CN112442388B - System and method for oxidizing and regenerating desulfurized alcohol alkali liquor - Google Patents
System and method for oxidizing and regenerating desulfurized alcohol alkali liquor Download PDFInfo
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- CN112442388B CN112442388B CN201910804034.9A CN201910804034A CN112442388B CN 112442388 B CN112442388 B CN 112442388B CN 201910804034 A CN201910804034 A CN 201910804034A CN 112442388 B CN112442388 B CN 112442388B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/12—Liquefied petroleum gas
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G19/00—Refining hydrocarbon oils in the absence of hydrogen, by alkaline treatment
- C10G19/08—Recovery of used refining agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Abstract
The invention relates to a system and a method for regenerating a desulfurized alcohol alkali liquor by oxidation, wherein the system comprises an oxygen-enriched gas inlet, an oxygen-enriched gas backflushing liquid bag, an alkali liquor oxidation tower and a gas circulation pipeline arranged outside the alkali liquor oxidation tower, and the alkali liquor oxidation tower is provided with an alkali-enriched liquid inlet, an excess gas outlet and a regenerated alkali liquor outlet; an oxygen-enriched gas distributor is arranged in the alkali liquor oxidation tower, and an oxygen-enriched gas inlet, an oxygen-enriched gas backflushing liquid bag and the inlet of the oxygen-enriched gas distributor are sequentially communicated along the oxygen-enriched gas flow direction; the excess gas outlet is arranged at the top of the alkali liquor oxidation tower; the inlet end of the gas circulation pipeline is communicated with the excess gas outlet, and the outlet end of the gas circulation pipeline is communicated with the inside of the alkali liquor oxidation tower; and an excess gas boosting device is arranged on the gas circulating pipeline. The method realizes zero consumption of fuel gas and zero emission of waste gas, and the oxygen-rich gas distributor in the alkali liquor oxidation tower can be cleaned on line, so that the oxidation regeneration efficiency of the desulfurized alcohol alkali liquor and the operation safety of the system are improved.
Description
Technical Field
The disclosure relates to the technical field of petrochemical industry, in particular to a system and a method for regenerating desulfurized alcohol alkali liquor by oxidation.
Background
The process uses alkali liquor as a mercaptan extraction agent to extract mercaptan in liquefied gas or gasoline into the alkali liquor and generate sodium mercaptan so that the concentration of mercaptan sulfur in the liquefied gas or gasoline product meets the product requirement. In the above-mentioned processing procedure, in order to recycle the lye, the lye containing sodium alcoholate must be subjected to an oxidative regeneration treatment. The alkali liquor oxidation regeneration process is a process of reacting sodium mercaptide in the alkali liquor with oxygen to generate disulfide and sodium hydroxide under the action of a catalyst.
The prior art adopts a method of injecting excess factory air, and a large amount of excess gas is discharged from the top of the alkali liquor oxidation tower and mainly comprises the excess air, a small amount of hydrocarbon,Water, sulfides, and the like. Usually, the excess gas is discharged as waste gas and burned, because the gas contains O 2 And hydrocarbons, many enterprises adopt a method of supplementing fuel gas into the exhaust gas to ensure the safety of the exhaust gas, and then send the mixed gas to a heating furnace or an incinerator for combustion treatment. When the sulfides in the mixed gas are sent to a heating furnace or an incinerator along with the mixed gas, the problems of corrosion of a conveying pipeline, over-standard sulfur dioxide generated by combustion and the like can be caused. In addition, in the production operation, the gas distributor in the alkali liquor oxidation tower needs to be immersed in the alkali liquor, so that the injection amount of factory wind is greatly reduced when abnormal conditions such as blockage occur, the alkali liquor oxidation reaction is influenced, the alkali liquor oxidation regeneration effect is reduced, the alkali liquor regeneration is incomplete, and the discharge amount of waste alkali is increased.
In addition, the existing alkali liquor regeneration system and method have low production efficiency, the alkali liquor oxidation regeneration capacity is difficult to expand, and the exhaust emission is difficult to adapt to increasingly strict environmental requirements.
Disclosure of Invention
The device and the method can enlarge the treatment capacity of an alkali liquor oxidation tower, realize no waste gas emission, no fuel gas consumption and online cleaning of a gas distributor in the tower, and obviously improve the alkali liquor regeneration efficiency and the safety and reliability of the system.
In order to achieve the above object, a first aspect of the present disclosure provides a system for regenerating a desulfurized alcohol alkali solution by oxidation, the system comprising an oxygen-enriched gas inlet, an oxygen-enriched gas backflushing liquid packet, an alkali solution oxidation tower and a gas circulation pipeline arranged outside the alkali solution oxidation tower, wherein the alkali solution oxidation tower is provided with an alkali-enriched liquid inlet, an excess gas outlet and a regenerated alkali solution outlet;
an oxygen-enriched gas distributor is arranged in the alkali liquor oxidation tower, and the oxygen-enriched gas inlet, the oxygen-enriched gas backflushing liquid bag and the inlet of the oxygen-enriched gas distributor are sequentially communicated along the oxygen-enriched gas flow direction;
the excess gas outlet is arranged at the top of the alkali liquor oxidation tower; the inlet end of the gas circulating pipeline is communicated with the excess gas outlet, and the outlet end of the gas circulating pipeline is communicated with the inside of the alkali liquor oxidation tower; and an excess gas boosting device is arranged on the gas circulation pipeline.
