CN217757302U - Separation system for catalyst and oxo-product in oxo-synthesis - Google Patents
Separation system for catalyst and oxo-product in oxo-synthesis Download PDFInfo
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- CN217757302U CN217757302U CN202221497419.9U CN202221497419U CN217757302U CN 217757302 U CN217757302 U CN 217757302U CN 202221497419 U CN202221497419 U CN 202221497419U CN 217757302 U CN217757302 U CN 217757302U
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Abstract
The utility model relates to a catalyst piece-rate system, in particular to catalyst and oxo-synthesis result's piece-rate system in oxo belongs to oxo technical field. The separation system adopts a two-stage separation mode to separate the catalyst of the oxo-synthesis from the oxo-synthesis product, the first-stage separation mainly comprises pre-separation and olefin recovery, the second-stage separation mainly comprises final separation of the catalyst and the oxo-synthesis product, the catalyst is recycled, and the catalyst circulation amount accounts for 1/3-1/4 of the total feed amount. The utility model discloses a catalyst solution in the two-stage system separation oxo-synthesis result carries out abundant separation with catalyst and oxo-synthesis result, and high temperature dwell time is short, does not have any catalyst loss, carries out recycle to alkene, alkane simultaneously.
Description
Technical Field
The utility model relates to a catalyst piece-rate system, in particular to catalyst and oxo synthesis result's piece-rate system in oxo synthesis belongs to oxo synthesis technical field.
Background
The oxo-product is an important organic chemical raw material and has wide application. The oxo products are industrially produced mainly by reacting carbon monoxide, hydrogen and olefins over a catalyst. In the production process, a homogeneous complex rhodium-phosphine catalyst system is mainly adopted, the catalyst is dissolved in a carbonyl synthesis product solution, a rhodium atom is taken as a center, and an organophosphorus compound is taken as a ligand. The produced oxo-synthesis product needs to be separated from rhodium, organic phosphorus compound and oxo-synthesis product, and unreacted materials are recycled.
CN201911275658.2 discloses a method of adding deionized water into a catalyst solution to separate the catalyst by using the difference of solubility of each substance, but introducing a new solvent results in a decrease in reaction effect, an increase in material consumption, and an entrainment loss of the catalyst.
CN95121416.0 discloses a method for separating by rectification, which comprises the steps of conducting heat transfer and mass transfer on a packed bed through a tower type separator, and conducting separation, wherein the activity of the catalyst is reduced due to high temperature, and the retention time of the catalyst is longer under the condition of high temperature, so that the service life of the catalyst is shorter.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a catalyst and oxo synthesis result's piece-rate system in oxo, this system have realized the effective separation of catalyst, have solved catalyst separation in-process catalyst and have received the problem that high temperature harmd and catalyst run and decrease.
The utility model provides a technical scheme that its technical problem adopted is:
a system for synthesizing catalyst and product by carbonyl reaction is composed of serially connected primary and secondary separating assemblies, condenser, gas-phase product line, product storage tank, liquid-phase outlet of product storage tank, compressor, and tail gas exhausting line.
The utility model discloses utilize the difference of boiling point to separate rhodium, organic phosphorus compound, unreacted raw materials to carry out recycle to the alkene. The mixed solution from the oxo apparatus contains mainly oxo product, oxo polymer, rhodium, organic phosphorus compound, carbon monoxide, hydrogen, olefin, alkane, etc. dissolved in the solution. The mixed solution of the oxo-product enters a separation system to be heated, separated and purified for two times.
