CN113385004B - Desulfurization method and device for sulfur production tail gas - Google Patents
Desulfurization method and device for sulfur production tail gas Download PDFInfo
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/34—Chemical or biological purification of waste gases
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- B01D2257/30—Sulfur compounds
- B01D2257/308—Carbonoxysulfide COS
Abstract
The invention provides a desulfurization method and a desulfurization device for sulfur production tail gas, wherein the desulfurization method comprises the following steps: carrying out a first reaction on the sulfur production tail gas and oxygen-containing gas in a converter to obtain a first-stage process gas; wherein the first reaction satisfies: oxidizing the sulfur-containing components in the sulfur production tail gas by oxygen-containing gas into sulfur oxides; the first-stage process gas from the converter enters a reactor, and is subjected to a second reaction with a desulfurizer in the reactor to respectively obtain a second-stage process gas and the desulfurizer to be generated; wherein the second reaction satisfies: the sulfur oxides in the primary process gas are absorbed by the desulfurizer and converted into sulfate; washing and electrically dedusting the secondary process gas from the reactor to obtain purified tail gas; after the to-be-generated desulfurizer is output from the reactor, at least part of the to-be-generated desulfurizer enters a regenerator for regeneration to obtain a regenerated desulfurizer; the regenerated desulfurizer returns to the reactor to participate in the second reaction. The invention has the advantages of short flow, low energy consumption, energy saving, environmental protection, low cost, small occupied area of the used device and the like.
Description
Technical Field
The invention relates to sulfur production tail gas treatment, in particular to a sulfur production tail gas desulfurization method and a sulfur production tail gas desulfurization device.
Background
At present, the common treatment process for the sulfur production tail gas generated by the sulfur recovery device mainly comprises a reduction absorption process mainly based on the SCOT process and an upgrading process thereof, such as an SSR process developed based on the SCOT process, a ZHSR process, and the like, and the processes generally include heating the sulfur production tail gas to raise the temperature of SO therein2、CS2COS and SxContaining sulfur component and H2Reacting with reducing agent to generate H2S, removing H in tail gas through heat exchange, quenching, amine liquid absorption, analysis and other processes2S and H2S is desorbed from the absorbent and then returns to the sulfur production unit, the purified tail gas is discharged after incineration and waste heat recovery, and in order to meet the requirements of the emission standard of pollutants for petroleum refining industry (GB31570-2015), purification measures such as alkaline washing (such as sodium desulfurization) and the like are generally required to be added after amine liquid absorption or an incinerator. The existing sulfur production tail gas treatment process has the defects of long flow, high energy consumption, heavy pollution, large investment, large occupied area of used devices and the like, and is a technical problem to be solved urgently by technical personnel in the field.
Disclosure of Invention
The invention provides a desulfurization method and a desulfurization device for sulfur production tail gas, which at least solve the problems of long process flow, high energy consumption, heavy pollution, large investment, large occupied area of used devices and the like in the prior art.
In one aspect of the present invention, a method for desulfurizing a sulfur production tail gas is provided, which comprises: carrying out a first reaction on the sulfur production tail gas and oxygen-containing gas in a converter to obtain a first-stage process gas; wherein the first reaction satisfies: oxidizing sulfur-containing components in the sulfur production tail gas to sulfur oxides by the oxygen-containing gas; the primary process gas from the converter enters a reactor, and undergoes a second reaction with a desulfurizer in the reactor to respectively obtain a secondary process gas and a desulfurizer to be generated; wherein the second reaction satisfies: adsorbing the sulfur oxides in the primary process gas by a desulfurizing agent and converting the sulfur oxides into sulfates; washing and electrically dedusting the secondary process gas from the reactor to obtain purified tail gas; after the to-be-generated desulfurizer is output from the reactor, at least part of the to-be-generated desulfurizer enters a regenerator for regeneration to obtain a regenerated desulfurizer; and the regenerated desulfurizer returns to the reactor to participate in the second reaction.
According to one embodiment of the invention, the secondary process gas from the reactor passes through a steam superheater, a waste heat boiler, a first heat exchanger and a preheater in sequence and then is subjected to the washing and electric dust removal treatment; the oxygen-containing gas exchanges heat with the secondary process gas flowing through the preheater to obtain preheated oxygen-containing gas; the preheated oxygen-containing gas is mixed with the sulfur production tail gas to obtain mixed gas; the mixed gas exchanges heat with a secondary process gas flowing through the first heat exchanger, and then enters the converter to generate the first reaction; the deaerated water enters a waste heat boiler to exchange heat with secondary process gas flowing through the waste heat boiler to generate medium-pressure steam; the medium-pressure steam enters the steam superheater to exchange heat with secondary process gas flowing through the steam superheater.
