CN213357400U - Oxide removing device in crude butadiene production by oxidative dehydrogenation of butylene - Google Patents
Oxide removing device in crude butadiene production by oxidative dehydrogenation of butylene Download PDFInfo
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- CN213357400U CN213357400U CN202022186989.3U CN202022186989U CN213357400U CN 213357400 U CN213357400 U CN 213357400U CN 202022186989 U CN202022186989 U CN 202022186989U CN 213357400 U CN213357400 U CN 213357400U
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Abstract
The utility model discloses an oxide desorption device in butene oxidative dehydrogenation production crude butadiene, along reaction formation gas flow direction, include the equipment that connects according to following mode: the reaction generated gas is compressed by a generated gas compressor, then is cooled by a cooler and then directly enters an oil absorption desorption unit, and the four carbon components separated by the oil absorption desorption unit enter an extraction tower from the bottom; the extraction agent circulating water enters from the top, and the tower kettle water of the extraction tower enters the stripping rectification tower from the middle part after being connected with the heat exchanger; the steam stripping rectifying tower is provided with a tower top condenser, gas phase extracted from the tower top is sent to be used as fuel gas, the tower kettle is provided with a reboiler, and tower kettle water is circulated back to the extraction tower after passing through a heat exchanger. The utility model discloses shortened the process flow that generates gas to between the oil absorption desorption unit, reduced butadiene polymerization's distance and time, reduced the interference of noncondensable gas component, and adopted liquid-liquid extraction technology, can improve the rate of recovery of butadiene, reduced the content of oxide.
Description
Technical Field
The utility model belongs to the technical field of the separation, concretely relates to oxide desorption device in butene oxidative dehydrogenation production crude butadiene.
Background
Butadiene is an important petrochemical basic material used for producing synthetic rubber, synthetic resin, adiponitrile, hexamethylenediamine, nylon 66, sulfolane, 1, 4-butanediol, etc. The butadiene production method comprises two methods of carbon four fraction separation and synthesis (including butane dehydrogenation, butene oxidative dehydrogenation and the like). Almost all butadiene from all countries in the world is directly derived from a carbon four fraction which is a by-product in the preparation of ethylene by hydrocarbon cracking. The production of butadiene by the oxidative dehydrogenation of butene is an important supplement to butadiene sources.
The butadiene is produced by butylene, oxygen-containing gas and steam through catalytic oxidative dehydrogenation reaction in a reactor, wherein the generated gas contains four carbon components, oxides, a large amount of non-condensable gas and the like, the four carbon components mainly comprise butadiene, unreacted butylene and butane, and the non-condensable gas mainly comprises nitrogen, unreacted oxygen, a small amount of carbon dioxide and the like. When the product is separated, firstly, the generated gas after heat recovery is quenched and pickled (acid gas is removed), then the generated gas is compressed, the compressed material is sent to an oxide removal tower for washing, the overhead gas is extracted and then sent to oil absorption desorption units A and D, crude butadiene can be obtained through separation, and the oxide, the carbon tetrahydrocarbon and the noncondensable gas which are washed in the tower kettle water are sent to a stripping tower for stripping, and can be used as fuel gas.
FIG. 1 is a process unit for removing the oxide generated by the oxidative dehydrogenation reaction of butene, which is widely used at present. The reaction generated gas S1 after heat recovery and quenching, the material S-2 compressed by the generated gas compressor C-1, and the material S-3 cooled by circulating water in the cooler E-1 are sent to the oxide removal tower T-1. Two sections of water washing are arranged at the upper section of the T-1, the second section of the T-1 adopts circulating washing water for washing, the first section of the T-1 tower kettle is washed by supplementary clean water, and the T-1 tower kettle water is sent to a stripping tower T-2 after being subjected to heat exchange and temperature rise by a heat exchanger E-2. In T-2, the washed oxides, the carbon tetrads and the noncondensable gas are stripped, and S6 is extracted from the top of the tower and is used as fuel gas. The stripped tower bottom water S7 without oxide and carbon tetrahydrocarbon is cooled by a heat exchanger E-2 and a cooler E-3 respectively, one part of the stripped tower bottom water is sent to T-1 to be used as second-stage washing water, and the other part of the stripped tower bottom water S13 is used as waste water for extraction. And (3) extracting the overhead gas S10 of the oxide removal tower T-1, and then sending the overhead gas to oil absorption desorption units A and D to respectively obtain crude butadiene S12 and tail gas S11.
