CN112299980B - Method and system for separating and purifying mixed valeraldehyde - Google Patents

Method and system for separating and purifying mixed valeraldehyde Download PDF

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Publication number
CN112299980B
CN112299980B CN202011080079.5A CN202011080079A CN112299980B CN 112299980 B CN112299980 B CN 112299980B CN 202011080079 A CN202011080079 A CN 202011080079A CN 112299980 B CN112299980 B CN 112299980B
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valeraldehyde
rectifying tower
carbon
mixed
rectifying
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CN112299980A (en
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蒋志魁
王志军
刘洪伟
孙乙淋
马智超
贺雪军
于耀添
鲍柏松
齐洪敏
李志光
孙高攀
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China Shenhua Coal to Liquid Chemical Co Ltd
Shenhua Baotou Coal Chemical Industry Co Ltd
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China Shenhua Coal to Liquid Chemical Co Ltd
Shenhua Baotou Coal Chemical Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C47/00Compounds having —CHO groups
    • C07C47/02Saturated compounds having —CHO groups bound to acyclic carbon atoms or to hydrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives
    • C07C45/81Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C45/82Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

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  • 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 the field of mixed valeraldehyde production, and discloses a method and a system for separating and purifying mixed valeraldehyde. The method comprises the following steps: (1) Heating and rectifying the mixed valeraldehyde to obtain refined valeraldehyde and light components; wherein the heating and rectifying conditions comprise: the pressure at the top of the rectifying tower is 0.3-1MPa, the temperature at the bottom of the rectifying tower is 150-160 ℃, and the temperature at the top of the rectifying tower is 50-60 ℃; the reflux ratio of the mixed valeraldehyde rectifying tower is 5-10; (2) Sequentially cooling and separating the light components to obtain wastewater and a carbon-carbon mixture; (3) Returning a portion of the carbon-four mixture as a recycle to the heated rectification in step (1). The mixed valeraldehyde is separated and extracted, and the purity of the obtained refined valeraldehyde can reach more than 99 weight percent.

Description

Method and system for separating and purifying mixed valeraldehyde
Technical Field
The invention relates to the field of mixed valeraldehyde production, in particular to a method and a system for separating and purifying mixed valeraldehyde.
Background
The production of mixed valeraldehyde products from mixed C4 is a process technology which has become industrialized in recent years. At present, only three industrial production devices are used in China, and the capacity is less than 30 ten thousand tons. The technological process is to mix C4 with synthetic gas (H) 2 And CO) as raw materials, and generating a mixed valeraldehyde product through a carbonylation reaction under the action of rhodium and a ligand catalyst. Further, the mixed valeraldehyde is subjected to condensation and hydrogenation reactions to produce a 2-propyl heptanol product.
In the production process of the mixed valeraldehyde, the existing production process and device can not realize the high-purity production of the mixed valeraldehyde product, thereby affecting the economy and safety of the device. Thus, there is a need for a process for the production of mixed valeraldehyde that achieves improved purity of the mixed valeraldehyde product.
Disclosure of Invention
The invention aims to improve the product purity of mixed valeraldehyde obtained by the prior art, and provides a method and a system for separating and purifying the mixed valeraldehyde and a method for producing 2-propyl heptanol.
In order to achieve the above object, the first aspect of the present invention provides a method for separating and purifying mixed valeraldehyde, comprising:
(1) Heating and rectifying the mixed valeraldehyde to obtain refined valeraldehyde and light components; wherein the heating and rectifying conditions comprise: the pressure at the top of the rectifying tower is 0.3-1MPa, the temperature at the bottom of the rectifying tower is 150-160 ℃, and the temperature at the top of the rectifying tower is 50-60 ℃; the reflux ratio of the mixed valeraldehyde is 5-10;
(2) Sequentially cooling and separating the light components to obtain wastewater and a carbon-carbon mixture;
(3) Returning a portion of the carbon-four mixture as a recycle to the heated rectification in step (1).