According to an embodiment of the present invention, the temperature of the preheated oxygen-containing gas is 130 to 170 ℃; and/or the temperature of the mixed gas after heat exchange with the secondary process gas flowing through the first heat exchanger is 250-400 ℃; and/or the medium-pressure steam is 3.6 MPa-4.4 MPa steam.
According to one embodiment of the invention, the primary process gas is output from the outlet of the converter and then enters the heater, and after the temperature of the primary process gas in the heater is raised to 600-750 ℃, the primary process gas enters the reactor and reacts with a desulfurizer for the second time; wherein the outlet temperature of the converter is 400-600 ℃.
According to an embodiment of the present invention, the washing and electric precipitation treatment includes: the second-stage process gas enters an evaporator to exchange heat with the filtered waste liquid and then enters a quenching washing tower to contact with washing liquid to carry out quenching washing, so as to respectively obtain third-stage process gas and non-gas-phase materials; feeding the three-stage process gas from the quenching washing tower into an electric precipitation section for electric precipitation treatment to obtain the purified tail gas; the non-gas phase material enters a filter for solid-liquid separation to respectively obtain waste residue and filtered waste liquid; part of the filtered waste liquid is cooled by a cooler and then returns to a quenching washing tower to be used as the washing liquid; and part of the filtered waste liquid enters the evaporator to exchange heat with the secondary process gas entering the evaporator, in the heat exchange process, the secondary process gas is cooled, meanwhile, the filtered waste liquid is evaporated and concentrated to respectively obtain concentrated liquid and steam generated by the evaporation and concentration, and the steam returns to the quenching washing tower.
According to one embodiment of the present invention, the pH of the washing solution is 6.5 to 6.8, and the temperature of the top of the quenching washing tower is 55 to 75 ℃.
According to an embodiment of the invention, the regeneration process comprises: the to-be-regenerated desulfurizer entering the regenerator is subjected to a regeneration reaction with a reducing agent to obtain the regenerated desulfurizer; wherein the regeneration reaction satisfies: reducing the sulfur element in the sulfate to hydrogen sulfide by the reducing agent.
According to an embodiment of the invention, the oxygen containing gas comprises air; and/or, the reducing agent comprises hydrogen and/or methane; and/or the temperature of the regeneration reaction is 500-650 ℃.
According to an embodiment of the invention, after the regeneration reaction, the regenerated desulfurizer and the regeneration gas containing the hydrogen sulfide are obtained, and the regeneration gas from the regenerator enters a filter for filtration after passing through a second heat exchanger, so as to obtain the filtered regeneration gas; and the reducing agent enters the second heat exchanger, exchanges heat with the regenerated gas flowing through the second heat exchanger, enters the regenerator, and performs the regeneration reaction with the to-be-regenerated desulfurizer entering the regenerator.
In another aspect of the present invention, there is provided a desulfurization apparatus comprising:
the converter is provided with a feeding inlet and a primary process gas outlet;
the heater is provided with a process gas outlet and a process gas inlet communicated with the primary process gas outlet of the converter;
the reactor is provided with a spent agent circulating inlet, a secondary process gas outlet, a spent agent outlet and a primary process gas inlet communicated with the process gas outlet of the heater;
the regenerator is provided with a reducing agent inlet, a regeneration gas outlet, a spent agent inlet communicated with a spent agent outlet of the reactor, and a regeneration agent outlet communicated with a spent agent circulating inlet of the reactor;
the second heat exchanger is provided with a regeneration gas channel and a reducing agent channel, and the reducing agent channel is communicated with a reducing agent inlet of the regenerator;
the regeneration gas outlet of the regenerator, the regeneration gas channel of the second heat exchanger and the filter are communicated in sequence;
the steam superheater is provided with a first process gas channel and a steam channel;
the waste heat boiler is provided with a second process gas channel and a steam/water channel, and the steam channel of the steam superheater is communicated with the steam/water channel of the waste heat boiler;
the first heat exchanger is provided with a third process gas channel and a feeding channel;
the preheater is provided with a fourth process gas channel and an oxygen-containing gas channel;
the evaporator is provided with a fifth process gas channel and a filtered waste liquid channel, and the filtered waste liquid channel is provided with a filtered waste liquid inlet and a steam outlet;
the oxygen-containing gas channel of the preheater, the feeding channel of the first heat exchanger and the feeding inlet of the converter are communicated in sequence;
a secondary process gas outlet of the reactor, a first process gas channel of the steam superheater, a second process gas channel of the waste heat boiler, a third process gas channel of the first heat exchanger, a fourth process gas channel of the preheater and a fifth process gas channel of the evaporator are communicated in sequence;
the quenching washing tower is provided with a washing liquid inlet, a third-stage process gas outlet, a non-gas-phase material outlet, a steam inlet communicated with the steam outlet of the evaporator and a second-stage process gas inlet communicated with the fifth process gas channel;
the filter is provided with a filtered waste liquid outlet and a feed liquid inlet communicated with the non-gas-phase material outlet of the quenching washing tower, and the filtered waste liquid outlet is communicated with the filtered waste liquid inlet of the filtered waste liquid channel of the evaporator;
a cooler provided with a filtered waste liquid inlet communicated with the filtered waste liquid outlet of the filter and a washing liquid outlet communicated with the washing liquid inlet of the quenching washing tower;
and the electric dust removal section is communicated with a three-stage process gas outlet of the quenching washing tower.