Optionally, the upper part of the alkali liquor oxidation tower is provided with a nitrogen inlet, the nitrogen inlet is connected with a nitrogen inlet pipe, and the nitrogen inlet pipe is provided with a pressure regulating valve.
Optionally, the system further comprises an excess gas backflushing liquid bag and an excess gas distributor; the excess gas backflushing liquid bag is arranged between the excess gas boosting device and the outlet end of the gas circulation pipeline, the excess gas distributor is arranged at the lower part in the alkali liquor oxidation tower, and the outlet end of the gas circulation pipeline is communicated with the inlet of the excess gas distributor; alternatively, the first and second electrodes may be,
and the outlet end of the gas circulation pipeline is communicated with the alkali-rich liquid inlet.
Optionally, the oxygen-enriched gas inlet is communicated with the oxygen-enriched gas backflushing liquid bag through an oxygen-enriched gas inlet pipe; an inlet pipe of the oxygen-enriched backflushing liquid bag is connected with an oxygen-enriched gas cut-off valve which can be opened and closed, so that the oxygen-enriched gas cut-off valve is closed to carry out online backflushing on the oxygen-enriched gas distributor;
an inlet pipe of the excess gas backflushing liquid bag is connected with an excess gas cut-off valve which can be opened and closed; to perform on-line backwash on the excess gas distributor by closing the excess gas shutoff valve;
the oxygen-enriched distributor is provided with oxygen-enriched injection holes to form an outlet of the oxygen-enriched distributor, the diameter of each oxygen-enriched injection hole is 0.1-2mm, and the injection direction is vertical downward and/or inclined downward;
the excess gas distributor is provided with excess gas injection holes to form an outlet of the excess gas distributor, the diameter of each excess gas injection hole is 0.1-2mm, and the injection direction is vertical downward and/or obliquely downward.
Optionally, an online component analyzer is arranged on the gas circulation pipeline and used for detecting the oxygen concentration of the excess gas at the excess gas outlet; an oxygen-enriched gas flow regulating valve is arranged on the oxygen-enriched gas inlet pipe, and the online component analyzer is connected with the oxygen-enriched gas flow regulating valve through an electric signal so as to regulate the oxygen-enriched gas flow at the oxygen-enriched gas inlet according to the oxygen concentration.
In order to achieve the above object, a second aspect of the present disclosure provides a method for oxidative regeneration of mercaptan removal using the system according to the first aspect of the present disclosure, the method comprising the steps of:
under the condition of alkali liquor oxidation regeneration reaction, making the oxygen-enriched gas raw material sequentially pass through an oxygen-enriched gas back flushing liquid bag and an oxygen-enriched gas distributor and enter an alkali liquor oxidation tower to contact with an alkali-enriched liquid to obtain regenerated alkali liquor and excess gas;
boosting the pressure of the excess residual gas to obtain boosted excess residual gas, and returning the boosted excess gas to the alkali liquor oxidation tower for recycling;
wherein the concentration of oxygen in the oxygen-enriched gas is 90 vol% or more.
Optionally, the method further comprises: enabling the boosted excess gas to sequentially pass through a residual gas backflushing liquid bag and an excess gas distributor and return to the alkali liquor oxidation tower; or, the residual gas after pressure increase and the alkali-rich liquid are mixed and then enter the alkali oxidation tower;
wherein the pressure of the residual gas after pressure increase is 0.4-0.7MPaG, and the temperature is 40-55 ℃.
Optionally, an openable oxygen-enriched gas shutoff valve is arranged at an inlet of the oxygen-enriched backflushing liquid bag, and an openable surplus gas shutoff valve is arranged at an inlet of the excess gas backflushing liquid bag; the method further comprises the following steps:
when the oxygen-enriched gas distributor is abnormally operated, closing the oxygen-enriched gas cut-off valve to enable alkali liquor in the alkali liquor oxidation tower to flow back into the oxygen-enriched back flushing liquid bag through the oxygen-enriched gas distributor so as to form on-line back flushing of the oxygen-enriched gas distributor;
and when the excess gas distributor is abnormally operated, closing the excess gas cut-off valve to enable the alkali liquor in the alkali liquor oxidation tower to flow back into the excess gas backflushing liquid bag through the excess gas distributor so as to form online backflushing on the excess gas distributor.
Optionally, the alkali liquor oxidation regeneration reaction conditions comprise: the pressure is 0.30-0.70MPaG, and the temperature is 40-55 ℃;
the oxygen concentration of the reaction section at the lower part of the alkali liquor oxidation tower is more than 30 volume percent; the oxygen concentration in the excess gas is 10-30% by volume;
the method further comprises the following steps: and enabling nitrogen to enter the alkali liquor oxidation tower through a pressure regulating valve, and regulating the pressure in the alkali liquor oxidation tower through the pressure regulating valve.