In a second aspect, the present invention provides a system for separating and purifying mixed valeraldehyde, which comprises:
the rectifying tower is used for heating and rectifying the mixed valeraldehyde to obtain refined valeraldehyde at the bottom of the tower and obtain light components at the top of the tower;
the reboiler is communicated with the bottom of the rectifying tower and is used for increasing the temperature of the mixed valeraldehyde;
the cooler is communicated with the top of the rectifying tower and is used for cooling the light components to obtain a cooled material flow; and
the liquid return tank is communicated with the cooler and is used for separating the cooled material flow to obtain wastewater and a carbon-carbon mixture;
a reflux pipeline is arranged between the liquid return tank and the top of the rectifying tower and is used for refluxing a part of the carbon-four mixture to the top of the rectifying tower;
the liquid return tank comprises: internally disposed coalescers and baffles, and externally disposed dewatering packages and automatic water cut controls.
Through the technical scheme, the mixed valeraldehyde is separated and extracted, and the purity of the obtained refined valeraldehyde reaches over 99 weight percent.
Drawings
FIG. 1 is a schematic diagram of a method and system for separating and purifying mixed valeraldehyde provided by the invention;
FIG. 2 is a schematic diagram of a prior art method and system for the separation and purification of mixed valeraldehyde.
Description of the reference numerals
1. Rectifying tower 2, reboiler 3 and cooler
4. Liquid return tank 5, preprocessor 6 and coalescer
7. Baffle 8, dewatering bag 9, liquid return pump
10. Blind plate 11, double valve
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The first aspect of the present invention provides a method for separating and purifying mixed valeraldehyde, as shown in fig. 1, comprising:
(1) Heating and rectifying the mixed valeraldehyde to obtain refined valeraldehyde and light components; wherein the heating and rectifying conditions comprise: the pressure at the top of the rectifying tower is 0.4-1MPa, the temperature at the bottom of the rectifying tower is 150-160 ℃, and the temperature at the top of the rectifying tower is 50-60 ℃; the reflux ratio of the mixed valeraldehyde is 5-10;
(2) Sequentially cooling and separating the light components to obtain wastewater and a carbon-carbon mixture;
(3) Returning a portion of the carbon-four mixture as a recycle to the heated rectification in step (1).
In the invention, the effective separation of the light components is combined, the heating and rectifying conditions are allowed to be better adjusted, the effective extraction of the valeraldehyde from the mixed valeraldehyde is realized, and the purity of the product is improved.
In some embodiments of the present invention, the heating and rectifying conditions further preferably include: the pressure at the top of the rectifying tower is 0.3-0.5MPa, the temperature at the bottom of the rectifying tower is 153-158 ℃, and the temperature at the top of the rectifying tower is 50-53 ℃; the reflux ratio of the mixed valeraldehyde is 6-8. In the present invention, the thermal rectification is carried out in a rectifying column. Furthermore, the temperature of the bottom of the rectifying tower can be increased by using a reboiler, and the heating rectification is controlled under the conditions, so that the purity of the obtained refined valeraldehyde can be improved.
In the present invention, the light components are more efficiently separated from the mixed valeraldehyde by the thermal rectification, and then efficiently treated by combining the steps (2) and (3) in the method provided by the present invention, achieving the purpose of improving the purity of the obtained refined valeraldehyde. The mixed valeraldehyde contains valeraldehyde 60-80 wt%, water 0.5-1.5 wt% and carbon four mixture 10-30 wt%. Wherein the valeraldehyde comprises various isomers. The refined valeraldehyde obtained by the method provided by the invention has a valeraldehyde content of 99 wt% or more. The mixed valeraldehyde can be an intermediate product obtained in the production process of 2-propyl heptanol, or a valeraldehyde product or an intermediate valeraldehyde product produced by taking mixed C4 as a raw material.
In some embodiments of the present invention, a portion of the carbo-tetra mixture is refluxed to step (1), preferably the weight ratio of the recovery liquid to the mixed valeraldehyde is from 0.7 to 1.25. Is beneficial to improving the purity of the obtained refined valeraldehyde.
In a second aspect, the present invention provides a system for separating and purifying mixed valeraldehyde, in which a preferred embodiment is shown in fig. 1, comprising:
the rectifying tower 1 is used for heating and rectifying the mixed valeraldehyde to obtain refined valeraldehyde at the bottom of the tower and obtain light components at the top of the tower;
a reboiler 2 which is communicated with the bottom of the rectifying tower and is used for increasing the temperature of the mixed valeraldehyde;
the cooler 3 is communicated with the top of the rectifying tower and is used for cooling the light components to obtain a cooled material flow; and
the liquid return tank 4 is communicated with the cooler and is used for separating the cooled material flow to obtain wastewater and a carbon-carbon mixture;
a reflux pipeline is arranged between the liquid return tank and the top of the rectifying tower and is used for refluxing a part of the carbon-four mixture to the top of the rectifying tower;
the liquid return tank comprises: internally disposed coalescers 6 and baffles 7, and externally disposed dewatering packages 8 and automatic water cut control.