The invention provides a novel sulfur-making tail gas treatment process (FECOT process for short), which comprises the step of reacting sulfur-making tail gas with oxygen-containing gas (namely, a first reaction) to ensure that H in the sulfur-making tail gas is subjected to reaction2S、CS2Sulfides (sulfur-containing components) such as COS are oxidized to sulfur oxides (mainly SO)2And SO3) And then the tail gas carrying sulfur oxide is contacted with a desulfurizer to carry out adsorption desulfurization reaction (namely, the second reaction), so that the sulfur oxide is converted into sulfate, and the purified tail gas is discharged up to the standard by matching with subsequent washing and electric dust removal treatment, wherein the desulfurizer to be generated is returned to participate in the adsorption desulfurization reaction after at least part of the desulfurizer to be generated is regenerated. Compared with the conventional sulfur production tail gas (or called sulfur tail gas) treatment process such as SCOT and the like, the invention adopts the oxidation adsorption desulfurization process, has short process flow, simple operation, capability of greatly reducing energy consumption, no discharge of acidic water and alkaline residue, low cost, small investment, energy saving, environmental protection and the like, and simultaneously the desulfurization device has simple structure and occupies less spaceThe land area is small, and the method has important significance for practical industrial application.
Drawings
Fig. 1 is a schematic configuration diagram of a desulfurization apparatus according to an embodiment of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The desulfurization method of the sulfur production tail gas provided by the invention comprises the following steps: carrying out a first reaction on the sulfur-making tail gas and an oxygen-containing gas in a converter to obtain a primary process gas; wherein the first reaction satisfies: oxidizing the sulfur-containing components in the sulfur production tail gas by oxygen-containing gas into sulfur oxides; the first-stage process gas from the converter enters a reactor, and a second reaction is carried out on the first-stage process gas and a desulfurizer to be generated in the reactor to respectively obtain a second-stage process gas and the desulfurizer to be generated; wherein the second reaction satisfies: the sulfur oxides in the primary process gas are absorbed by the desulfurizer and converted into sulfate; washing and electrically dedusting the secondary process gas from the reactor to obtain purified tail gas; after the to-be-generated desulfurizer is output from the reactor, at least part of the to-be-generated desulfurizer enters a regenerator for regeneration to obtain a regenerated desulfurizer; the regenerated desulfurizer returns to the reactor to participate in the second reaction, and a cycle is formed.
In the invention, the sulfur production tail gas is derived from tail gas of a sulfur production device/a sulfur recovery device, and the sulfur-containing component mainly comprises H2S、CS2、COS、SxAnd SO2After the first reaction, the sulfur-containing components are generally oxidized to SO by the oxygen in the oxygen-containing gas2Most of the SO2Is oxidized into SO3The main reaction formula is as follows:
H2S+O2→SO2+H2O
CS2+O2→SO2+CO2
COS+O2→SO2+CO2
Sx+O2→SO2
SO2+O2→SO3。
in the specific implementation, an oxidation catalyst is generally introduced, so that the sulfur production tail gas is reacted with O in oxygen-containing gas under the action of the oxidation catalyst2Reaction, converting the sulfide in the reaction product into SO as completely as possible3. Specifically, in some embodiments, the oxygen-containing gas may comprise air.
