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System and method for separating out acetonitrile in acetonitrile-water-dicyclopentadiene system

A technology of dicyclopentadiene and dicyclopentadiene tower, which is applied in the field of acetonitrile purification, can solve the problem of inability to separate streams, and achieve the effects of reducing the possibility of decomposition and lowering the operating temperature

Inactive Publication Date: 2014-04-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention is to solve the ACN-H formed in the operation process of the existing acetonitrile method isoprene extraction device 2 The problem that the O-DCPD stream cannot be separated, to make up for the shortcomings of the existing technology, a method for separating acetonitrile in the acetonitrile-water-dicyclopentadiene system is proposed, and then high-purity acetonitrile is obtained, and the recovery rate of acetonitrile is over 99.3%.

Method used

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  • System and method for separating out acetonitrile in acetonitrile-water-dicyclopentadiene system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] After mixing acetonitrile-water-dicyclopentadiene stream 4 (to be refined) and cyclohexane (entrainer) stream 9 (its composition is 88.0% acetonitrile, 2.0% dicyclopentadiene, 7.0% water and 3.0% cyclohexane ) enters the de-dicyclopentadiene tower 1 from the middle, and the de-dicyclopentadiene tower 1 still obtains 97.56% dicyclopentadiene and 2.44% acetonitrile, and the top of the tower obtains acetonitrile, water and cyclohexane stream 6, and its composition is respectively 90.81%, 7.15% and 2.04%. The bottom temperature of tower 1 of the debicyclopentadiene tower is 115.82°C, the temperature at the top of the tower is 29.24°C, the pressure at the top of the tower is 20KPa (absolute), the reflux ratio is 4, and there are 20 theoretical plates.

[0038] The top stream 6 of the de-dicyclopentadiene tower 1 enters the middle part of the dehydration tower 2, and the top of the dehydration tower 2 obtains 25% hexanaphthene and 75% water stream. A part of the cyclohexane ...

Embodiment 2

[0042]Acetonitrile-water-dicyclopentadiene stream 4 (to be refined) and cyclohexane (entrainer) stream 9 are mixed (its composition is acetonitrile 93.03%, dicyclopentadiene 0.9%, water 5.0% and cyclohexane 4.1% ) enters the de-dicyclopentadiene tower 1 from the middle, and the dicyclopentadiene tower 1 tank still obtains 96.29% dicyclopentadiene and 3.71% acetonitrile, and the top of the tower obtains acetonitrile, water and cyclohexane stream 6, and its composition is respectively 87.24%, 4.92% and 7.84%. Dicyclopentadiene tower 1 has a bottom temperature of 113.76°C, a tower top temperature of 34.57°C, a tower top pressure of 40KPa (absolute), a reflux ratio of 3.5, and 23 theoretical plates.

[0043] The top flow of de-dicyclopentadiene tower 1 enters the middle part of dehydration tower 2, and the top of dehydration tower 2 obtains 62.3% cyclohexane and 37.7% water flow. Part of the hexane is used as the reflux of the dehydration tower, and part of it is recycled as the ...

Embodiment 3

[0047] Acetonitrile-water-dicyclopentadiene stream 4 (to be refined) and cyclohexane (entrainer) stream 9 are mixed (its composition is 85.02% of acetonitrile, 4.4% of dicyclopentadiene, 6.90% of water and 3.68% of cyclohexane ) enters the de-dicyclopentadiene tower 1 from the middle, and the de-dicyclopentadiene tower 1 still obtains 97.43% dicyclopentadiene and 2.57% acetonitrile, and the top of the tower obtains acetonitrile, water and cyclohexane stream 6, which consists of They are 88.94%, 7.21% and 3.85% respectively. The bottom temperature of tower 1 of the debicyclopentadiene tower is 116.76°C, the temperature at the top of the tower is 47.93°C, the pressure at the top of the tower is 70KPa (absolute), the reflux ratio is 2.4, and there are 21 theoretical plates.

[0048] The stream at the top of the de-dicyclopentadiene tower 1 enters the middle part of the dehydration tower 2, and the top of the dehydration tower 2 obtains 65.22% hexanaphthene and 34.78% water stream...

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Abstract

The invention provides a system and a method for separating out acetonitrile in an acetonitrile-water-dicyclopentadiene system. The material flow of acetonitrile-water-dicyclopentadiene is converged with the material flow of an entrainer cyclohexane to go into the middle part of a dicyclopentadiene removal tower so that the dicyclopentadiene is removed; under the entraining action of the cyclohexane, the dehydration task is completed by a dehydrating tower, and after layering, the cyclohexane is recycled; and then the material flow of acetonitrile containing little moisture goes into an acetonitrile refining tower. According to the invention, the cyclohexane is introduced into the acetonitrile-water-dicyclopentadiene system, and the acetonitrile is purified by virtue of the azeotropic relationship between materials and based on the oil-water separation principle; and the purity of the acetonitrile is more than 99.5%. As the entrainer cyclohexane is introduced, the azeotropy between water and the acetonitrile and the azeotropy between water and the dicyclopentadiene are broken; and the cyclohexane can be recycled. The refining tower is guaranteed to have a low operating temperature so that the decomposition possibility of the dicyclopentadiene is greatly reduced. Furthermore, the recovery rate of the acetonitrile is ensured.

Description

technical field [0001] The invention relates to a method for refining acetonitrile, in particular to a system and method for separating acetonitrile in an acetonitrile-water-dicyclopentadiene system. Background technique [0002] It is difficult to separate the carbon five components by ordinary distillation. According to the relative volatility of the carbon five components in the mixed solvent of acetonitrile and water, the polymerization can be obtained by ordinary distillation, extractive distillation, analysis, and water washing. Grade isoprene, dicyclopentadiene (DCPD) and piperylene are by-products at the same time. C5 contains active cyclopentadiene, which self-polymerizes to form dicyclopentadiene or even polymerizes due to the high operating temperature in the process of extractive distillation and analysis, so that DCPD, poly polymer and water (H 2 O) content gradually accumulates, seriously affecting the selectivity and extractability of the solvent. In order ...

Claims

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Application Information

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IPC IPC(8): C07C255/03C07C253/34
Inventor 任海伦孙永利张志恒张敬罗铭芳姜斌
Owner TIANJIN UNIV
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