Optionally, the method further comprises detecting the oxygen concentration of the excess gas using an online component analyzer, and adjusting the flow of oxygen-rich gas to the lye oxidation tower according to the oxygen concentration.
The system and the method disclosed by the invention can improve the processing capacity of the alkali liquor regeneration tower and the oxygen concentration of the reaction section at the lower part of the alkali liquor oxidation tower, reduce the excess gas amount at the top of the alkali liquor regeneration tower, and realize the circulation of the excess gas, no waste gas discharge and no fuel gas consumption by the mode of regenerating the mercaptan-removed alkali liquor by using the oxygen-rich gas and returning the excess gas to the regeneration tower for recycling; meanwhile, the use of the oxygen-enriched gas backflushing liquid bag realizes the online cleaning of the distributor in the tower, eliminates the local blockage of the gas distributor in the tower, further improves the oxidation regeneration efficiency of the desulfurized alcohol alkali liquid and the operation safety of the system, and reduces the waste alkali discharge.
Additional features and advantages of the disclosure will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure without limiting the disclosure. In the drawings:
FIG. 1 is a process flow diagram of one embodiment of the presently disclosed system for the oxidative regeneration of a desulfurized alcohol lye.
FIG. 2 is a process flow diagram of a sweetening alcohol lye oxidation regeneration device in a comparative example of the present disclosure.
Description of the reference numerals
Device
1. Flow regulating valve 2, oxygen-enriched gas back flushing liquid bag 3, alkali liquor oxidation tower
4. Oxygen-rich gas distributor 5, pressure regulating valve 6, on-line component analyzer
7. Excess gas pressure boosting device 8, excess gas back flushing liquid bag 9 and excess gas distributor
Logistics
11. Rich oxygen 12, nitrogen 13, excess gas
14. Rich alkali liquor 15, regenerated alkali liquor 16, factory air
17. Fuel gas 18. waste gas
Detailed Description
The following detailed description of specific embodiments of the present disclosure is provided in connection with the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present disclosure, are given by way of illustration and explanation only, not limitation.
In the present disclosure, unless otherwise stated, the use of directional words such as "up" and "down" generally refers to the up and down of the device in normal use, and specifically refers to the orientation of the drawing in fig. 1. "inner and outer" are meant to refer to the profile of the device itself.
As shown in fig. 1, a first aspect of the present disclosure provides a system for regenerating a desulfurized alcohol lye through oxidation, the system comprises an oxygen-rich gas inlet, an oxygen-rich gas backflushing liquid package 2, a lye oxidation tower 3 and a gas circulation pipeline arranged outside the lye oxidation tower 3, wherein the lye oxidation tower 3 is provided with an oxygen-rich liquid inlet, an excess gas outlet and a regenerated lye outlet; an oxygen-enriched gas distributor 4 is arranged in the alkali liquor oxidation tower 3, and an oxygen-enriched gas inlet, an oxygen-enriched gas backflushing liquid bag 2 and an inlet of the oxygen-enriched gas distributor 4 are sequentially communicated along the oxygen-enriched gas flow direction; the excess gas outlet is arranged at the top of the alkali liquor oxidation tower 3; the inlet end of the gas circulation pipeline is communicated with the excess gas outlet, and the outlet end of the gas circulation pipeline is communicated with the inside of the alkali liquor oxidation tower 3; the gas circulation line is provided with an excess gas booster 7.
The system and the method disclosed by the invention can improve the processing capacity of the alkali liquor regeneration tower and the oxygen concentration of the reaction section at the lower part of the alkali liquor oxidation tower, reduce the excess gas amount at the top of the alkali liquor regeneration tower, and realize the circulation of the excess gas, no waste gas discharge and no fuel gas consumption by the mode of regenerating the mercaptan-removed alkali liquor by using the oxygen-rich gas and returning the excess gas to the regeneration tower for recycling; meanwhile, the use of the oxygen-enriched gas backflushing liquid bag realizes the online cleaning of the distributor in the tower, eliminates the local blockage of the gas distributor in the tower, further improves the oxidation regeneration efficiency of the desulfurized alcohol alkali liquid and the operation safety of the system, and reduces the waste alkali discharge.
The lye oxidation towers in the regeneration system may be of a type conventional in the art in light of this disclosure, which is not specifically intended. The excess gas boosting device may be one of a liquid ring compressor, a reciprocating compressor or a screw compressor, preferably a liquid ring compressor.
In order to facilitate the adjustment of the pressure in the alkali oxidation tower, in one embodiment of the present disclosure, as shown in fig. 1, the upper portion of the alkali oxidation tower 3 may be provided with a nitrogen inlet, the nitrogen inlet may be connected with a nitrogen inlet pipe, and the nitrogen inlet pipe may be provided with a pressure adjusting valve 5. The flow of nitrogen gas entering the alkali liquor oxidation tower can be adjusted by the pressure adjusting valve 5 so as to maintain the normal pressure in the tower and the normal operation of the regeneration process.