The primary process gas from the converter enters the reactor to contact with the desulfurizer to carry out a second reaction, SO that the sulfide is absorbed by the desulfurizer and converted into sulfate, wherein SO possibly existing in the primary process gas2Will continue to react with the oxygen-containing gas to form SO3，SO3Reacts with a desulfurizing agent to generate sulfate. Specifically, the desulfurizing agent can comprise an alkaline oxide and can also comprise a trace amount of non-alkaline oxide generally so as to improve the reduced performance of the desulfurizing agent to be generated and ensure that the desulfurizing agent is easier to regenerate; among them, the basic oxide includes, for example, an oxide of an alkaline earth metal, and preferably includes active magnesium oxide. The desulfurizing agent is particularly useful for removing SO present in a process gas at an elevated temperature (e.g., the second reaction temperature described below)2Oxidation to SO3And rapid absorption of SO3And stable sulfate is generated, and the sulfate can react with a reducing agent to realize rapid decomposition and reduction (particularly, the sulfate can be rapidly decomposed and reduced under the condition of high temperature (such as regeneration reaction temperature) to realize regeneration.
Specifically, the main reaction formula of the above-described second reaction is as follows:
SO2+O2→SO3
XO+SO3→XSO4(XO represents a basic oxide, wherein X represents a metal).
And the secondary process gas from the reactor sequentially passes through a steam superheater, a waste heat boiler, a first heat exchanger and a preheater and then is subjected to washing and electric dust removal treatment.
Wherein, the oxygen-containing gas is subjected to heat exchange with a secondary process gas flowing through the preheater to obtain a preheated oxygen-containing gas; mixing the preheated oxygen-containing gas with the sulfur production tail gas to obtain a mixed gas; the mixed gas exchanges heat with the secondary process gas flowing through the first heat exchanger and then enters the converter to generate a first reaction; the deaerated water enters a waste heat boiler to exchange heat with secondary process gas flowing through the waste heat boiler to generate medium-pressure steam; the medium pressure steam from the waste heat boiler enters the steam superheater to exchange heat with the secondary process gas flowing through the steam superheater, the medium pressure steam is superheated through the heat of the secondary process gas, and the superheated medium pressure steam is discharged from the steam superheater. The heat is recovered through the process, which is beneficial to further saving energy.
The method comprises the following steps that secondary process gas is cooled step by step in the process of sequentially flowing through a steam superheater (called a superheater for short), a waste heat boiler, a first heat exchanger and a preheater, and specifically, the waste heat boiler generates medium-pressure steam, namely water in the waste heat boiler is vaporized to generate the medium-pressure steam through the heat of the secondary process gas, and meanwhile, the secondary process gas is cooled; a steam superheater (a superheater for short) superheats medium-pressure steam to meet the requirement of a pipe network and further cools secondary process gas; in first heat exchanger, second grade process gas and gas mixture heat transfer to preheat the gas mixture, make second grade process gas further cool down simultaneously, in the pre-heater, second grade process gas and oxygen-containing gas carry out the heat transfer, thereby preheat oxygen-containing gas, obtain above-mentioned oxygen-containing gas that preheats, make second grade process gas further cooling down simultaneously. Wherein the temperature of the preheated oxygen-containing gas is 130-170 ℃, for example 155 ℃, the temperature of the mixed gas after heat exchange with the secondary process gas flowing through the first heat exchanger is 250-400 ℃, and then the mixed gas enters the converter to perform a first reaction (namely, the mixed gas enters the converter after heat exchange with the secondary process gas in the first heat exchanger is carried out to 250-400 ℃), namely, the temperature of the first reaction is 250-400 ℃; the medium-pressure steam may be steam of 3.6MPa to 4.4 MPa.
In some embodiments, the primary process gas is output from the outlet of the converter (the primary process gas outlet), enters the heater, is heated to 600-750 ℃ in the heater, and then enters the reactor to perform a second reaction with the desulfurizing agent, i.e., the temperature of the second reaction is 600-750 ℃; wherein, the outlet temperature of the converter can be 400-600 ℃. The first-stage process gas can be heated and heated on line through the heater, and the efficiency of the second reaction is improved. The heater can be a conventional heating furnace, an electric heater and other heating equipment, and can be selected according to the treatment capacity of the sulfur production tail gas in specific implementation.
In specific implementation, the feeding amount and the circulating amount of the desulfurizer in the reactor can be controlled to ensure that the sulfur content in the secondary process gas is less than or equal to 200mg/Nm3(wet basis), particulate matter content not more than 200mg/Nm3(wet basis).