Through research and analysis, the oxide removal process has the following defects:
1) the gas generated by compressing the oxidative dehydrogenation reaction gas contains 1-2% of oxygen, the generated gas also contains oxides such as aldehyde, ketone, furan and the like, and the existence of the impurities causes the butadiene in the generated gas to be polymerized, thereby reducing the recovery rate of the butadiene. The longer the process of the generated gas, the more the butadiene is lost, the oxide removal tower is arranged at the outlet of the compressor, and in the actual production, more polymers in the tower are observed;
2) more than 60% of reaction generated gas is non-condensable gas such as nitrogen, carbon dioxide, oxygen and the like, the oxide removal tower is arranged at the outlet of a compressor of the generated gas, the size of the oxide removal tower is large, the washing water amount is also large, and the steam consumption of the corresponding stripping tower is increased;
3) when the oxygen-containing compounds in the generated gas are removed to a certain concentration, the hydrocarbon oxides in the crude butadiene are correspondingly concentrated due to the separation of the generated gas and the hydrocarbon components, so that the content of the hydrocarbon oxides is multiplied, and the removal difficulty is higher particularly for removing the oxygen-containing compounds to the concentration of ppm level.
Disclosure of Invention
The utility model aims to overcome the defects of the prior art and provide a crude butadiene oxide removing device.
The purpose of the invention is realized by the following technical scheme:
a device for removing oxide in crude butadiene produced by oxidative dehydrogenation of butylene comprises reaction generated gas from an oxidative dehydrogenation reactor after heat recovery, quenching and acid washing, and is characterized in that the device comprises equipment connected in the following mode along the material flow direction: the reaction generated gas is compressed by a generated gas compressor, and then is cooled by a cooler and then directly enters an oil absorption and desorption unit, the four carbon components separated by the oil absorption and desorption unit enter an extraction tower from the bottom, the extractant circulating water enters the extraction tower from the top, the tower kettle water of the extraction tower is connected with a heat exchanger, and after heat exchange and temperature rise, the four carbon components enter a stripping rectification tower from the middle part, the stripping rectification tower is provided with a tower top condenser, and the gas phase extracted from the tower top is sent to be used as fuel gas; the tower kettle of the stripping rectification tower is provided with a reboiler, and the tower kettle water is circulated back to the extraction tower through a heat exchanger.
In the device, the tail gas separated by the oil absorption and desorption unit is connected with a tail gas treatment device and then is discharged.
In the device, the extraction tower is washed by one-stage circulating water in a counter-current manner, and the extractant circulating water is added from the top of the extraction tower and comes from the tower kettle of the stripping rectification tower.
The extraction tower adopts a plate tower or a packed tower, preferably a plate tower, and the operation pressure is 0.3 MPaG-1.8 MPaG, preferably 0.8 MPaG-1.5 MPaG; the operating temperature is 10 ℃ to 55 ℃, and the preferred operating temperature is 20 ℃ to 45 ℃.
The content of hydrocarbon oxide in the overhead discharge of the extraction tower is 10 ppm-200 ppm, and the preferable control value is 80 ppm-150 ppm.
The temperature of the extractant circulating water sent to the extraction tower is 10-55 ℃, and the preferred operation temperature is 20-45 ℃.
Compared with the prior art, the utility model has the advantages of as follows:
(1) by adopting the liquid-liquid extraction process, the tower diameter of the oxide removal tower is greatly reduced, and the investment is reduced;
(2) the interference of a large amount of non-condensable gas components is avoided, and the content of oxide in the crude butadiene can be reduced to a lower level;
(3) the process flow from the outlet of the oxidative dehydrogenation reactor to the tail gas at the top of the oil absorption tower is shortened, the route and time of butadiene polymerization are reduced, and the recovery rate of butadiene is equivalently improved.
