CN115382233A - Cyclohexanone rectification device and method - Google Patents

Cyclohexanone rectification device and method Download PDF

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Publication number
CN115382233A
CN115382233A CN202110571593.7A CN202110571593A CN115382233A CN 115382233 A CN115382233 A CN 115382233A CN 202110571593 A CN202110571593 A CN 202110571593A CN 115382233 A CN115382233 A CN 115382233A
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China
Prior art keywords
tower
cyclohexanone
lightness
column
light component
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CN202110571593.7A
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Chinese (zh)
Inventor
李运岭
刘广恒
张艳
刘华伟
张华强
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Yuncheng Xuyang Energy Co ltd
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SHANDONG HONGDA CHEMICAL CO Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00—Systems containing only non-condensed rings
    • C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/14—The ring being saturated

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a device and a method for rectifying cyclohexanone. The rectifying device comprises: a first lightness-removing column, a second lightness-removing column and a cyclohexanone column, and the rectification apparatus does not comprise a conventional ketone second column. Compared with the rectification device and method of cyclohexanone in the prior art, the rectification device and method of cyclohexanone of the invention omit the ketone second tower, save power consumption 57888 KW/year, save steam 4320 t/year, have controlled the quality of cyclohexanone effectively at the same time.

Description

Cyclohexanone rectification device and method
Technical Field
The invention belongs to the field of chemical engineering, and particularly relates to a cyclohexanone rectification device and method.
Background
In the prior art, as shown in figure 1, crude alcohol ketone produced by oxidation in a cyclohexanone rectification section enters a light first tower C-301a (with the inner diameter of 3000 mm) through a pump, and tower bottom materials are sent to a ketone tower C-303 (with the inner diameter of 4000 mm); the top of the tower is pumped into a light second tower C-302 (the inner diameter is 1000 mm) by a condensing pump, the light second tower C-302 is heated by 1.1MPa steam, the negative pressure distillation is carried out, light components are distilled out, and the light components are pumped into a light oil tank by the condensing pump, namely the light oil. The materials in the bottom of the light second tower are pressurized by a pump and sent into a second ketone tower C-301 (the inner diameter is 2200 mm) to be heated and separated by 1.1MPa steam, the extracted materials from the top of the second ketone tower C-301 are sent into a solvent ketone tank by a condensing pump, the solvent ketone is the solvent ketone, the content of the ketone in the solvent ketone is up to more than 95 percent, and the extracted materials from the bottom of the tower are sent into a ketone tower C-303. The process has high energy consumption, poor product quality and low additional value, namely, the low-price solvent ketone is generated, the yield of the high-price cyclohexanone is reduced, and the consumption is increased. The volume of the light second tower (DN =1000 mm) is too small, so that the index control of light components is influenced, and finally, the light components contained in cyclohexanone products are higher, and the ketone content is influenced.
Therefore, there is a need for a method and an apparatus for controlling the content of light components in cyclohexanone and ensuring the quality of cyclohexanone while reducing energy consumption.
Disclosure of Invention
The invention aims to provide a cyclohexanone rectification device and a method, and the device can improve the yield of cyclohexanone, control the content of light components in the cyclohexanone, save equipment and reduce energy consumption.
In one aspect, the present invention relates to an apparatus for rectifying cyclohexanone, the apparatus comprising:
the first lightness-removing column is provided with a feed inlet and is used for receiving crude alcohol ketone;
the second light component removal tower is connected with the tower top of the first light component removal tower and is used for enabling light components separated from the first light component removal tower to enter the second light component removal tower, and the tower top of the second light component removal tower is connected with a light oil tank;
and the cyclohexanone tower is respectively connected with the tower bottom of the first light component removal tower and the tower bottom of the second light component removal tower and is used for enabling heavy components in tower kettles of the first light component removal tower and the second light component removal tower to respectively enter the cyclohexanone tower, and a cyclohexanone outlet is formed in the tower top of the cyclohexanone tower.
In a specific embodiment, the second light component removal tower can be cylindrical, the inner diameter of the second light component removal tower is 1200-2800mm, and the volume of the second light component removal tower is 52-284m 3 Taking into consideration the index requirement and investment consumption of cyclohexanone in the market, the preferred inner diameter is 2200mm, the height is 48655mm, and the volume is 175.3m 3 。
In a specific embodiment, the top of the first light component removal tower is connected to the second light component removal tower through a first pipeline, and a condenser and a pump are arranged on the first pipeline, and the condenser is located upstream of the pump.
In a specific embodiment, the bottom of the first light component removal tower is connected to the cyclohexanone tower through a second pipeline, the bottom of the second light component removal tower is connected to the cyclohexanone tower through a third pipeline, and the second pipeline and the third pipeline are respectively provided with a pump.
In a specific embodiment, the device further comprises a cyclohexanol tower connected with the bottom of the cyclohexanone tower, and the top of the cyclohexanol tower is provided with a cyclohexanol extraction outlet.