In some embodiments, the washing and electric precipitation treatment comprises: the second-stage process gas enters an evaporator to exchange heat with the filtered waste liquid and then enters a quenching washing tower to contact with washing liquid to carry out quenching washing, so as to respectively obtain third-stage process gas and non-gas-phase materials; outputting the three-stage process gas from the quenching washing tower and then entering an electric dust removal section for electric dust removal treatment to obtain purified tail gas; the non-gas phase material enters a filter for solid-liquid separation to respectively obtain waste residue (solid residue) and filtered waste liquid; the filtered waste liquid is divided into two paths, and part of the filtered waste liquid (generally a small amount of filtered waste liquid) is cooled by a cooler and then returns to a quenching washing tower to be used as washing liquid (circulating liquid); part of the filtered waste liquid enters the evaporator to exchange heat with the secondary process gas entering the evaporator, in the heat exchange process, the secondary process gas is cooled, meanwhile, the part of the filtered waste liquid is evaporated and concentrated to respectively obtain concentrated solution (concentrated solution) and steam generated by the evaporation and concentration, and the steam returns to the quenching washing tower to participate in quenching washing. Wherein, the solid slag can be recycled.
Specifically, the filtered waste liquid and the washing liquid can include water, the secondary process gas is subjected to quenching washing, the secondary process gas can be cooled and purified, impurities such as sulfate carried in the secondary process gas are removed, after the secondary process gas is subjected to quenching washing, a generated filtered waste liquid part enters the evaporator, heating, evaporating and concentrating are carried out through heat provided by the secondary process gas flowing through the evaporator, the concentrated liquid and steam (water vapor) are respectively obtained, the concentrated liquid (containing the impurities such as sulfate) is discharged from the evaporator, the impurities such as sulfate in the washing liquid (circulating liquid) in the circulating washing process are discharged intermittently, and the washing efficiency of the secondary process gas is improved. The main reaction scheme in the cyclic washing process is as follows:
SO2+H2O→H2SO3
H2SO3+O2→H2SO4
XO+H2SO3→XSO3+H2O
XO+H2SO4→XSO4+H2O。
in specific implementation, the tail gas can be purified more efficiently by controlling the circulating amount of the washing liquid in the quenching washing tower, the pH value of the washing liquid, the tower top temperature of the quenching washing tower and other conditions, in some preferred embodiments, the pH value of the washing liquid in the quenching washing tower is 6.5-6.8, and the tower top temperature of the quenching washing tower is 55-75 ℃.
Generally, the sulfur content in the three-stage process gas is less than or equal to 50mg/Nm3Dry basis, particulate matter content less than or equal to 50mg/Nm3(wet basis), after the three-stage process gas is subjected to electric precipitation treatment, the obtained purified tail gas has the sulfur content of less than or equal to 50mg/Nm3(dry basis) particulate matter content of 10mg/Nm or less3(dry basis), the purge tail gas can be evacuated. Wherein the electric dust removal treatment is specifically electrostatic dust removal.
In some embodiments, the regeneration process comprises: the to-be-regenerated desulfurizer entering the regenerator is subjected to a regeneration reaction with a reducing agent to obtain a regenerated desulfurizer; wherein the regeneration reaction satisfies: the sulfur element in the sulfate is reduced to hydrogen sulfide by a reducing agent. Optionally, the reducing agent can comprise hydrogen and/or methane, the regeneration reaction temperature is 500-650 ℃, the regeneration efficiency is favorably improved, and the resolution ratio of the desulfurizing agent is generally up to more than 95%. In some embodiments, the reducing agent is hydrogen and the primary reaction scheme for the regeneration reaction is as follows: XSO4+H2→XO+H2S+H2O(XSO4Representing sulfate). In specific implementation, the spent desulfurizer enters the regenerator from a spent agent inlet of the regenerator, and the spent desulfurizer is regenerated and removedThe sulfur agent enters the reactor from a regenerant outlet of the regenerator, and the temperature of the regeneration reaction can be controlled as follows: the temperature of the to-be-regenerated agent inlet of the regenerator and the temperature of the regenerated agent outlet are both 500-650 ℃.
Further, after the regeneration reaction, a regenerated desulfurizer and regenerated gas containing hydrogen sulfide are obtained, and the regenerated gas from the regenerator enters a filter for filtering after passing through a second heat exchanger so as to filter out solid particles in the regenerated gas and obtain filtered regenerated gas; the reducing agent enters the second heat exchanger, exchanges heat with the regenerated gas flowing through the second heat exchanger and then enters the regenerator, and carries out regeneration reaction with the desulfurizing agent to be generated entering the regenerator. In addition, as shown in fig. 1, the regenerator may be further provided with a stripping gas inlet for introducing a stripping gas, which may be steam in particular, into the regenerator to strip out hydrogen sulfide adsorbed on the solid particles.