Drawings
FIG. 1 is a schematic flow diagram of a conventional oxide removal unit;
FIG. 2 is a schematic structural diagram of the device for removing oxides from crude butadiene produced by oxidative dehydrogenation of butene;
the meaning of each mark in fig. 1 to 2 is:
c-1 is a gas-generating compressor, and A & D are oil absorption desorption units.
T-1 is an oxide removal tower, T-2 is a stripping tower, T-3 is an extraction tower, and T-4 is a stripping rectification tower.
E-1 is a compressor outlet cooler, E-2 is a stripping tower inlet/outlet heat exchanger, E-3 is a circulating washing water cooler, E-4 is a stripping tower reboiler, E-12 is a stripping rectifying tower inlet/outlet heat exchanger, E-13 is a circulating washing water cooler, E-14 is a stripping rectifying tower reboiler, and E-15 is a stripping rectifying tower condenser.
S1-S20 represent streams, where S12 is crude butadiene and S20 is make-up fresh wash water.
Detailed Description
Example 1
Example 1 describes the oxidative dehydrogenation of butene to butadiene on a scale of 10 million tons/year.
Description of the basic parameters of the device: hydrocarbon oxygenate control requirements in crude butadiene feed: the content of hydrocarbon oxygen-containing compounds is less than or equal to 100 ppm; annual operating time 8000 hours; the treatment capacity of the reaction product gas is 53.0 tons/hour, and the composition is shown in Table 1;
TABLE 1 reaction product gas composition
As shown in figure 2, the device for removing oxide in the crude butadiene production by oxidative dehydrogenation of butylene of the utility model comprises the following devices connected in the following mode:
the reaction generated gas S1 from the oxidative dehydrogenation reactor, which is subjected to heat recovery, quenching and acid gas removal, is compressed by a generated gas compressor C-1, is cooled by a cooler E-1 and then directly enters an oil absorption desorption system to separate non-condensable gas and four carbon components, the tail gas S11 is sent to an extraction tower T-3 for tail gas treatment and evacuation, and the four carbon components S15 are sent to an extraction tower T-3. The extraction tower T-3 adopts a section of circulating water countercurrent washing, and the circulating water washing water comes from the tower kettle of the stripping rectification tower T-4. The water in the T-3 tower kettle is sent to the middle part of a stripping rectification tower T-4 after heat exchange and temperature rise through a heat exchanger E-12, the T-4 is provided with a tower top condenser, and gas phase extracted from the tower top is sent to be used as fuel gas; the tower kettle is provided with a reboiler, and water is circulated to the top of the T-3 tower after the tower kettle is stripped.
The extraction tower T-3 adopts a plate tower or a packed tower, the operating pressure is 0.3MPaG to 1.8MPaG, and the preferable operating pressure is 0.8MPaG to 1.5 MPaG; the operating temperature is 10 ℃ to 55 ℃, and the preferred operating temperature is 20 ℃ to 45 ℃. The temperature of the extractant circulating water sent to the extraction tower T-3 is 10 ℃ to 55 ℃, and the preferred operation temperature is 20 ℃ to 45 ℃.
In operation, the content of hydrocarbon oxides in the top discharge of the extraction tower T-3 is controlled to be 10ppm to 200ppm, and the preferable control value is 80ppm to 150 ppm.