Because the solubility of the olefin and the alkane in the oxo-synthesis product is strong, the mixed solution containing the oxo-synthesis product, the oxo-synthesis product polymer, rhodium, an organic phosphorus compound and carbon monoxide, hydrogen, olefin and alkane dissolved in the solution needs to be heated in a first-stage heater, and then enters a gas-liquid separator in a first-stage separator for pre-separation, larger droplets and gas-phase components are separated firstly, so that droplets contained in the gas-phase components are reduced, the main components in the gas phase are the oxo-synthesis product, the olefin and the alkane, at the moment, the gas phase still contains droplets, the droplets contain the dissolved organic phosphorus compound and need to be further removed, at the moment, the gas phase carries the droplets to enter a membrane separator at the top of the first-stage separator, the liquid carrying amount is continuously reduced, but the droplets still carry with the droplets due to the small droplets, the droplets at the moment, the droplets are micron-sized droplets, the gas phase carries with the micron-sized droplets to enter the first-stage enhanced separator, a filter with a coalescence function is arranged in the enhanced separator, all the droplets are completely recovered, and the oxo-synthesis product, the olefin and the alkane in the gas phase enter a condenser for the oxo-synthesis product. Realizes the separation of a small amount of carbonyl synthesis product and all olefin and alkane from the catalyst solution.
The liquid phase at the bottom of the primary separator is a catalyst solution containing most of the oxo product, at which point the concentration of the oxo product in the catalyst solution is still high and the oxo product needs to be further separated. The catalyst solution containing most of the oxo-synthesis product enters a secondary heater for heating, and enters a gas-liquid separator in a secondary intensified separator after being heated for pre-separation, larger liquid drops and gas phase components are firstly separated, so that the liquid drops contained in the gas phase components are reduced, the main component in the gas phase is butyraldehyde, at the moment, the gas phase still contains liquid drops which contain dissolved organic phosphorus compounds and need to be further removed, at the moment, the gas phase enters a membrane separator at the top of the secondary intensified separator with the liquid drops to continuously reduce the liquid carrying capacity, but the liquid drops still can be carried because the liquid drops are smaller, the liquid drops are micron-sized liquid drops, the gas phase carries the micron-sized liquid drops to enter the secondary intensified separator, a filter with a coalescence function is arranged in the intensified separator, the liquid drops are completely and completely recovered, and butyraldehyde in the gas phase enters a butyraldehyde condenser. The gas phase is converged with the gas phase from the first-stage separation, the carbonyl synthesis product is completely condensed and then enters a product storage tank, the olefin and the alkane dissolved in the carbonyl synthesis product are released after pressure reduction, the olefin and the alkane are pressurized by an olefin compressor and then return to the reactor to continue to react, and the olefin product in the product storage tank enters a downstream device for use, so that the separation of a large amount of olefin products and a catalyst solution is realized. At the moment, the catalyst is recycled from the bottom secondary enhanced separator to the olefin device for continuous use. The process needs to control the output of olefin and maintain the output in a reasonable interval, so as to prevent the catalyst from being excessively concentrated and blocking a pipeline.
Preferably, the first-stage separation component is formed by sequentially connecting a first-stage heater, a first-stage separator and a first-stage reinforced separator, the first-stage separator is connected with a gas-phase inlet of the first-stage reinforced separator through a gas-phase pipeline, a gas-phase outlet of the first-stage reinforced separator is connected with an olefin-containing product pipeline, and a liquid-phase outlet of the first-stage reinforced separator is refluxed into the first-stage separator through a recovery liquid pipeline;
the structure of the second-stage separation component is the same as that of the first-stage separation component, and the second-stage separation component is formed by connecting a second-stage heater, a second-stage separator and a second-stage intensified separator, wherein the second-stage separator is connected with a gas-phase inlet of the second-stage intensified separator through a second-stage gas-phase pipeline, a gas-phase outlet of the second-stage intensified separator is connected with a product pipeline, and a liquid-phase outlet of the second-stage intensified separator reflows into the second-stage separator through a second-stage recovery liquid pipeline;
the first-stage separator is connected with the second-stage heater through a tail liquid pipeline, and a liquid phase outlet of the second-stage separator is a circulating catalyst pipeline for recovering the catalyst.