The filtered regenerated gas can be sent to a sulfur production unit to participate in sulfur production, so that sulfur recovery is realized, and during specific implementation, the content of particulate matters in the filtered regenerated gas can meet the standard requirement of a sulfur product by controlling the filtering precision of a filter. Generally, the content of particulate matter in the regeneration gas from the regenerator is less than or equal to 200mg/Nm3After heat exchange by the second heat exchanger and filtration by the filter, the content of particulate matters in the regenerated gas is less than or equal to 100mg/Nm3。
In specific implementation, fresh desulfurizer can be supplemented into the reactor through a fresh agent tank containing desulfurizer as required, as shown in fig. 1, in some embodiments, the regenerator comprises a regeneration section for performing a regeneration reaction and a conveying section for conveying the regenerated desulfurizer to the reactor, and the desulfurizer from the fresh agent tank can firstly enter the conveying section of the regenerator and enter the reactor together with the regenerated desulfurizer.
As shown in fig. 1, the desulfurization apparatus of the present invention comprises:
the converter is provided with a feeding inlet and a primary process gas outlet;
the heater is provided with a process gas outlet and a process gas inlet communicated with the primary process gas outlet of the converter;
the reactor is provided with a spent agent circulating inlet, a secondary process gas outlet, a spent agent outlet and a primary process gas inlet communicated with the process gas outlet of the heater;
the regenerator is provided with a reducing agent inlet, a regeneration gas outlet, a first spent agent inlet communicated with a spent agent outlet of the reactor, and a regeneration agent outlet communicated with a spent agent circulating inlet of the reactor;
the second heat exchanger is provided with a regeneration gas channel and a reducing agent channel, and the reducing agent channel is communicated with a reducing agent inlet of the regenerator;
the regeneration gas outlet of the regenerator, the regeneration gas channel of the second heat exchanger and the filter are communicated in sequence;
the steam superheater is provided with a first process gas channel and a steam channel;
the waste heat boiler is provided with a second process gas channel and a steam/water channel, and the steam channel is communicated with the steam/water channel of the steam superheater;
the first heat exchanger is provided with a third process gas channel and a feeding channel;
the preheater is provided with a fourth process gas channel and an oxygen-containing gas channel;
the evaporator is provided with a fifth process gas channel and a filtered waste liquid channel, and the filtered waste liquid channel is provided with a filtered waste liquid inlet and a steam outlet;
an oxygen-containing gas channel of the preheater, a feeding channel of the first heat exchanger and a feeding inlet of the converter are communicated in sequence; a second-stage process gas outlet of the reactor, the steam superheater, the waste heat boiler, a third process gas channel of the first heat exchanger, a fourth process gas channel of the preheater and a fifth process gas channel of the evaporator are communicated in sequence;
the quenching washing tower is provided with a washing liquid inlet, a third-stage process gas outlet, a non-gas-phase material outlet, a steam inlet communicated with the steam outlet of the evaporator and a second-stage process gas inlet communicated with the fifth process gas channel;
the filter is provided with a filtered waste liquid outlet and a feed liquid inlet communicated with the non-gas-phase material outlet of the quenching washing tower, and the filtered waste liquid outlet is communicated with a filtered waste liquid inlet of a filtered waste liquid channel of the evaporator;
a cooler provided with a filtered waste liquid inlet communicated with the filtered waste liquid outlet of the filter and a washing liquid outlet communicated with the washing liquid inlet of the quenching washing tower;
and the electric dust removal section is communicated with a three-stage process gas outlet of the quenching washing tower.
Wherein the regenerator may also be provided with a stripping gas inlet. In addition, the desulfurizing device also comprises a fresh agent tank which is communicated with a spent agent circulating inlet of the reactor and is used for containing and conveying fresh desulfurizing agent into the reactor; the reactor is also provided with a second spent agent inlet which is communicated with a spent agent outlet of the reactor. In some embodiments, the regenerator comprises a regeneration section for performing the regeneration reaction and a conveying section for conveying the regenerated desulfurizer to the reactor, the regenerant outlet of the regenerator is arranged on the conveying section, and the fresh agent tank is communicated with the conveying section, that is, the fresh agent tank is communicated with the spent agent circulation inlet of the reactor through the conveying section of the regenerator.