Comparative example 1
As shown in figure 1, the reaction product gas S1 after heat recovery and quenching, the material S-2 after compression by the product gas compressor C-1, and the material S-3 after cooling by circulating water in the cooler E-1 are sent to the oxide removal tower T-1. Two sections of water washing are arranged at the upper section of the T-1, the second section of the T-1 adopts circulating washing water for washing, the first section of the T-1 tower kettle is washed by supplementary clean water, and the T-1 tower kettle water is sent to a stripping tower T-2 after being subjected to heat exchange and temperature rise by a heat exchanger E-2. In T-2, the washed oxides, the carbon tetrads and the noncondensable gas are stripped, and S6 is extracted from the top of the tower and is used as fuel gas. The stripped tower bottom water S7 without oxide and carbon tetrahydrocarbon is cooled by a heat exchanger E-2 and a cooler E-3 respectively, one part of the stripped tower bottom water is sent to T-1 to be used as second-stage washing water, and the other part of the stripped tower bottom water S13 is used as waste water for extraction. And (3) extracting the overhead gas S10 of the oxide removal tower T-1, and then sending the overhead gas to oil absorption desorption units A and D to respectively obtain crude butadiene S12 and tail gas S11.
TABLE 2 comparison of operating parameters of two plant process flows
Table 2 is a comparison of the process flow parameters for the two devices. As can be seen from the data in Table 2, the utility model discloses the device all is superior to the device of figure 1 in the consumption of public work consumption, fresh wash water, and the tower footpath is littleer. Namely, the hydrocarbon oxide in the crude butadiene is controlled under the requirement of the same control index, the utility model has more advantages.
The utility model provides a crude butadiene oxide removal process which has considerable economic benefits. The embodiments are described in detail, and those skilled in the relevant art can implement the technology by making appropriate changes, modifications and combinations according to the method provided by the present invention. It is expressly stated that all such modifications or alterations and subcombinations which would be apparent to persons skilled in the art by making similar changes or variations to the process flow provided by the present invention are deemed to be within the spirit, scope and content of the invention.
Claims (5)
1. An apparatus for removing oxides from crude butadiene produced by oxidative dehydrogenation of butene, comprising a reaction product gas (S1) from an oxidative dehydrogenation reactor after heat recovery, quenching and acid washing, characterized in that, along the direction of material flow, said apparatus comprises means connected in the following manner: the method comprises the following steps that reaction generated gas (S1) is compressed by a generated gas compressor (C-1), and then directly enters an oil absorption desorption unit (A & D) after being cooled by a cooler (E-1), carbon four components (S15) separated by the oil absorption desorption unit (A & D) enter an extraction tower (T-3) from the bottom, extractant circulating water (S9) enters the extraction tower (T-3) from the top, tower kettle water (S4) of the extraction tower (T-3) is connected with a heat exchanger (E-12), the extraction tower enters a stripping rectification tower (T-4) from the middle part after being subjected to heat exchange and temperature rise, the stripping rectification tower (T-4) is provided with a tower top condenser, and gas phase extracted from the tower top is sent to be used as fuel gas; the tower kettle of the stripping and rectifying tower (T-4) is provided with a reboiler, and the tower kettle water is circulated back to the extraction tower (T-3) after passing through a heat exchanger (E-12).
2. The apparatus for removing oxides from crude butadiene produced by oxidative dehydrogenation of butene according to claim 1, wherein the tail gas (S11) separated by the oil absorption and desorption unit (A & D) is discharged after being connected with a tail gas treatment device.
3. The apparatus for removing oxides from crude butadiene produced by oxidative dehydrogenation of butene according to claim 1, wherein said extraction column (T-3) is washed with a single-stage counter-current of circulating water.
4. The apparatus for removing oxides from crude butadiene produced by oxidative dehydrogenation of butene according to claim 1, wherein said extraction column (T-3) is a tray column or a packed column.
5. The apparatus for removing oxides from crude butadiene produced by oxidative dehydrogenation of butene according to claim 1, wherein the operating pressure of said extraction column (T-3) is from 0.3mpa g to 1.8mpa g, and the operating temperature is from 10 ℃ to 55 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115999315A (en) * | 2021-10-21 | 2023-04-25 | 中国石油化工股份有限公司 | Internal heat integration type absorption stabilization process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115999315A (en) * | 2021-10-21 | 2023-04-25 | 中国石油化工股份有限公司 | Internal heat integration type absorption stabilization process |
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