Preferably, the primary heater and the secondary heater are vertical or horizontal, and have the characteristics of short retention time and high heating efficiency; the operation pressure of the first-stage separator and the first-stage intensified separator is 0.2-0.8 MPaG, and the operation pressure of the second-stage separator and the second-stage intensified separator is 0.01-0.2 MPaG.
Preferably, the first-stage separator and the second-stage separator have the same structure, and are internally provided with a gas-liquid separator and a gas-liquid membrane separator for filtering micron-sized liquid drops in the gas and leading the liquid drops to be gathered and sink to the bottom of the first-stage separator or the second-stage separator.
Preferably, the gas-liquid membrane separator is in a fan shape and can block liquid drops entrained in gas rising, the fiber membrane tube wall in the gas-liquid membrane separator is full of 30-40 nanometer micropores, and the fiber membrane tube wall is hydrophobic and liquid cannot pass through the micropores, so that gas can pass through the micropores.
Preferably, the first-stage intensified separator and the second-stage intensified separator are gas-liquid separation devices with double-layer filtering structures. The gas-liquid separation device has a coalescence function and can collect micron-sized liquid drops into large liquid drops; the number of the gas-liquid separation devices can be adjusted according to the actual production capacity.
Preferably, the compressor is a reciprocating type or a screw type.
When the separation system is used, the catalyst for the oxo-synthesis and the oxo-synthesis product are separated in a two-stage separation mode, the first-stage separation mainly comprises pre-separation and olefin recovery, the second-stage separation mainly comprises final separation of the catalyst and the oxo-synthesis product, the catalyst is recycled, and the catalyst circulation amount accounts for 1/3-1/4 of the total feeding amount.
The utility model discloses can carry out the accurate separation to the catalyst that the oxo adopted and oxo result to retrieve unreacted alkene, improve whole economic nature. The oxo reaction is mainly that olefins and synthesis gas generate aldehydes such as: the propylene reacts with the synthesis gas to generate butyraldehyde which dissolves the catalyst, the ethylene reacts with the synthesis gas to generate propionaldehyde which dissolves the catalyst, and the like. The mixture obtained by the oxo reaction is subjected to primary heating and then primary separation, 1/10-1/8 of oxo products and all olefins are recovered after the primary separation, tail liquid obtained by the primary separation is subjected to secondary heating and then secondary separation, and all the oxo products and catalysts which can be recycled are recovered after the secondary separation; after the oxo product is separated from all the olefins, the olefins are sent back to the oxo device through a compressor, and the oxo product is sent out as a product. The temperature of the first-stage heating is 100-200 ℃, and the time of the first-stage heating of the material is controlled within 40S; the temperature of the secondary heating is 100-160 ℃, and the time of the secondary heating of the material is controlled within 40S.
The utility model has the advantages that: the utility model discloses a catalyst solution in the two-stage system separation oxo process product carries out abundant separation with catalyst and oxo process product, and high temperature dwell time is short, does not have any catalyst loss, carries out recycle to alkene, alkane simultaneously.
Drawings
FIG. 1 is a schematic diagram of the separation system for catalyst and oxo product in oxo process of the present invention,
description of the reference symbols:
a first-stage heater 1, a first-stage separator 2, a gas phase pipeline 3, a recovered liquid pipeline 4, a first-stage intensified separator 5, a tail liquid pipeline 6,
7 second-stage heater, 9 second-stage separator, 10 circulating catalyst pipeline, 11 second-stage recovered liquid pipeline, 12 second-stage gas phase pipeline, 13 second-stage intensified separator,
14 gas phase product line, 15 olefin containing product line, 16 condenser, 17 product storage tank, 18 export line, 19 tail gas discharge line, 20 olefin line, 21 compressor.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any modifications and/or changes in form made to the invention are intended to fall within the scope of the invention.
In the utility model, all parts and percentages are weight units, and the adopted equipment, raw materials and the like can be purchased from the market or commonly used in the field if not specified. The methods in the following examples are conventional in the art unless otherwise specified.
