring was continued for 10 minutes. The temperature was lowered to 30° C., and the layers were left to stand. After separation, 33.5 g of tert-butanol was obtained. Gas chromatographic detection showed that TBA and the water phase did not contain TBHP, and TBA contained 31.5% water, and did not contain 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 purification of tert-butanol, in particular to a post-treatment method of tert-butanol containing tert-butyl hydroperoxide. Background technique [0002] The production of propylene oxide (PO) began in 1931 with the chlorohydrin method using chlorine gas as the raw material of the UCC company in the United States. Thereafter, the methods for industrialization were developed and industrialized: in 1969, the PO with isobutane as the raw material was developed by the Arco company in the United States. / TBA co-oxidation method, PO / SM co-oxidation method using ethylbenzene as raw material in 1977, CHP co-oxidation method using cumene as raw material in 2003, and so on. At present, the global production capacity of 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 usi...

Claims

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Application Information

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Patent Type & Authority Applications(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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