In some embodiments of the invention, the return tank is configured to separate the cooled stream into a water and carbon four mixture.
The rectifying tower is arranged to be vertically placed. The middle part of the tower is provided with a mixed valeraldehyde feeding port. The tower top is provided with a light component discharge port, and the tower bottom is provided with a refined valeraldehyde discharge port. Feeding the mixed valeraldehyde into the rectifying tower to be heated and rectified, discharging light components from the top of the rectifying tower, and discharging refined valeraldehyde without the light components from the bottom of the rectifying tower. And a structure is arranged in the rectifying tower to meet the rectification requirement of the mixed valeraldehyde. The reboiler heats the material obtained at the bottom of the tower in a mode of indirect heat exchange with external steam, so that the light components can be more fully separated. The invention can improve and control the temperature of the bottom of the rectifying tower in the rectifying tower by improving the temperature of steam in the reboiler.
The cooler may be a tubular indirect heat exchanger, cooling the temperature of the light components to facilitate separation of the cooled stream in a subsequent return liquid tank.
In some embodiments of the present invention, it is preferable that the coalescer and the baffle are horizontally spaced in the return tank to horizontally divide the interior of the return tank into a liquid collection zone, a water collection and drainage zone, and a carbon four collection zone.
In some embodiments of the invention, preferably, the coalescer occupies the entire cross section of the return tank, and the baffle occupies a part of the cross section of the return tank.
In some embodiments of the present invention, preferably, the dewatering drum is disposed below the return tank and is communicated with the water collecting and draining region.
In the present invention, the liquid-receiving zone collects the cooled stream. The coalescer accelerates the coalescence of the water and carbon-carbon mixture in the cooled stream to accumulate in said water collection and drainage region. Because the density of each of the water and carbon four mixtures is different, the water is in the lower layer and can be collected in the dewatering package. The carbon four mixture is on the upper layer. When the collected water and carbon four mixture is enough and the liquid level exceeds the height of the baffle, the upper carbon four mixture flows into the carbon four collecting area to realize separation to obtain the water and carbon four mixture, and the water is prevented from flowing back to the rectifying tower. As shown in fig. 1, the return tank can be arranged horizontally, and the coalescer and the baffle plate are arranged perpendicular to the axis of the return tank. The height of the baffle can be more than 2/3 of the diameter of the liquid return tank. The automatic water cutting control arranged in the system provided by the invention is provided with a field boundary level liquid level indication and a boundary level liquid level remote transmission control, when the boundary level liquid level reaches a set high boundary level, the automatic water cutting is carried out to the wastewater system, and when the boundary level liquid level reaches a set low boundary level, the automatic water cutting valve is automatically closed.
In some embodiments of the present invention, preferably, the reflux line communicates the carbon four collecting region of the reflux drum with the top of the rectification column.
In some embodiments of the present invention, it is preferable that the system further comprises an outlet line disposed at the bottom of the dewatering drum, and a communication line with a double valve 11 and a blind plate 10 for material returning or replacing work in emergency stop is disposed between the outlet line and the return line.
In the invention, a liquid return pump is arranged on the liquid return line and used for conveying the carbon four mixture.
In some embodiments of the present invention, preferably, the system further comprises at least 2 pretreaters arranged in parallel, the pretreaters communicating the cooler and the liquid recovery zone of the liquid recovery tank. The plurality of parallel pretreaters can be configured to be used alternately, for example, when 2 pretreaters are configured, the pretreaters can be used one by one, and the service life of the coalescer is ensured.