Example (b):
this example illustrates the separation of the catalyst from the product of the butyraldehyde synthesis by propylene carbonylation, the system for separation being shown in fig. 1.
A separation system of catalyst and products of oxo-synthesis comprises a first-stage separation component and a second-stage separation component which are connected in series, wherein the first-stage separation component is connected with a condenser 16 through an olefin-containing product pipeline 15, the second-stage separation component is connected with the condenser 16 through a gas-phase product pipeline 14, the condenser is connected to a product storage tank 17, and the product storage tank is a vertical tank body. The liquid phase outlet of the product storage tank is connected with an outward conveying pipeline 18, the gas phase outlet of the product storage tank is connected with a compressor 21 through an olefin pipeline 20, and the gas phase outlet of the product storage tank is also provided with a tail gas discharge pipeline 19. The compressor is a reciprocating type or a screw type.
The first-stage separation component is formed by sequentially connecting a first-stage heater 1, a first-stage separator 2 and a first-stage intensified separator 5, the first-stage separator is connected with a gas-phase inlet of the first-stage intensified separator through a gas-phase pipeline 3, a gas-phase outlet of the first-stage intensified separator is connected with an olefin-containing product pipeline, and a liquid-phase outlet of the first-stage intensified separator is refluxed into the first-stage separator through a recovery liquid pipeline 4;
the structure of the second-stage separation component is the same as that of the first-stage separation component, and the second-stage separation component is formed by connecting a second-stage heater 7, a second-stage separator 9 and a second-stage intensified separator 13, wherein the second-stage separator is connected with a gas-phase inlet of the second-stage intensified separator through a second-stage gas-phase pipeline 12, a gas-phase outlet of the second-stage intensified separator is connected with a product pipeline, and a liquid-phase outlet of the second-stage intensified separator reflows into the second-stage separator through a second-stage liquid recovery pipeline 11;
the first-stage separator is connected with the second-stage heater through a tail liquid pipeline 6, and a liquid phase outlet of the second-stage separator is a circulating catalyst pipeline 10 for recovering the catalyst.
The primary heater and the secondary heater are vertical or horizontal, and have the characteristics of short retention time and high heating efficiency; the operation pressure of the first-stage separator and the first-stage intensified separator is 0.2-0.8 MPaG, and the operation pressure of the second-stage separator and the second-stage intensified separator is 0.01-0.2 MPaG.
The structure of the first-stage separator is the same as that of the second-stage separator, and a gas-liquid separator and a gas-liquid membrane separator are arranged in the first-stage separator and the second-stage separator and are used for filtering micron-sized liquid drops in the gas and enabling the micron-sized liquid drops to be gathered and sink to the bottom of the first-stage separator or the second-stage separator. The gas-liquid membrane separator is in a fan shape and can prevent liquid drops from being carried when gas rises, the fiber membrane tube wall in the gas-liquid membrane separator is full of 30-40 nanometer micropores, and the fiber is hydrophobic and liquid-proof, so that liquid cannot pass through the micropores and gas can pass through the micropores.
The first-stage intensified separator and the second-stage intensified separator are gas-liquid separation devices with double-layer filtering structures. The gas-liquid separation device has a coalescence function and can collect micron-sized liquid drops into large liquid drops; the number of the gas-liquid separation devices can be adjusted according to the actual production capacity.
In this example, 1000Kg/h of catalyst solution was composed of: 2.20% of propylene, 2.80% of propane, 6.00% of isobutyraldehyde, 64.64% of n-butyraldehyde, 0.09% of n-butanol, 10.00% of phosphine ligand (triphenylphosphine and rhodium catalyst) and 14.27% of butyraldehyde trimer, wherein the total content is 100%.
