Production method of cyclohexyl acetate and used reaction rectifying tower

A technology of cyclohexyl acetate and a reactive distillation column, which is applied in the field of preparation of cyclohexyl acetate, can solve the problems of low conversion rate of cyclohexene, slow reaction speed, and inability to fully meet production needs, so as to improve conversion rate and reduce Energy consumption, the effect of reducing equipment investment costs and energy consumption

Active Publication Date: 2015-07-22
河北美邦工程科技股份有限公司
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method is that the conversion rate of cyclohexene is low, the reaction speed is slow, and the filtrate needs to undergo a separate distillation process to obtain cyclohexyl acetate. These many defects make this method unable to fully meet the production needs, and urgently need to be improved.

Method used

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  • Production method of cyclohexyl acetate and used reaction rectifying tower

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Embodiment 1

[0022] The following examples are tests carried out to the present invention under laboratory conditions. The filler is a 4mm metal θ ring, the height of the packing layer in the upper rectifying section is 0.3m, and the height of the packing layer in the lower rectifying section is 0.5m. Of course, the present invention is not limited to the following examples, and changes, modifications, additions or replacements made by those skilled in the art within the essential scope of this patent also belong to the protection scope of this patent.

[0023] Example 1

[0024] Using a sulfonic acid-based ion exchange resin as a catalyst, the feed rate of acetic acid is 1.3kg / h, the feed temperature is 83°C, and the feed pressure is 101kPa. The mixed gas after benzene hydrogenation reaction (mass fraction: cyclohexene 0.341, benzene 0.412, cyclohexane 0.247) The feed rate is 2.465kg / h, the feed temperature is 83°C, the feed pressure is 101kPa, and the cyclohexene and acetic acid are coun...

Embodiment 2

[0026] Using a sulfonic acid-based ion exchange resin as a catalyst, the feed rate of acetic acid is 1.3kg / h, the feed temperature is 83°C, and the feed pressure is 101kPa. The mixed gas after benzene hydrogenation reaction (mass fraction: cyclohexene 0.341, benzene 0.412, cyclohexane 0.247) The feed rate is 2.465kg / h, the feed temperature is 83°C, the feed pressure is 101kPa, and the cyclohexene and acetic acid are countercurrently contacted and reacted on the surface of the solid catalyst. The reactive distillation column is operated under normal pressure, the reflux ratio R=0.64, and the circulation volume of side line extraction is 0.642kg / h. The output of liquid at the bottom of the tower is 1.347kg / h, the molar fraction of cyclohexyl acetate is 0.9411, the molar fraction of acetic acid is 0.0589, and hardly contains benzene, cyclohexane and cyclohexene; the output of the tower top is 2.418kg / h, and the The molar fraction of hexene was 0.0303, the molar fraction of acetic...

Embodiment 3

[0028] Using a sulfonic acid-based ion exchange resin as a catalyst, the feed rate of acetic acid is 1.3kg / h, the feed temperature is 83°C, and the feed pressure is 101kPa. The mixed gas after benzene hydrogenation reaction (mass fraction: cyclohexene 0.341, benzene 0.412, cyclohexane 0.247) The feed rate is 2.465kg / h, the feed temperature is 83°C, the feed pressure is 101kPa, and the cyclohexene and acetic acid are countercurrently contacted and reacted on the surface of the solid catalyst. The reactive distillation column is operated under normal pressure, the reflux ratio R=0.64, and the circulation volume of the side line is 1.22kg / h. The output of liquid at the bottom of the tower is 1.203kg / h, the molar fraction of cyclohexyl acetate is 0.9957, the molar fraction of acetic acid is 0.0043, and hardly contains benzene, cyclohexane and cyclohexene; the output of the tower top is 2.562kg / h, and the cyclohexyl acetate The molar fraction of hexene is 0.0267, the molar fraction...

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Abstract

The invention discloses a production method of cyclohexyl acetate and a used catalytic reaction rectifying tower. The structure of the catalytic reaction rectifying tower for producing cyclohexyl acetate comprises a main tower, a reboiler, a condenser and a cooler; the main tower internally comprises two rectifying sections, a stripping section, a reaction section, a liquid phase distributor and a gas phase distributor. An operation method comprises the steps: under a normal pressure, acetic acid is fed into the reaction section from a feed inlet on the upper part of the reaction section, and products of partial hydrogenation of benzene are directly fed into the reaction section in a gas phase or a liquid phase from an feed inlet on the lower part of the reaction section without separation treatment; cyclohexene and acetic acid in the reaction section are in inverse contact on a catalyst surface, so as to complete an esterification reaction; and the reaction product is cyclohexyl acetate and is discharged from the tower bottom along downstream of the main tower, unreacted acetic acid is extracted from a side line between the stripping section and the second rectifying section and returns to the acetic acid feed inlet to continue to participate in the esterification reaction, and a little of unreacted cyclohexene and the partial hydrogenated products benzene and cyclohexane which do not participate in the reaction are extracted from the tower top of the main tower.

Description

technical field [0001] The present invention relates to cyclohexyl acetate preparation technology, specifically relate to a kind of preparation method that is used to produce cyclohexyl acetate and the used reactive distillation column thereof. Background technique [0002] CN102875371A discloses a preparation method of cyclohexyl acetate, which uses cyclohexene and acetic acid to undergo a synthesis reaction under the action of a catalyst sulfonic acid-based cation exchange resin, filters after the reaction, recycles the catalyst, and distills the filtrate at atmospheric pressure to collect cyclohexyl acetate Esters, the yield can reach 89%. This preparation method has the low conversion rate of cyclohexene, slow reaction speed, and the filtrate needs to undergo a separate distillation process to obtain cyclohexyl acetate. These many defects lead to the method not being able to fully meet the production needs, and urgently need improvement. Contents of the invention [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/04C07C67/54B01D3/14B01J8/02
CPCB01D3/009B01D3/14B01J8/02C07C67/04C07C67/54C07C2601/14C07C69/14
Inventor 张旭斌李进廖洪王富民金作宏张玉新尹更昌高文杲
Owner 河北美邦工程科技股份有限公司
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