Method for refining sec-butyl acetate coarse products through dual-reflux and preparation method of sec-butyl acetate

A technology for sec-butyl acetate and crude products, which is applied in the field of preparation of sec-butyl acetate, can solve problems such as insufficient material exchange, improper operation, and unguaranteed purity of sec-butyl acetate, and achieve sufficient material transfer and improved The effect of purity

Active Publication Date: 2012-07-18
HUIZHOU YUSSEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yet, in above-mentioned patent application, entrainer (namely water) is with containing C 8 The olefin and the oil phase product of sec-butyl acetate are added to the azeotropic rectification column together, so that the material exchange between the entrainer water and the feed material is insufficient, so that the purity of sec-butyl acetate cannot be guaranteed
In addition, in the above patent application, water is added in liquid form. Due to the phase change, a large amount of heat needs to be provided by the tower kettle. Improper operation can easily lead to water falling, causing the water content in the sec-butyl acetate product to exceed the standard.

Method used

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  • Method for refining sec-butyl acetate coarse products through dual-reflux and preparation method of sec-butyl acetate
  • Method for refining sec-butyl acetate coarse products through dual-reflux and preparation method of sec-butyl acetate
  • Method for refining sec-butyl acetate coarse products through dual-reflux and preparation method of sec-butyl acetate

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preparation example Construction

[0042] According to another aspect of the present invention, the present invention also provides a kind of preparation method of sec-butyl acetate, the method comprises the following steps:

[0043] (1) In the presence of a catalyst and under addition reaction conditions, make C 4 Contact reaction of alkenes with acetic acid;

[0044] (2) separate unreacted C from the reaction product obtained in step (1) 4 Olefins, obtained containing sec-butyl acetate, C 5 A mixture of the above hydrocarbons and unreacted acetic acid;

[0045] (3) by azeotropic distillation from said containing sec-butyl acetate, C 5 Separate acetic acid in the mixture of above hydrocarbon and unreacted acetic acid, obtain sec-butyl acetate crude product;

[0046] (4) According to the method for refining sec-butyl acetate by double reflux provided by the invention, refine sec-butyl acetate from the crude product of sec-butyl acetate.

[0047] According to the preparation method of the sec-butyl acetate ...

Embodiment 1

[0055] This embodiment is used to illustrate the method for refining the crude product of sec-butyl acetate by double reflux and the preparation method of sec-butyl acetate provided by the present invention.

[0056] (1) Preparation of sec-butyl acetate crude product

[0057] With 100 grams of strongly acidic ion exchange resin catalyst (sulfonated styrene-divinylbenzene type resin, specific surface area 30m 2 / g, average particle diameter is 1.0mm, pore volume 0.25mL / g) is loaded in the fixed-bed reactor (φ 32 * 4 * 1000mm), acetic acid is passed in the fixed-bed reactor continuously with the speed of 1000 grams / hour, Will C 4 Olefin mixture (mass composition: n-butane 36.2%, trans-butene 39.5%, n-butene 4.2%, cis-butene 20.1%) was continuously fed into the fixed-bed reactor at a speed of 800 g / hour. Circulating water with a temperature of 80° C. was passed into the jacket of the reactor to control the reaction temperature, and the gauge pressure of the system was controlle...

Embodiment 2

[0080] This embodiment is used to illustrate the method for refining the crude product of sec-butyl acetate by double reflux and the preparation method of sec-butyl acetate provided by the present invention.

[0081] (1) Preparation of sec-butyl acetate crude product

[0082] With 100 grams of strongly acidic ion exchange resin catalyst (sulfonated styrene-divinylbenzene type resin, specific surface area 30m 2 / g, average particle diameter is 1.0mm, pore volume 0.25mL / g) is loaded in the fixed-bed reactor (φ 32 * 4 * 1000mm), acetic acid is passed in the fixed-bed reactor continuously with the speed of 900 grams / hour, Will C 4Olefin mixture (mass composition: isobutane 39.0%, n-butane 9.7%, trans-butene 20.1%, n-butene 17.5%, butene 13.7%) is continuously fed into the fixed-bed reactor at a speed of 800 g / hour middle. Circulating water with a temperature of 80° C. was passed into the jacket of the reactor to control the reaction temperature, and the gauge pressure of the sy...

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Abstract

The invention provides a method for refining sec-butyl acetate coarse products through dual-reflux and a preparation method of sec-butyl acetate comprising the refining process. The refining method of the sec-butyl acetate coarse products comprises (1) enabling the sec-butyl acetate coarse products to feed in a rectifying tower through a first feed port, enabling the water to feed in the rectifying tower through a second feed port in a water vapor mode, conducting azeotropy rectification under operation conditions of the azeotropy rectification, and obtaining mixture mainly containing water and impurities from a tower top; and (2) cooling the mixture, conducting oil-water separation to obtain the water phase and the oil phase, enabling reflux maters at least containing partial oil phase to flow back the rectifying tower, enabling at least partial water phase to form the water vapor and returning the water vapor to return and add in the rectifying tower from a third feed port. The second feed port and the third feed port are same or different, and both located at the position of 1-10 tower boards or theoretical tower boards below the first feed port. The method can be used for preparing the sec-butyl acetate with high purity.

Description

technical field [0001] The invention relates to a method for refining a crude sec-butyl acetate product through double reflux, and a preparation method for sec-butyl acetate. Background technique [0002] Second-butyl acetate, also known as second-butyl acetate and second-butyl acetate, is one of the four isomers of butyl acetate. It is a colorless, flammable, fruity liquid. Performance is similar in most cases and can dissolve a wide variety of resins and organics. Its boiling point is lower than that of commonly used n-butyl ester and isobutyl ester, and its evaporation rate is faster. It can be widely used as solvent, reaction medium, extractant component, metal cleaning agent, fruit fragrance, etc., and can also be used in the pharmaceutical industry. Especially in recent years, due to increasingly stringent environmental protection requirements, the use of toxic solvents such as benzene, toluene, and chlorinated hydrocarbons has been restricted, and the amount of envi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C67/54C07C67/04
Inventor 胡先念
Owner HUIZHOU YUSSEN CHEM CO LTD
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