In a specific embodiment, the bottoms of the first light component removal column, the second light component removal column and the cyclohexanone column can be respectively connected with a reboiler.
In another aspect, the present invention provides a method for rectifying cyclohexanone using the above-described rectifying apparatus, the method comprising the steps of:
step 1: crude alcohol ketone enters a first lightness-removing tower through a feed inlet of the first lightness-removing tower by a pump, a bottom material flow of the first lightness-removing tower is sent into a cyclohexanone tower, and a top material flow of the first lightness-removing tower is sent into a second lightness-removing tower;
step 2: feeding the top material flow of the first lightness-removing tower as the feed of a second lightness-removing tower into the second lightness-removing tower, heating the second lightness-removing tower, extracting light components at the top of the second lightness-removing tower into a light oil tank, and sending the bottom material flow of the second lightness-removing tower into a cyclohexanone tower;
and step 3: cyclohexanone was withdrawn from the top of the cyclohexanone column and fed to the cyclohexanone tank.
In a specific embodiment, in step 2, the second lightness-removing column is heated with 1.1MPa steam.
In a specific embodiment, in step 2, the overhead pressure of the second lightness-removing column is-44 to-47 kpa.
In a specific embodiment, in the step 2, the ketone content of the light component at the top of the second lightness-removing column is less than 5 wt%.
In a specific embodiment, in the step 2, the feeding amount of the second light component removal tower is 3-5m 3 In the range of/h.
In a specific embodiment, in step 2, the feed amount of the second light component removal tower is 4.5m 3 /h。
In a specific embodiment, the stream extracted from the bottom of the cyclohexanone tower enters the cyclohexanol tower, and after rectification, cyclohexanol is extracted from the top of the cyclohexanol tower.
Advantageous effects
The application relates to a cyclohexanone rectification device and a method, because compared with a second lightness-removing column in the prior art, a new second lightness-removing column with increased volume and height is used, therefore, by adopting the device, light components are easily evaporated, hexanal + 2-heptanone is also extracted, and simultaneously, because the feeding amount of the second lightness-removing column is also increased, the index of the light components is easily controlled, and the ketone content extracted from the top of the column is correspondingly reduced. The content of ketone at the bottom of the tower is correspondingly improved, the discharge amount is also increased, after the cyclohexanone is sent to the cyclohexanone tower, the steam consumption of the cyclohexanone tower is reduced, meanwhile, the light components in the cyclohexanone extracted by the cyclohexanone tower are relatively low, and the hexanal and the 2-heptanone can be effectively controlled.
The device of the invention does not generate solvent ketone any more, and the solvent ketone is completely converted into cyclohexanone, so that the yield of the cyclohexanone is improved. Compared with a cyclohexanone distillation device in the prior art, the device provided by the application reduces two pumps, also saves a conventional ketone second tower, saves electricity consumption 57888 KW/year, saves steam 4320 t/year, effectively controls the quality of cyclohexanone, controls light components to be about 200ppm, controls hexanal to be 0,2-heptanone to be about 15ppm, and controls the qualification rate of cyclohexanone to be 100%.
Drawings
Fig. 1 shows a schematic diagram of a rectification apparatus for cyclohexanone according to the prior art.
FIG. 2 shows a schematic of a rectification apparatus for cyclohexanone according to example 1 of the present invention.
Description of the reference numerals
C-301: ketone two tower
C-301a: light tower
C-302: light second tower
C-303: ketone tower
1: first lightness-removing tower
2: second lightness-removing tower
3. Cyclohexanone tower
4. Cyclohexanol tower
5. Light oil tank
6. Cyclohexanone tank
7. Cyclohexanol tank
C1, C2, C3, C4: condenser
R1, R2, R3, R4: return channel
P1, P2, P3: pump and method of operating the same
B1, B2, B3, B4: reboiler device
Detailed Description
The technical content of the present invention is explained below by specific examples, which, however, are not intended to limit the scope of the present invention.
Term(s)
In the present application, "crude alcohol ketone" refers to a product produced by the following oxidation process: benzene reacts with hydrogen to produce cyclohexane; cyclohexane reacts with oxygen in the air at a certain temperature and pressure to produce cyclohexyl hydroperoxide, which decomposes in an alkaline environment to produce the crude alcohol ketone, which comprises a mixture of cyclohexanone and cyclohexanol as well as a small amount of cyclohexane, as well as light oils and some heavy components.
In this application, "light oil" comprises n-valeraldehyde, butanol, 2 hexanone, n-pentanol. "heavies" include cyclohexenone, cyclohexane ether, cyclohexanediol, 2-cyclohexylidene cyclohexan-1-one, 2,3-bicyclohexane-one.
The invention relates to a rectification device of cyclohexanone, which comprises:
the first light component removal tower 1 is provided with a feed inlet, and is used for receiving crude alcohol ketone;
a second light component removal tower 2 connected with the top of the first light component removal tower 1 and used for leading the light components separated from the first light component removal tower 1 to enter the second light component removal tower 2, wherein the top of the second light component removal tower 2 is connected with a light oil tank 5;
and the cyclohexanone tower 3 is respectively connected with the tower bottom of the first light component removal tower 1 and the tower bottom of the second light component removal tower 2, and is used for enabling heavy components in tower kettles of the first light component removal tower 1 and the second light component removal tower 2 to respectively enter the cyclohexanone tower 3, and a cyclohexanone outlet is formed in the tower top of the cyclohexanone tower 3.