The implementation process of the method for separating and purifying mixed valeraldehyde provided by the invention is described by combining a system for separating and purifying mixed valeraldehyde in a specific embodiment shown in figure 1:
introducing mixed valeraldehyde (the content of valeraldehyde is 60-80 wt%, the content of the carbon-carbon four mixture is 10-30 wt%, and the content of water is 0.5-1.5 wt%) from the middle part of the rectifying tower 1, and heating and rectifying; the bottom of the rectifying tower 1 is provided with a reboiler 2, materials obtained at the bottom of the tower are heated in a mode of indirect heat exchange with external steam, light components contained in the materials at the bottom of the tower can be more fully separated, and meanwhile, the temperature of the steam in the reboiler is allowed to be increased by combining the system provided by the invention, so that the temperature of the middle bottom of the rectifying tower 1 is increased and controlled. Meanwhile, the separated refined valeraldehyde is obtained from the bottom of the rectifying tower 1. Controlling the operating conditions of the rectifying tower 1, wherein the pressure at the top of the rectifying tower is 0.4-1MPa, the temperature at the bottom of the rectifying tower is 150-160 ℃, and the temperature at the top of the rectifying tower is 50-60 ℃; the reflux ratio of the mixed valeraldehyde is 5-10.
Light components are discharged from the top of the rectifying tower 1, enter a cooler 3 for heat exchange and temperature reduction, and the obtained cooling material flow enters a liquid receiving area in a reflux tank 4 after partial impurities are removed by a preprocessor 5 (a plurality of preprocessors can be connected in parallel and used in a switching way). The reflux tank 4 is provided with a coalescer 6 and a baffle 7, which horizontally divides the interior of the reflux tank 4 into a liquid collecting area, a water collecting and draining area and a carbon four collecting area. The accumulation of the water and carbon tetra mixture in the cooled stream to the catchment drain is accelerated by the coalescer 6. A dewatering drum 8 is arranged below the water collecting and draining area to collect water, and the carbon-carbon mixture flows into a carbon-carbon collecting area when the liquid level of the separated liquid is higher than the baffle, so that the separation of the water and the carbon-carbon mixture is realized. The separated carbon-carbon four mixture is discharged through a liquid return pump 9, or part of the carbon-carbon four mixture is used as a recovery liquid and is introduced to the top of the rectifying tower 1, and the weight ratio of the recovery liquid to the mixed valeraldehyde entering the rectifying tower 1 is 0.7-1.25, which is favorable for better separating refined valeraldehyde.
The water collected in the dewatering bag is controlled by automatic water cutting at the bottom end of the dewatering bag, and is automatically cut into a wastewater system when the liquid level of the interface reaches a set high interface level and automatically closes a water cutting valve when the liquid level of the interface reaches a set high interface level through field interface level liquid level indication and interface level remote transmission control. In addition, a communication line with a double valve 11 and a blind plate 10 is arranged between the water outlet line and the return line of the system of the invention, and is used for material returning or replacing work in emergency shutdown.
The method for separating and purifying the mixed valeraldehyde provided by the invention can be further applied to a production method of 2-propyl heptanol, and the product yield and purity of the 2-propyl heptanol are improved. A method for producing 2-propylheptanol, comprising: carrying out carbonylation reaction on the mixed C4 and the synthesis gas to obtain mixed valeraldehyde; separating and purifying the mixture aldehyde by the method provided by the invention to obtain refined valeraldehyde; carrying out condensation and hydrogenation reactions on the refined valeraldehyde to obtain 2-propyl heptanol; wherein the purity of the refined valeraldehyde reaches more than 99 weight percent. The conditions of the carbonylation reaction and the condensation and hydrogenation reaction may be conventional in the art, and are not described in detail.
In the present invention, the pressures are gauge pressures.
The present invention will be described in detail below by way of examples.
Examples 1 to 7
10000kg/h of a pentanal/carbon tetra mix feed (pentanal content 75 wt%, carbon tetra mix content 24 wt%, water content about 1 wt%) was fed into the system shown in fig. 1. The conditions for the heating and rectification in the rectification column were as indicated in Table 1.
The composition of the resulting refined valeraldehyde product is shown in Table 2, and the composition of the carbon-tetrad mixture recovered at the top of the column is shown in Table 3.
Comparative example 1
FIG. 2 is a prior art method and system for separating and purifying mixed valeraldehyde. 10000kg/h of a pentanal/carbontetra mixture feed (pentanal content 75 wt%, carbontetra mixture content 24 wt%) was fed to the system shown in fig. 2, with a water content of about 1 wt%. The conditions for the heated rectification in the rectification column were carried out according to the prior art and are shown in Table 1.