Example 1 (two stage Claus + FECOT)
The desulfurization device shown in fig. 1 is adopted to desulfurize the sulfur production tail gas generated by the sulfur recovery device (the capacity of the sulfur recovery device is 10 ten thousand tons/year), and the desulfurization process is as follows:
the oxygen-containing gas enters an oxygen-containing gas channel of the preheater to exchange heat with the secondary process gas flowing through a fourth process gas channel of the preheater, so that the secondary process gas is cooled, and meanwhile, the oxygen-containing gas is preheated by the heat of the secondary process gas to obtain the preheated oxygen-containing gas; mixing the preheated oxygen-containing gas with the sulfur production tail gas to obtain a mixed gas;
the mixed gas enters a feeding channel of the first heat exchanger, exchanges heat with the secondary process gas flowing through a third process gas channel of the first heat exchanger to cool the secondary process gas, and heats the mixed gas by the heat of the secondary process gas; then, the heated mixed gas enters the converter from a feed inlet of the converter, and a first reaction is carried out in the converter to obtain a first-stage process gas;
the first-stage process gas is output from a first-stage process gas outlet of the converter, enters the heater from a process gas inlet of the heater for heating and temperature rise, is output from a process gas outlet of the heater, enters the reactor from a first-stage process gas inlet of the reactor, and undergoes a second reaction with the desulfurizer entering the reactor in the reactor to respectively obtain a second-stage process gas and the desulfurizer to be generated;
the secondary process gas is output from a secondary process gas outlet of the reactor and sequentially flows through a first process gas channel of the steam superheater, a second process gas channel of the waste heat boiler, a third process gas channel of the first heat exchanger, a fourth process gas channel of the preheater and a fifth process gas channel of the evaporator; the deaerated water enters a steam/water channel of the waste heat boiler and exchanges heat with secondary process gas flowing through a second process gas channel of the waste heat boiler, and in the heat exchange process, the water is vaporized to generate medium-pressure steam and the secondary process gas is cooled; the medium-pressure steam enters a first process gas channel of the steam superheater and exchanges heat with secondary process gas flowing through the steam superheater, and in the heat exchange process, the medium-pressure steam is superheated, and meanwhile, secondary tail gas is cooled;
in the evaporator, the secondary process gas exchanges heat with the filtered waste liquid flowing through a filtered waste liquid channel of the evaporator so as to cool the secondary process gas, and the filtered waste liquid is evaporated and concentrated by the heat of the secondary process gas;
in the evaporator, after the heat exchange between the secondary process gas and the filtered waste liquid, the filtered waste liquid respectively generates concentrated liquid and steam, the concentrated liquid is discharged out of the desulfurization device, the steam is output from a steam outlet of a filtered waste liquid channel and enters the quenching washing tower from a steam inlet of the quenching washing tower to participate in the quenching washing of the secondary process gas entering the quenching washing tower;
in the evaporator, after the heat exchange between the secondary process gas and the filtered waste liquid, the secondary process gas is output from a fifth process gas channel of the evaporator, enters the quenching washing tower from a secondary process gas inlet of the quenching washing tower, and is in contact with washing liquid in the quenching washing tower to carry out quenching washing to respectively obtain a tertiary process gas and a non-gas phase material;
outputting the three-stage process gas from a three-stage process gas outlet of the quenching washing tower, and then entering an electric dust removal section for electric dust removal treatment to obtain purified tail gas, wherein the purified tail gas is discharged out of a desulfurization device and enters the atmosphere (namely is emptied);
discharging non-gas-phase materials from a non-gas-phase material outlet of the quenching washing tower, enabling the non-gas-phase materials to enter a filter from a feed liquid inlet of the filter, performing solid-liquid separation in the filter to respectively obtain solid residues and filtered waste liquid, and discharging the solid residues from the filter; after the filtered waste liquid is discharged from a filtered waste liquid outlet of the filter, part of the filtered waste liquid enters the cooler from a filtered waste liquid inlet of the cooler to be cooled to obtain a washing liquid, the washing liquid is output from a washing liquid outlet of the cooler and then enters the quenching washing tower from a washing liquid inlet of the quenching washing tower, and the quenching washing is carried out on the secondary process gas entering the quenching washing tower; part of the filtered waste liquid enters the filtered waste liquid channel of the evaporator from the filtered waste liquid inlet of the filtered waste liquid channel of the evaporator and exchanges heat with the secondary process gas flowing through the fifth process gas channel of the evaporator;