The butyraldehyde which is a material of synthesis reaction and a catalyst solution enter a first-stage heater 1 to be heated together, the temperature is raised to 120-160 ℃ after the heating and the retention time is 20S, the butyraldehyde and the catalyst solution enter a first-stage separator 2, the pressure of the first-stage separator 2 is controlled to be 0.4-0.8 MPaG, a gas-liquid separator and a gas-liquid membrane separator are arranged in the first-stage separator 2, a small part of butyraldehyde, all propylene and propane components in the gas-liquid separator are separated from liquid-phase butyraldehyde, butyraldehyde trimer, rhodium and organic phosphorus compounds, a small part of butyraldehyde and all propylene and propane components enter a membrane separator at the top of the first-stage separator to recover entrained liquid drops, rhodium and organic phosphorus compounds are contained in the liquid drops, most of the liquid drops can be recovered in the membrane separator, the gas phase obtained by the first-stage separator 2 enters a first-stage intensified separator 5 through a gas-phase pipeline 3, the first-stage intensified separator 5 contains a double-layer filter with the function, micron-level liquid drops entrained in the gas phase are coalesced into large liquid drops, the bottom of the first-stage intensified separator 5 and return to the first-stage separator 2 through a recycle liquid pipeline 4, and the gas phase condenser 16 from which olefin product is completely removed from which the liquid drops.
The liquid containing most of butyraldehyde, butyraldehyde trimer, rhodium and organic phosphorus compounds enters a secondary heater 7 through a tail liquid pipeline 6, the liquid is heated to 100-160 ℃, the heated material enters a secondary separator 9, the structure of the secondary separator 9 is the same as that of a primary reinforced separator, the liquid also comprises a gas-liquid separator and a gas-liquid membrane separator, butyraldehyde and liquid-phase butyraldehyde, butyraldehyde trimer, rhodium and organic phosphorus compounds in the gas-liquid separator are separated, most of gas-phase butyraldehyde enters a membrane separator at the top of the secondary separator, entrained liquid drops are recovered, rhodium and organic phosphorus compounds are contained in the liquid drops, most of the gas-phase butyraldehyde can be recovered in the membrane separator and enters the secondary reinforced separator 13 through a secondary gas pipeline 12, the secondary reinforced separator 13 contains a double-layer filter with a coalescence function, micron-sized liquid drops entrained in the gas phase are coalesced into large liquid drops which fall to the bottom of the secondary reinforced separator 13 and return to the secondary separator 9, and the gas-phase butyraldehyde from which the liquid drops are completely removed enters a condenser 16 through a gas-phase product pipeline 14. The second separator 9 is circulated at the bottom thereof with a catalyst line 10 to obtain a concentrated catalyst solution.
At this time, the flow rate of the catalyst solution concentrated at the bottom of the second separator 9 was 300Kg/h, and the components: isobutyraldehyde 0.6%, n-butyraldehyde 20.88%, n-butanol 0.05%, phosphine ligand 33.30%, and butyraldehyde trimer 45.17%.
The gas phase products of the first-stage enhanced separator 5 and the second-stage separator 9 are cooled to 30-45 ℃ in a condenser 16, condensed butyraldehyde enters a product storage tank 17 for gas-liquid separation, liquid butyraldehyde is sent out through an outgoing pipeline 18, the gas phase is a mixed gas of propylene and propane, the mixed gas is sent to a compressor 21 through an olefin pipeline 20 to be recovered, and due to the fact that the reaction of the recovered products is not good due to accumulation of nitrogen and propane, tail gas is discharged through a tail gas discharge pipeline 19, and it is guaranteed that the nitrogen and the propane in the components of the tail gas do not exceed standards.
At this time, the flow rate of the recovered tail gas is 80Kg/h, and the components: 10.00 percent of nitrogen plus argon, 27.50 percent of propylene, 34.50 percent of propane, 4.00 percent of isobutyraldehyde and 24.00 percent of n-butyraldehyde; the flow rate of butyraldehyde product is 620Kg/h, and the components are as follows: 9.00 percent of isobutyraldehyde, 90.50 percent of n-butyraldehyde and 0.50 percent of butyraldehyde trimer.
