High-purity tert-butyl alcohol online recovery technology for continuously producing potassium tert-butoxide

Abstract

The invention discloses a high-purity tert-butyl alcohol online recovery technology for continuously producing potassium tert-butoxide. The high-purity tert-butyl alcohol online recovery technology comprises the following operation steps: S401) transferring a heavy-phase separation liquid in a settling tank into a tert-butyl alcohol rectifying tower through a tert-butyl alcohol recovery pump; S402) evaporating and rectifying tert-butyl alcohol in the heavy-phase separation liquid under the heating action of the tert-butyl alcohol rectifying tower to form a tert-butyl alcohol gas phase of whichthe purity is not lower than 80%, extracting the tert-butyl alcohol gas phase from the tower top of the tert-butyl alcohol rectifying tower, and extracting purified water of which the purity is not lower than 99% from the tower bottom of the tert-butyl alcohol rectifying tower; and S403) cooling the tert-butyl alcohol gas phase extracted in step S4020), allowing the cooled tert-butyl alcohol gasphase to enter the settling tank, and allowing a mixed solution of tert-butyl alcohol and cyclohexane to form a light-phase separation solution of the settling tank under the settling separation action of the light phase and the heavy phase of the settling tank. The online recovery technology realizes clean, environment-friendly, efficient, continuous and stable production process of potassium tert-butoxide, no excess material is consumed in the whole production process, and no waste water or waste residues are generated.

Description

technical field [0001] The invention belongs to the preparation technology of potassium tert-butoxide, in particular to an on-line recovery process of high-purity tert-butanol for continuous production of potassium tert-butoxide. Background technique [0002] Potassium tert-butoxide is an important organic base, which is much more basic than sodium hydroxide and potassium hydroxide. Due to (CH 3 ) 3 The inductive effect of CO-three methyl groups makes it more basic and active than other potassium alkoxides, so it is a good catalyst and is widely used in various organic synthesis fields such as chemical industry, medicine, and pesticides In, for example, transesterification, condensation, rearrangement, polymerization, ring opening and preparation of heavy metal orthoesters, etc. Specifically, potassium tert-butoxide can be used to catalyze Michael addition reaction, Pinacol rearrangement reaction and Ramberg-Backlund rearrangement reaction, to prepare condensing agent of ...

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Problems solved by technology

[0003] At present, the mainstream method for domestic manufacturers to produce potassium tert-butoxide is to use tert-butanol to react with potassium metal, which requires the use of a large amount of active potassium metal, which is poor in safety, has a risk of explosion, and is not easy to transport and store

At the same time, metal potassium is expensive, making the production cost higher

[0004] Potassium tert-butoxide is also prepared by using potassium hydroxide aqueous solution and tert-butanol as the reaction raw materials. However, due to the dissolution and ionization equilibrium of the tert-butanol-potassium hydroxide-water system, it is a strongly reversible reaction system, which cannot spontaneously change from hydrogen to hydrogen. Potassium oxide is converted into potassium tert-butoxide, otherwise potassium tert-butoxide will react immediately to form potassium hydroxide when it meets water, and water must be removed from the system quickly

In order to solve this technical problem, there is a technical route for producing potassium tert-butoxide by azeotropic reaction rectification. The process of combining reaction and azeotropic distillation on the interface and a packed column with a large specific surface area are used as a process route for the preparation of potassium tert-butoxide. The technical difficulties of online recycling have led to the failure of this technical route to be widely used

In order to solve the technical problem of on-line recovery in the technical route of producing potassium tert-butoxide by azeotropic reaction distillation, it is usually necessary to enter the third component to realize the recovery of water in the reaction system and the problem of high energy consumption for recovery. The announcement number is CN206033617U The utility model patent proposed a production device of potassium tert-butoxide, including: a reaction kettle, which is connected to the pervaporation membrane separation unit through a delivery pump and a heater in turn; the intercepting side of the pervaporation membrane separation unit The outlet is connected to the reaction kettle; the permeate side of the pervaporation membrane separation unit is equipped with a vacuum pump and a permeate condenser, and the outlet of the permeate condenser is also connected with a permeate tank and a permeate pump; the process requires a pervaporation membrane High, need to face the problem of frequent replacement and maintenance, resulting in low production efficiency and further increase in production costs

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