The composition of the resulting refined valeraldehyde product is shown in Table 2, and the composition of the carbon-tetrad mixture recovered at the top of the column is shown in Table 3.
Comparative example 2
The procedure of example 1 was followed except that the conditions for the thermal rectification were changed, as shown in Table 1. The results are shown in tables 2 and 3.
Comparative example 3
10000kg/h of a pentanal/carbontetra mixture feed (pentanal content 75 wt%, carbontetra mixture content 24 wt%) was passed through the system shown in FIG. 2, with a water content of about 1 wt%. The conditions for the thermal rectification in the rectification column were as indicated in Table 1.
The composition of the resulting refined valeraldehyde product is shown in Table 2, and the composition of the top reflux C-C mixture is shown in Table 3.
TABLE 1
Numbering Pressure at the top of the column Temperature of the column bottom Temperature at the top of the column Reflux ratio Flow rate of recovery liquid
Example 1 0.40MPa 156℃ 50 8 8200kg/h
Example 2 0.3MPa 158℃ 52 7 12500kg/h
Example 3 0.5MPa 153℃ 53 6 7000kg/h
Example 4 0.5MPa 160℃ 60 5 8200kg/h
Example 5 1.0MPa 150℃ 57 10 8200kg/h
Example 6 0.40MPa 156℃ 50 8 6500kg/h
Example 7 0.40MPa 156℃ 50 8 13000kg/h
Comparative example 1 0.38MPa 145℃ 49 10 7800kg/h
Comparative example 2 0.38MPa 145℃ 49 11 7800kg/h
Comparative example 3 0.40MPa 156℃ 50 8 8200kg/h
Note: the weight ratio of the recovered liquid to the mixed pentanal is 10000kg/h of mixed pentanal/carbon four.
TABLE 2
Composition, by weight% Pentanal Mixed carbon four Water (W) Heavy fraction
Example 1 ≥99.5 <0.3 ≤0.1 ≤0.4
Example 2 ≥99.3 <0.3 ≤0.1 ≤0.4
Example 3 ≥99.4 <0.3 ≤0.1 ≤0.4
Example 4 ≥99.1 ≤0.5 ≤0.1 <0.5
Example 5 ≥99.2 ≤0.4 ≤0.1 <0.5
Example 6 ≥99 ≤0.6 ≤0.2 <0.5
Example 7 ≥99 ≤0.7 ≤0.2 <0.5
Comparative example 1 95.5 3 1 0.5
Comparative example 2 96.5 2 0.3 0.5
Comparative example 3 97.5 0.4 ≤0.4 0.5
Note: * By weight%
TABLE 3
Composition of Mixed carbon four Water (W)
Example 1 Not less than 99.9 wt% ≤30ppm
Example 2 Not less than 99.9 wt% ≤20ppm
Example 3 Not less than 99.9 wt% ≤28ppm
Example 4 Not less than 99.9 wt% ≤35ppm
Example 5 Not less than 99.9 wt% ≤35ppm
Example 6 Not less than 99.9 wt% ≤35ppm
Example 7 Not less than 99.9 wt% ≤35ppm
Comparative example 1 Not less than 99.9 wt% ≥300ppm
Comparative example 2 Not less than 99.9 wt% ≥300ppm
Comparative example 3 Not less than 99.9 wt% ≥300ppm
As can be seen from the results of the examples, the comparative examples and tables 1 to 3, by adopting the method and the system provided by the invention, the content of mixed C4 in the refined valeraldehyde obtained from the bottom of the rectifying tower in the examples can be reduced to below 0.7 wt% (Table 2), the purity of the refined valeraldehyde is stabilized to above 99 wt%, so that the risk of discharge of C4 in the downstream of the process and the risk of carrying C4 in the selling of the valeraldehyde product are reduced; meanwhile, the water content in the carbon-four mixture refluxed at the top of the rectifying tower is stabilized within 35ppm (Table 3). Four 1900 tons of mixed carbon (calculated as 10000kg/h of pentanal/carbon four-mixed feed) can be recovered each year.