In order to further promote the distribution of the excess gas in the lye regeneration tower and improve the efficiency of lye regeneration according to the present disclosure, in one embodiment of the present disclosure, as shown in fig. 1, the system may comprise an excess gas distributor 9, the excess gas distributor 9 may be disposed in the lye regeneration tower, preferably in the lower part of the tower, more preferably below the oxygen-rich gas distributor 4; the outlet end of the gas circulation pipeline can be communicated with the inlet of the excess gas distributor 9, so that the excess gas 13 in the regeneration system is uniformly distributed in the alkali liquor oxidation tower 3 through the residual gas distributor 9 after being boosted by the excess gas boosting device 7 of the gas circulation pipeline; further, in order to prevent the blockage of the excess gas distributor and realize the online back flushing of the distributor, the system can also comprise an excess gas back flushing liquid bag 8; the excess gas backflushing liquid pack 8 may be provided between the excess gas pressure rising device 7 and the outlet end of the gas circulation line. In another embodiment of the present disclosure, the outlet end of the gas circulation line may be communicated with the rich lye inlet, so that the excess gas and the rich lye are mixed and then enter the lye regeneration tower.
In the method according to the present disclosure, the surplus gas backflushing liquid packet and the oxygen-rich gas backflushing liquid packet may be of a type conventional in the art, without particular limitation, and in one embodiment of the present disclosure, the oxygen-rich gas 11 inlet is communicated with the oxygen-rich gas backflushing liquid packet 4 through the oxygen-rich gas 11 inlet pipe; the upstream of the oxygen-enriched back flushing liquid bag 2 can be connected with an oxygen-enriched gas cut-off valve which can be opened and closed, so that when the oxygen-enriched gas distributor 4 is abnormally operated, the oxygen-enriched gas cut-off valve is closed to carry out on-line back flushing on the oxygen-enriched gas distributor 4; wherein the abnormal operation of the oxygen-rich gas distributor 4 means that the oxygen-rich gas distributor 4 is blocked, unsmooth and the like. Specifically, the oxygen-enriched gas shutoff valve may be disposed on an inlet line of the oxygen-enriched gas backflushing liquid pack.
In one embodiment, an openable excess gas shutoff valve may be connected upstream of the excess gas backflushing liquid pack 8; to perform on-line back flushing of the surplus gas distributor 9 by closing the surplus gas shut-off valve when the surplus gas distributor 9 is abnormally operated. The abnormal operation of the excess gas distributor 9 means that the excess gas distributor 9 is blocked or unsmooth. In particular, the excess gas shutoff valve may be provided on the inlet line of the excess gas backflush cartridge.
The backflushing liquid bag disclosed by the invention can realize online flushing treatment on the distributor, and further improves the production efficiency of the device and the safety and reliability of the system.
In one embodiment of the present disclosure, the oxygen-rich gas distributor 4 may be provided with oxygen-rich gas injection holes to form the outlet of the oxygen-rich gas distributor 4, the diameter of the oxygen-rich gas injection holes may be 0.1-2mm, preferably 0.2-1mm, and the injection direction of the oxygen-rich gas injection holes is vertically downward and/or obliquely downward; the excess gas distributor 9 can be provided with excess gas injection holes to form the outlet of the excess gas distributor 9, the diameter of the excess gas injection holes can be 0.1-2mm, preferably 0.2-1mm, and the injection direction of the excess gas injection holes is preferably vertically downward and/or obliquely downward. So as to uniformly distribute the oxygen-rich gas and the surplus gas in the alkali liquor oxidation tower 3 to be fully contacted with the alkali-rich liquid, thereby improving the reaction efficiency and the conversion rate.
In one embodiment of the present disclosure, the gas circulation line may be provided with an on-line component analyzer 6 for detecting the oxygen concentration of the excess gas at the excess gas outlet, which may be of a type conventional in the art, without particular requirement of the present disclosure. Further, an oxygen-enriched air flow regulating valve 1 can be arranged on the oxygen-enriched air inlet pipe, and the online component analyzer 6 can be connected with the oxygen-enriched air flow regulating valve 1 through an electric signal so as to regulate the oxygen-enriched air flow at the oxygen-enriched air inlet according to the oxygen concentration.
A second aspect of the present disclosure provides a method for oxidative regeneration of a sweetening agent using the system of the first aspect of the present disclosure, the method comprising the steps of: under the condition of alkali liquor oxidation regeneration reaction, oxygen-enriched gas raw materials sequentially pass through an oxygen-enriched gas back flushing liquid bag 2 and an oxygen-enriched gas distributor 4 to enter an alkali liquor oxidation tower 3 and contact with an alkali-enriched liquid to obtain regenerated alkali liquor 15 and excess gas 13; the excess gas 13 is boosted to obtain boosted excess gas, and the boosted excess gas is returned to the alkali liquor oxidation tower 3 for recycling; the oxygen concentration in the oxygen-rich gas may be 90 vol% or more, and preferably 95 to 98 vol%.