In a specific embodiment, the second lightness-removing column 2 is cylindrical, the inner Diameter (DN) of the second lightness-removing column is 1200-2800mm, and the volume of the second lightness-removing column is 52-284m 3 Preferably 2200mm in internal diameter, 48655mm in height and 175.3m in volume 3 。
In a specific embodiment, the top of the first light component removal tower 1 is connected to the second light component removal tower 2 through a first pipeline, the first pipeline is provided with a condenser C1, a reflux tank R1 and a pump, and the condenser C1 is located upstream of the pump.
In a specific embodiment, the bottom of the first light and light component removing tower 1 is connected to the cyclohexanone tower 3 through a second pipeline, the bottom of the second light and light component removing tower 2 is connected to the cyclohexanone tower 3 through a third pipeline, and pumps are respectively arranged on the second pipeline and the third pipeline.
In a specific embodiment, the device further comprises a cyclohexanol tower 4 connected to the bottom of the cyclohexanone tower 3, and a cyclohexanol extraction port is arranged at the top of the cyclohexanol tower 4.
In a specific embodiment, the bottoms of the first light component removal column 1, the second light component removal column 2 and the cyclohexanone column 3 are respectively connected with a reboiler.
The invention also relates to a method for rectifying cyclohexanone by using the rectifying device, which comprises the following steps:
step 1: crude alcohol ketone enters a first lightness-removing tower 1 through a feed inlet of the first lightness-removing tower 1, a bottom material flow of the first lightness-removing tower 1 is sent to a cyclohexanone tower 3, and a top material flow of the first lightness-removing tower 1 is sent to a second lightness-removing tower 2;
step 2: after the top stream of the first lightness-removing column 1 is fed into the second lightness-removing column 2 as the feed of the second lightness-removing column 2, the second lightness-removing column 2 is heated, the top light components of the second lightness-removing column 2 are extracted into a light oil tank 5, and the bottom stream of the second lightness-removing column 2 is sent into a cyclohexanone column 3;
and step 3: cyclohexanone was taken from the top of the cyclohexanone column 3 and fed to the cyclohexanone tank 6.
In a specific embodiment, in step 2, the second lightness-removing column 2 is heated with 1.1MPa steam.
In a specific embodiment, in step 2, the overhead pressure of the second lightness-removing column 2 is-44 kpa.
In a specific embodiment, in the step 2, the ketone content of the light component at the top of the second lightness-removing column 2 is less than 5 wt%.
In the specific embodiment, in the step 2, the feeding amount of the second light component removal tower 2 is 3-5m 3 In the range of/h, the feed amount of the second lightness-removing column 2 is preferably 4.5m 3 /h。
In the following embodiments, the detection method of cyclohexanone refers to national standard GB10669-2001, the detection method: gas chromatography normalization. Detection conditions are as follows: capillary column 60 m x 0.32 m x 0.50 m (thickness of tube); the injection port temperature was 280 ℃.
Example 1
As shown in FIG. 2, crude alcohol ketone produced by oxidation is pumped through a feed port (not shown) into a first lightness-removing column 1 (inner diameter of 3000 mm) for separating light oil from alcohol, ketone and heavy components, the bottom stream of the first lightness-removing column 1 is sent into a cyclohexanone column 3 through a second line, and the top stream of the first lightness-removing column 1 is sent into a second lightness-removing column 2 (inner diameter of 2200mm, height of 48655mm, volume of 175.3 m) through a first line 3 The feeding amount is 4.5m 3 H, column head pressureForce-44- — 47kpa, vs. the corresponding prior art light second column C-302 has dimensions of 1000mm (inside diameter) × 46010mm (height) and a volume of 32.5m 3 The feeding amount is 2m 3 H, the pressure at the top of the tower is-55 kpa); heating a second lightness-removing column 2 by using 1.1MPa steam for separating light oil and cyclohexanone, extracting light components at the top of the second lightness-removing column 2 into a light oil tank 5 (wherein the ketone content is 5wt%, and the ketone content extracted at the top of a light second column C-302 in the prior art is 15 wt%), and sending a bottom stream of the second lightness-removing column 2 into a cyclohexanone column 3 (the inner diameter is 4000 mm) through a third pipeline; the cyclohexanone extracted from the top of the cyclohexanone tower 3 enters the cyclohexanone tank 6, the bottom material flow of the cyclohexanone tower 3 enters the cyclohexanol tower 4 through a pipeline, and further, the cyclohexanol extracted from the top of the cyclohexanol tower 4 enters the cyclohexanol tank 7. In the above apparatus, the condenser C1 and the pump are connected to the first line, the reboiler is connected to the bottoms of the first lightness-removing column, the second lightness-removing column and the cyclohexanone column, respectively, and the condenser and the pump are provided in the lines upstream of the light oil tank 5, the cyclohexanone tank 6 and the cyclohexanol tank 7, respectively.
The quality of the cyclohexanone obtained by the device is effectively controlled, and the quality is detected by a gas chromatography normalization method, so that the light component is controlled to be about 200ppm, the hexanal content is 0,2-heptanone content is about 15ppm, and the qualification rate of the cyclohexanone is 100%.
From the results of the above specific examples, it can be seen that the apparatus of the present application, when used for cyclohexanone rectification, achieves the following technical effects: the quality of cyclohexanone is effectively controlled while related devices are reduced and energy consumption is reduced.