The method provided by the invention is combined with the improvement of a surrounding reflux tank in the system, so that the effective separation of light components discharged from the top of the rectifying tower is realized, the rectifying tower is allowed to be better controlled, and the purity of a refined valeraldehyde product obtained by separating and purifying mixed valeraldehyde reaches more than 99 percent by weight. Examples 1-3 were run under the most preferred heated rectification conditions, with the best purification results. The heating and rectifying conditions of examples 4 to 5 were carried out under less preferable conditions, and the weight ratio of the recovered liquid to the mixed valeraldehyde on the rectifying tower in examples 6 and 7 was out of the preferable range, and the purification effect was slightly poor. Comparative example 1 employed a prior art system and thermal distillation conditions, comparative example 3 employed a prior art system but thermal distillation conditions were within the scope of the invention, and comparative example 2 employed a system of the invention but thermal distillation conditions were prior art, resulting in less purified valeraldehyde than the examples.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (13)

1. A method for separating and purifying mixed valeraldehyde comprises the following steps:
(1) Heating and rectifying the mixed valeraldehyde to obtain refined valeraldehyde and light components; wherein the heating and rectifying conditions comprise: the pressure at the top of the rectifying tower is 0.3-1MPa, the temperature at the bottom of the rectifying tower is 150-160 ℃, and the temperature at the top of the rectifying tower is 50-60 ℃; the reflux ratio of the mixed valeraldehyde rectifying tower is 5-10;
(2) Sequentially cooling and separating the light components to obtain wastewater and a carbon-carbon mixture;
(3) Returning a portion of the carbon-four mixture as a recycle to the heated rectification in step (1).
2. The method of claim 1, wherein the conditions of the heated rectification comprise: the pressure at the top of the rectifying tower is 0.3-0.5MPa, the temperature at the bottom of the rectifying tower is 153-158 ℃, and the temperature at the top of the rectifying tower is 50-53 ℃; the reflux ratio of the mixed valeraldehyde is 6-8.
3. The method according to claim 1 or 2, wherein the weight ratio of the recovering solution to the mixed valeraldehyde is 0.7 to 1.25.
4. A system for mixed valeraldehyde separation and purification according to any one of claims 1 to 3, comprising:
the rectifying tower is used for heating and rectifying the mixed valeraldehyde to obtain refined valeraldehyde at the bottom of the tower and obtain light components at the top of the tower;
the reboiler is communicated with the bottom of the rectifying tower and is used for increasing the temperature of the mixed valeraldehyde;
the cooler is communicated with the top of the rectifying tower and is used for cooling the light components to obtain a cooled material flow; and
the liquid return tank is communicated with the cooler and is used for separating the cooled material flow to obtain wastewater and a carbon-carbon mixture;
a reflux pipeline is arranged between the liquid return tank and the top of the rectifying tower and is used for refluxing a part of the carbon-four mixture to the top of the rectifying tower;
the liquid return tank comprises: internally disposed coalescers and baffles, and externally disposed dewatering packages and automatic water cut controls.
5. The system of claim 4 wherein said coalescer and baffle are horizontally spaced within said return tank to horizontally divide the interior of said return tank into a liquid collection zone, a water collection and drainage zone, and a carbon-four collection zone.
6. The system according to claim 5, wherein said coalescer occupies the entire cross-section of said return tank, and said baffle occupies a portion of the cross-section of said return tank.
7. The system of claim 6, wherein the dewatering drum is disposed below the return tank and is in communication with the water collection and drainage area.
8. The system of any one of claims 4-7, wherein the system further comprises at least 2 preconditioners arranged in parallel, the preconditioners communicating between the cooler and a liquid recovery zone of a return liquid tank.
9. The system of any one of claims 4, 5, 6, and 7, wherein the reflux line communicates the carbon-four collection zone of the reflux drum with the top of the rectification column.
10. The system of claim 8, wherein the return line communicates a carbon four collection zone of the return tank with a top of the rectification column.
11. The system according to any one of claims 4, 5, 6, 7 and 10, wherein the system further comprises an outlet line arranged at the bottom of the dewatering drum, and a communication line with a double valve and a blind plate is arranged between the outlet line and the return line, and the communication line is used for material returning or replacing work in emergency stop.
12. The system of claim 8, further comprising an outlet line disposed at the bottom of the dewatering drum, and a communication line with a double valve and a blind plate is disposed between the outlet line and the return line, the communication line being used for material refuelling or replacement work during emergency shut-down.
13. The system of claim 9, further comprising an outlet line disposed at the bottom of the dewatering drum, and a communication line with a double valve and a blind plate for material returning or replacing work in emergency stop is disposed between the outlet line and the return line.
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