The method adopts an oxygen-enriched gas injection mode, reduces the volume flow of injected gas while ensuring the oxygen consumption, circulates the excess gas obtained by reaction and returns the excess gas to the alkali liquor oxidation tower for use, and realizes zero consumption of fuel gas and zero emission of waste gas; the method also realizes the on-line back washing of the oxygen-enriched distributor, and improves the oxidation regeneration efficiency of the desulfurized alcohol alkali liquor and the operation safety of the system.
In one embodiment of the present disclosure, as shown in fig. 1, the pressurized excess gas may be returned to the lye oxidation tower 3 through the excess gas distributor 9 so as to uniformly distribute the excess gas in the lye oxidation tower; further, the pressurized residual gas can enter the residual gas distributor 9 after passing through the residual gas backflushing liquid bag 8, so that the residual gas backflushing liquid bag 8 is controlled to perform online backflushing on the residual gas distributor, and the distributor is prevented from being blocked. In another embodiment, the pressure-increased residual gas can be mixed with the rich alkali liquor 14 and then enter the alkali liquor oxidation tower 3.
In the process according to the present disclosure, the pressure of the pressure-boosted residual gas may vary within a wide range, for example the pressure of the pressure-boosted residual gas may be from 0.4 to 0.7MPaG and the temperature may be from 40 to 55 ℃; preferably, the pressure of the pressure-raised residual gas is 0.45-0.55MPaG and the temperature is 45-50 ℃. The excess gas in the pressure and temperature ranges can be fully contacted with the alkali-rich liquid to participate in the reaction, so that the reaction efficiency is improved.
According to the method disclosed by the invention, the surplus gas backflushing liquid bag and the oxygen-enriched gas backflushing liquid bag can be of conventional types in the field, and are not particularly limited, in one specific embodiment of the disclosure, an oxygen-enriched gas cut-off valve which can be opened and closed can be arranged at the inlet of the oxygen-enriched gas backflushing liquid bag 2, when the oxygen-enriched gas distributor 4 is abnormally operated, the oxygen-enriched gas cut-off valve can be closed, so that alkali liquor in the alkali liquor oxidation tower 3 flows back into the oxygen-enriched gas backflushing liquid bag 2 through the oxygen-enriched gas distributor 4, online backflushing is carried out on the oxygen-enriched gas distributor 4, the blockage of the oxygen-enriched gas distributor is prevented, and the safe operation is ensured. Wherein the oxygen-enriched gas distributor operational anomaly may include at least one of a blockage, an obstruction.
In one embodiment of the present disclosure, an inlet of the excess gas backflushing liquid bag 8 may be provided with an excess gas shutoff valve that can be opened and closed; when the excess gas distributor 9 is abnormally operated, the excess gas cut-off valve can be closed, so that the alkali liquor in the alkali liquor oxidation tower 3 flows back into the excess gas backwashing liquid bag 8 through the excess gas distributor 9, the excess gas distributor 9 is subjected to online backwashing, the blockage of the excess gas distributor is prevented, and the regeneration efficiency and the operation safety of the mercaptan removal alkali liquor oxidation tower are improved.
In one embodiment of the present disclosure, the alkali oxidation regeneration reaction conditions may vary within a wide range, and preferably, the alkali oxidation regeneration reaction conditions may include: the pressure is 0.30-0.70MPaG, and the temperature is 40-55 ℃; further preferably, the pressure is 0.45-0.55MPaG and the temperature is 45-50 ℃.
In the method disclosed by the invention, the oxygen concentration in the alkali oxidation tower can be increased by adopting oxygen-rich gas and circulating the excess gas into the alkali oxidation tower, and preferably, the oxygen concentration in the lower reaction section of the alkali oxidation tower is more than 30 volume percent, and more preferably 35-40 volume percent; further, the volume flow rate of the excess gas obtained from the outlet of the alkali liquor oxidation tower is reduced, the excess gas is not discharged outside, and the oxygen concentration in the excess gas can be 10-30 vol%, more preferably 15-25 vol%.
In one embodiment of the present disclosure, an inert gas may be introduced into the lye oxidation tower 3 to adjust the pressure therein, for example, as shown in FIG. 1, nitrogen gas 12 may be introduced into the lye oxidation tower 3 through a pressure regulating valve, and the amount of nitrogen gas introduced may be adjusted by a pressure regulating valve 5 to adjust the pressure therein the lye oxidation tower 3.
In one embodiment of the present disclosure, the oxygen concentration of the excess gas may be detected using an online component analyzer, for example, an online component analyzer is disposed at the excess gas outlet of the lye oxidation tower to detect the oxygen concentration of the excess gas at the outlet; further, the flow rate of the oxygen-enriched gas to be introduced into the lye oxidation tower may be adjusted in accordance with the detected oxygen concentration of the excess gas, for example, in a further embodiment, an on-line composition analyzer 6 may be provided on the excess gas circulation line to detect the oxygen concentration of the excess gas, and the on-line composition analyzer may be electrically connected to the oxygen-enriched gas flow regulating valve to adjust the flow rate of the oxygen-enriched gas 11 to be introduced into the lye oxidation tower in accordance with the detected oxygen concentration.