Claims (10)

1. An apparatus for rectifying cyclohexanone, the apparatus comprising:
the first light component removal tower is provided with a feed inlet and is used for receiving crude alcohol ketone;
the second light component removal tower is connected with the tower top of the first light component removal tower and is used for enabling light components separated from the first light component removal tower to enter the second light component removal tower, and the tower top of the second light component removal tower is connected with a light oil tank;
and the cyclohexanone tower is respectively connected with the tower bottom of the first light component removal tower and the tower bottom of the second light component removal tower and is used for enabling heavy components in tower kettles of the first light component removal tower and the second light component removal tower to respectively enter the cyclohexanone tower, and a cyclohexanone outlet is formed in the tower top of the cyclohexanone tower.
2. A rectification apparatus according to claim 1, wherein said second lightness-removing column has a cylindrical shape with an inner diameter of 1200 to 2800mm and a volume of 52 to 284m 3 Preferably 2200mm in internal diameter, 48655mm in height and 175.3m in volume 3 。
3. The rectification apparatus according to claim 1, wherein the top of the first lightness-removing column is connected to the second lightness-removing column through a first line, and a condenser and a pump are disposed on the first line, and the condenser is located upstream of the pump.
4. The rectification apparatus according to claim 1, wherein the bottom of the first lightness-removing column is connected to the cyclohexanone column through a second line, the bottom of the second lightness-removing column is connected to the cyclohexanone column through a third line, and pumps are respectively disposed on the second line and the third line.
5. The rectification apparatus according to claim 1, wherein the apparatus further comprises a cyclohexanol column connected to the bottom of the cyclohexanone column, and a cyclohexanol extraction port is provided at the top of the cyclohexanol column.
6. The rectification apparatus according to claim 1, wherein the bottoms of the first light component removal column, the second light component removal column and the cyclohexanone column are respectively connected to a reboiler.
7. A process for the rectification of cyclohexanone using a rectification apparatus as claimed in any one of claims 1 to 6, said process comprising the steps of:
step 1: feeding the crude alcohol ketone into a first lightness-removing tower through a feed inlet of the first lightness-removing tower, feeding a bottom material flow of the first lightness-removing tower into a cyclohexanone tower, and feeding a top material flow of the first lightness-removing tower into a second lightness-removing tower;
step 2: feeding the top material flow of the first lightness-removing tower as the feeding material of a second lightness-removing tower into the second lightness-removing tower, heating the second lightness-removing tower, extracting light components at the top of the second lightness-removing tower into a light oil tank, and sending the bottom material flow of the second lightness-removing tower into a cyclohexanone tower;
and step 3: and collecting the cyclohexanone from the top of the cyclohexanone tower and feeding the cyclohexanone into a cyclohexanone tank.
8. The process of claim 7, wherein in step 2, the second lightness-removing column is heated with 1.1MPa steam.
9. The process of claim 7, wherein in step 2, the overhead pressure of the second lightness-removing column is from-44 to-47 kpa.
10. The method of claim 7, wherein,
in the step 2, the process is carried out,
the ketone content of the light components at the top of the second light component removal tower is less than 5wt%, and/or
The feeding amount of the second light component removal tower is 3-5m 3 In the range of/h, the second lightness-removing column preferably has a feed of 4.5m 3 /h。
CN202110571593.7A 2021-05-25 2021-05-25 Cyclohexanone rectification device and method Pending CN115382233A (en)

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