The utility model discloses in, with product and catalyst separation in the oxo process of production, the catalyst recycles, and the effect is better, effectually separates catalyst and oxo result to recycle olefin, the catalyst runs to decrease extremely, does not basically have the loss, and the activity of catalyst under the high temperature condition has been avoided in low temperature evaporation and has been descended, assurance catalyst long service life that can be better.
The embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same or similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The above details are provided for the separation system of the catalyst and the oxo product in the oxo process. The principles and embodiments of the present invention have been explained herein using specific examples, and the above descriptions of the embodiments are only used to help understand the method and its core ideas of the present invention. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, the present invention can be further modified and modified, and such modifications and modifications also fall within the protection scope of the appended claims.
Claims (7)
1. A separation system of catalyst and oxo-product in oxo-synthesis is characterized in that: the separation system comprises a first-stage separation assembly and a second-stage separation assembly which are connected in series, wherein the first-stage separation assembly is connected with a condenser (16) through an olefin-containing product pipeline (15), the second-stage separation assembly is connected with the condenser (16) through a gas-phase product pipeline (14), the condenser is connected to a product storage tank (17), a liquid-phase outlet of the product storage tank is connected with an outward delivery pipeline (18), a gas-phase outlet of the product storage tank is connected with a compressor (21) through an olefin pipeline (20), and a tail gas discharge pipeline (19) is further arranged at the gas-phase outlet of the product storage tank.
2. The separation system of claim 1, wherein: the first-stage separation component is formed by sequentially connecting a first-stage heater (1), a first-stage separator (2) and a first-stage intensified separator (5), the first-stage separator is connected with a gas-phase inlet of the first-stage intensified separator through a gas-phase pipeline (3), a gas-phase outlet of the first-stage intensified separator is connected with an olefin-containing product pipeline, and a liquid-phase outlet of the first-stage intensified separator reflows into the first-stage separator through a recovery liquid pipeline (4);
the structure of the second-stage separation component is the same as that of the first-stage separation component, and the second-stage separation component is formed by connecting a second-stage heater (7), a second-stage separator (9) and a second-stage intensified separator (13), wherein the second-stage separator is connected with a gas-phase inlet of the second-stage intensified separator through a second-stage gas-phase pipeline (12), a gas-phase outlet of the second-stage intensified separator is connected with a product pipeline, and a liquid-phase outlet of the second-stage intensified separator reflows into the second-stage separator through a second-stage recovery liquid pipeline (11);
the first-stage separator is connected with the second-stage heater through a tail liquid pipeline (6), and a liquid phase outlet of the second-stage separator is a circulating catalyst pipeline (10) for recovering the catalyst.
3. The separation system of claim 2, wherein: the primary heater and the secondary heater are vertical or horizontal; the operation pressure of the first-stage separator and the first-stage intensified separator is 0.2-0.8 MPaG, and the operation pressure of the second-stage separator and the second-stage intensified separator is 0.01-0.2 MPaG.
4. The separation system of claim 2, wherein: the first-stage separator and the second-stage separator have the same structure, and are internally provided with a gas-liquid separator and a gas-liquid membrane separator for filtering micron-sized liquid drops in the gas and leading the liquid drops to be gathered and sink to the bottom of the first-stage or second-stage separator.
5. The separation system of claim 2, wherein: the gas-liquid membrane separator is in a fan shape, and the wall of a fiber membrane tube inside the gas-liquid membrane separator is fully distributed with 30-40 nanometer micropores.
6. The separation system of claim 2, wherein: the first-stage intensified separator and the second-stage intensified separator are gas-liquid separation devices with double-layer filtering structures.
7. The separation system of claim 1, wherein: the compressor is a reciprocating type or a screw type.
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