According to the present disclosure, the source of the oxygen-rich gas is not particularly limited and may be from a system oxygen pipe network, an oxygen cylinder; the oxygen concentration in the excess gas obtained from the excess gas outlet of the lye oxidation tower can vary within certain limits, for example the oxygen concentration can be in the range of 10 to 30% by volume, preferably 15 to 25% by volume.
The present disclosure is further illustrated by the following examples, but is not to be construed as being limited thereby.
Comparative example
The process flow of the existing alkali liquor oxidation regeneration system is shown in figure 2 and comprises the following steps:
introducing plant air 16 (with the oxygen concentration of 21 vol%) and an alkali-rich liquid 14 into an alkali oxidation tower 3, and carrying out oxidation regeneration reaction by contacting the plant air and the alkali-rich liquid with the reaction temperature of 40 ℃, the reaction pressure of 0.55MPaG and the oxygen concentration of 21 vol% in a reaction section at the lower part of the alkali oxidation tower; excess gas 13 (volume) obtained in the reactionFlow rate of 9.7m 3 And/h) leading out from the top of the tower, regulating the pressure by a pressure regulating valve 5, mixing with fuel gas 17 to obtain waste gas 18, and sending the waste gas 18 to a heating furnace or an incinerator for combustion treatment. The alkali liquor treatment capacity of the system is 14m 3 /h。
Examples
The mercaptan-removing lye oxidation regeneration system shown in the figure 1 (the diameter and the height of the lye oxidation tower device are the same as those in the comparative example) is adopted, and the system comprises: the device comprises a flow regulating valve 1, an oxygen-enriched gas back flushing liquid bag 2, an alkali liquor oxidation tower 3, an oxygen-enriched gas distributor 4, a pressure regulating valve 5, an online component analyzer 6, an excess gas pressure boosting device 7, an excess gas back flushing liquid bag 8 and an excess gas distributor 9. The method for carrying out the oxidative regeneration comprises the following steps:
a. oxygen-enriched gas 11 (the oxygen concentration is 90 volume percent) enters the inlet of the oxygen-enriched gas back flushing liquid bag 2 through the flow regulating valve 1;
b. oxygen-enriched gas obtained by back flushing the liquid bag outlet with the oxygen-enriched gas in the step a enters an oxygen-enriched gas inlet at the lower part of the alkali liquor oxidation tower 3;
c. the oxygen-enriched gas in the step b is uniformly sprayed into the alkali oxidation tower 3 through an oxygen-enriched gas distributor 4 connected with an oxygen-enriched gas inlet of the alkali oxidation tower, and contacts with the alkali-enriched liquid to carry out oxidation regeneration reaction, wherein the reaction temperature is 40 ℃, the reaction pressure is 0.55MPaG, and the oxygen concentration of a reaction section at the lower part of the alkali oxidation tower is 40 volume percent;
e. excess gas 13 (volume flow 4 m) obtained by the reaction 3 H, the oxygen concentration is 23 vol%) is discharged from the top of the alkali liquor oxidation tower 3 and enters an inlet of an online component analyzer 6;
f. the excess gas (oxygen concentration 23 vol%) obtained at the outlet of the online component analyzer in the step e enters the inlet of the excess gas pressure boosting device 7;
g. step f, enabling the boosted excess gas obtained from the outlet of the excess gas boosting device to enter the inlet of an excess gas backflushing liquid bag 8, wherein the pressure of the boosted excess gas is 0.56MPaG, and the temperature is 40 ℃;
h. g, allowing the surplus gas obtained by backflushing the liquid bag outlet with the surplus gas in the step g to enter an excess gas inlet at the lower part of the alkali liquor oxidation tower 3;
i. and (h) uniformly spraying the excess gas in the step h into the alkali liquor oxidation tower through an excess gas distributor 9 connected with an excess gas inlet of the alkali liquor oxidation tower.
At this time, the alkali treatment capacity of the system was 18m 3 /h。
In the embodiment, the alkali liquor oxidation regeneration system has no waste gas discharge, no fuel gas is required to be supplemented, no fuel gas is consumed, the environmental protection requirement is met, the potential safety hazard is eliminated, the operation period of the alkali liquor oxidation regeneration system is prolonged, the gas distributor in the tower can be used for online treatment, the alkali liquor oxidation regeneration efficiency is ensured, and the safety and the reliability of the system operation are greatly improved.
The mercaptan-removing alkali liquor oxidation regeneration system of the embodiment can be modified on the basis of the existing system (such as the system in the comparative example), a flow regulating valve 1, an oxygen-enriched gas back-flushing liquid bag 2, an oxygen-enriched gas distributor 4, a pressure regulating valve 5, an online component analyzer 6, an excess gas pressure boosting device 7, an excess gas back-flushing liquid bag 8 and an excess gas distributor 9 are additionally arranged, an oxygen-enriched gas inlet is additionally arranged at the lower part of an alkali liquor oxidation tower, the control mode of the operation pressure of the alkali liquor oxidation tower is modified into control and adjustment of the injection quantity of nitrogen at the upper part of the tower by controlling and adjusting the discharge quantity of excess gas at the top of the tower, the control and adjustment of the injection quantity of the oxygen-enriched gas are increased, the oxygen concentration of a reaction section at the lower part of the alkali liquor oxidation tower is improved, the total gas volume flow quantity injected into the tower is reduced, the excess gas is circulated back to the lower part of the tower from the top of the alkali liquor oxidation tower, an external waste gas winding displacement, a fuel gas supplementing line and related facilities are cancelled, strengthens the on-line treatment facility of the excess gas distributor in the corresponding tower, and can solve the problems of the reduction of the regeneration efficiency of the alkali liquor and the increase of the discharge amount of the waste alkali.
By the mercaptan removal alkali liquor oxidation regeneration system and the mercaptan removal alkali liquor oxidation regeneration method, under the condition that the diameter and the height of an alkali liquor oxidation tower device are not changed, the treatment capacity of an alkali liquor regeneration tower is improved by 15-30%, the oxygen concentration of a reaction section at the lower part of the alkali liquor oxidation tower is improved and is not lower than 30% in volume, the surplus gas flow at the top of the alkali liquor regeneration tower is reduced by 30-60%, the circulation of excess gas, no exhaust gas discharge and no fuel gas consumption are realized, the problems of alkali liquor regeneration efficiency reduction and waste alkali discharge increase caused by local blockage of a gas distributor in the tower are solved, the environmental protection requirement is met, the potential safety hazard is eliminated, the alkali liquor oxidation regeneration efficiency is ensured, and the operation safety and the reliability of the system are improved.
The preferred embodiments of the present disclosure are described in detail with reference to the accompanying drawings, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all belong to the protection scope of the present disclosure.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various combinations that are possible in the present disclosure are not described again.
In addition, any combination of various embodiments of the present disclosure may be made, and the same should be considered as the disclosure of the present disclosure, as long as it does not depart from the spirit of the present disclosure.
Claims (9)
1. A system for oxidizing and regenerating desulfurized alcohol alkali liquor is characterized by comprising an oxygen-enriched gas inlet, an oxygen-enriched gas backflushing liquid bag, an alkali liquor oxidation tower and a gas circulation pipeline arranged outside the alkali liquor oxidation tower, wherein the alkali liquor oxidation tower is provided with an alkali-enriched liquid inlet, an excess gas outlet and a regenerated alkali liquor outlet;
an oxygen-enriched gas distributor is arranged in the alkali liquor oxidation tower, and the oxygen-enriched gas inlet, the oxygen-enriched gas backflushing liquid bag and the inlet of the oxygen-enriched gas distributor are sequentially communicated along the oxygen-enriched gas flow direction;
the excess gas outlet is arranged at the top of the alkali liquor oxidation tower; the inlet end of the gas circulation pipeline is communicated with the surplus gas outlet, and the outlet end of the gas circulation pipeline is communicated with the inside of the alkali liquor oxidation tower; an excess gas pressure boosting device is arranged on the gas circulation pipeline;
the oxygen-enriched distributor is provided with oxygen-enriched spraying holes to form an outlet of the oxygen-enriched distributor, and the spraying direction of the oxygen-enriched spraying holes is vertically downward and/or obliquely downward;
an openable oxygen-enriched gas cut-off valve is arranged at the inlet of the oxygen-enriched gas backflushing liquid bag; when the oxygen-enriched gas distributor is abnormally operated, closing the oxygen-enriched gas cut-off valve to enable alkali liquor in the alkali liquor oxidation tower to flow back into the oxygen-enriched back flushing liquid bag through the oxygen-enriched gas distributor so as to form on-line back flushing of the oxygen-enriched gas distributor;
the system also comprises an excess gas backflushing liquid bag and an excess gas distributor; the excess gas backflushing liquid bag is arranged between the excess gas boosting device and the outlet end of the gas circulation pipeline, the excess gas distributor is arranged at the lower part in the alkali liquor oxidation tower, and the outlet end of the gas circulation pipeline is communicated with the inlet of the excess gas distributor;
the oxygen-enriched gas inlet is communicated with the oxygen-enriched gas backflushing liquid bag through an oxygen-enriched gas inlet pipe; an inlet pipe of the oxygen-enriched backflushing liquid bag is connected with an oxygen-enriched gas cut-off valve which can be opened and closed, so that the oxygen-enriched gas cut-off valve is closed to carry out online backflushing on the oxygen-enriched gas distributor;
an inlet pipe of the excess gas backflushing liquid bag is connected with an excess gas cut-off valve which can be opened and closed; to perform on-line backwash on the excess gas distributor by closing the excess gas shutoff valve;
the excess gas distributor is provided with excess gas injection holes to form an outlet of the excess gas distributor, and the injection direction of the excess gas distributor is vertically downward and/or obliquely downward;
an inlet of the excess gas backflushing liquid bag is provided with an excess gas cut-off valve which can be opened and closed; and when the excess gas distributor is abnormally operated, closing the excess gas cut-off valve to enable the alkali liquor in the alkali liquor oxidation tower to flow back into the excess gas backflushing liquid bag through the excess gas distributor so as to form online backflushing on the excess gas distributor.
2. The system of claim 1, wherein the upper part of the lye oxidation tower is provided with a nitrogen inlet which is connected with a nitrogen inlet pipe, and the nitrogen inlet pipe is provided with a pressure regulating valve.
3. The system of claim 1, wherein an outlet end of the gas recycle line is in communication with the rich liquor inlet.
4. The system of claim 1, wherein the oxygen-rich injection holes are 0.1-2mm in diameter; the diameter of the residual gas spraying hole is 0.1-2 mm.
5. The system according to claim 1, wherein an on-line component analyzer is provided on the gas circulation line for detecting an oxygen concentration of the excess gas at the excess gas outlet; an oxygen-enriched gas flow regulating valve is arranged on the oxygen-enriched gas inlet pipe, and the online component analyzer is connected with the oxygen-enriched gas flow regulating valve through an electric signal so as to regulate the oxygen-enriched gas flow at the oxygen-enriched gas inlet according to the oxygen concentration.
6. A method for oxidative regeneration of a sweetening lye by using the system of any of claims 1 to 5, characterized in that the method comprises the following steps:
under the condition of alkali liquor oxidation regeneration reaction, making the oxygen-enriched gas raw material sequentially pass through an oxygen-enriched gas back flushing liquid bag and an oxygen-enriched gas distributor and enter an alkali liquor oxidation tower to contact with an alkali-enriched liquid to obtain regenerated alkali liquor and excess gas;
boosting the pressure of the excess residual gas to obtain boosted excess residual gas, and returning the boosted excess gas to the alkali liquor oxidation tower for recycling;
wherein the concentration of oxygen in the oxygen-enriched gas is 90 vol% or more.
7. The method of claim 6, wherein the method further comprises: enabling the boosted excess gas to sequentially pass through a residual gas backflushing liquid bag and an excess gas distributor and return to the alkali liquor oxidation tower; or, the residual gas after pressure increase and the alkali-rich liquid are mixed and then enter the alkali oxidation tower;
wherein the pressure of the residual gas after pressure increase is 0.4-0.7MPaG, and the temperature is 40-55 ℃.
8. The method of claim 6, wherein the lye oxidation regeneration reaction conditions comprise: the pressure is 0.30-0.70MPaG, and the temperature is 40-55 ℃;
the oxygen concentration of the reaction section at the lower part of the alkali liquor oxidation tower is more than 30 volume percent; the oxygen concentration in the excess gas is 10-30% by volume;
the method further comprises the following steps: and enabling nitrogen to enter the alkali liquor oxidation tower through a pressure regulating valve, and regulating the pressure in the alkali liquor oxidation tower through the pressure regulating valve.
9. The method of claim 6, further comprising detecting an oxygen concentration of the excess gas using an on-line composition analyzer and adjusting a flow rate of oxygen-rich gas to the caustic oxidation tower based on the oxygen concentration.
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| CN204058377U (en) * | 2014-09-02 | 2014-12-31 | 徐振华 | A kind of mercaptan oxidation and alkali liquor oxidized regenerating unit |
| CN104263403A (en) * | 2014-09-02 | 2015-01-07 | 徐振华 | Method and device for deep oxidation of sweetening alkali liquor and separation of disulfide |
| CN104711023A (en) * | 2015-03-11 | 2015-06-17 | 郝天臻 | Treatment method for liquefied petroleum gas sweetening tail gas and alkaline residues and special equipment used in method |
| CN109929583A (en) * | 2019-03-21 | 2019-06-25 | 宁波章甫能源科技有限公司 | A kind of device and method of the liquid hydrocarbon mercaptan removal alkali liquid regeneration of tail gas zero-emission |
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| CN204058377U (en) * | 2014-09-02 | 2014-12-31 | 徐振华 | A kind of mercaptan oxidation and alkali liquor oxidized regenerating unit |
| CN104263403A (en) * | 2014-09-02 | 2015-01-07 | 徐振华 | Method and device for deep oxidation of sweetening alkali liquor and separation of disulfide |
| CN104711023A (en) * | 2015-03-11 | 2015-06-17 | 郝天臻 | Treatment method for liquefied petroleum gas sweetening tail gas and alkaline residues and special equipment used in method |
| CN109929583A (en) * | 2019-03-21 | 2019-06-25 | 宁波章甫能源科技有限公司 | A kind of device and method of the liquid hydrocarbon mercaptan removal alkali liquid regeneration of tail gas zero-emission |
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