after the to-be-generated desulfurizer is output from a to-be-generated agent outlet of the reactor, returning a part of the to-be-generated desulfurizer from a second to-be-generated agent inlet of the reactor to continuously participate in a second reaction, and allowing the rest of the to-be-generated desulfurizer to enter a regenerator from a first to-be-generated agent inlet of the regenerator and contact with a reducing agent entering the regenerator in the regenerator for regeneration to respectively obtain a regenerated desulfurizer and regenerated gas;
the regenerated desulfurizer is output from the regenerator outlet of the regenerator and returns to the reactor from the spent agent circulation inlet of the reactor to participate in the second reaction; wherein, the insufficient part of the desulfurizer is supplemented from the new agent tank, and the desulfurizer from the new agent tank firstly enters the conveying section of the regenerator and enters the reactor together with the regenerated desulfurizer. Steam enters the regenerator through a stripping gas inlet of the regenerator to strip out the regeneration gas adsorbed on the solid particles such as the desulfurizing agent; the regenerated gas is output from a regenerated gas outlet of the regenerator, flows through a regenerated gas channel of the second heat exchanger, exchanges heat with the reducing agent flowing through a reducing agent channel of the second heat exchanger to cool the regenerated gas, heats the reducing agent by the heat of the regenerated gas, and the heated reducing agent enters the regenerator from a reducing agent inlet of the regenerator; filtering the regenerated gas after heat exchange and cooling in the second heat exchanger through a filter, and then removing a sulfur production unit to participate in sulfur production;
wherein the used oxygen-containing gas is air, the temperature of the preheated oxygen-containing gas is 155 ℃, the temperature of the mixed gas formed by mixing the preheated oxygen-containing gas and the sulfur production tail gas after heat exchange by a first heat exchanger is 350 ℃, the temperature of the outlet of the converter is 511 ℃, the first-stage process gas is heated in a heater to 725 ℃ and then enters the reactor to perform a second reaction with a desulfurizer, and the desulfurizer comprises active magnesium oxide; controlling the pH value of a washing liquid in the quenching washing tower to be 6.5-6.8, and controlling the tower top temperature of the quenching washing tower to be 67 ℃; the reducing agent in the regeneration process is methane (saturated dry gas), the inlet temperature of the spent regenerant of the regenerator is 610 ℃, and the outlet temperature of the regenerant of the regenerator is 589 ℃; the main parameters of reagent dosage, energy consumption and the like are shown in a table 1, and the parameters of sulfur dioxide emission, particulate matter emission, solid residue emission, emission of concentrated solution containing sulfate, consumption of each reagent, cost calculated by reference price, income and the like after desulfurization are shown in a table 2.
Comparative example 1
The sulfur production tail gas with the same properties as those of the sulfur production tail gas in the embodiment 1 is desulfurized by adopting the existing two-stage Claus + non-online furnace SCOT + sodium method, the main parameters of energy consumption and the like are shown in a table 1, and the parameters of sulfur dioxide emission, particulate matter emission, reagent consumption, engineering cost calculated by reference price, income and the like after desulfurization are shown in a table 2.
TABLE 1
TABLE 2
Reference price (unit price): 1000 yuan/ton of sulfur, 2300 yuan/ton of sodium hydroxide (solid caustic soda), 1.25 ten thousand/ton of hydrogen, 1500 yuan/ton of fuel gas and standard oil used for heating, 3 ten thousand/ton of MDEA (methyldiethanolamine) used in the process of absorbing amine liquid, and 15 ten thousand/ton of desulfurizer;
"Kgeo/t sulfur" means the energy consumption for the desulfurization treatment of tail gas produced in the production of 1 ton (t) of sulfur; "Yuan/t sulfur" means the yield of desulfurization treatment for tail gas produced by producing 1 ton (t) of sulfur.
In embodiment 1, firstly, sulfide in the sulfur production tail gas (or called sulfur tail gas) is oxidized into sulfur oxide through a medium-temperature oxidation process, and then a high-temperature adsorption process of a desulfurizer and a regeneration process of a desulfurizer to be generated are combined to be matched with a subsequent electric precipitation process, so that the sulfur production tail gas can be efficiently purified, and compared with the existing sulfur tail gas treatment scheme, the sulfur production tail gas treatment method at least has the following advantages:
(1) low energy consumption
According to statistics, the average energy consumption of the existing sulfur recovery device (such as an SCOT process, an SSR process, a ZHSR process and the like) is about-106.1 kgeo/1t of sulfur, and the energy consumption of the embodiment 1 is-252 kgeo/1t of sulfur, which is far lower than the existing average energy consumption level (reduced by 138 percent relative to the existing average energy consumption level); meanwhile, as can be seen from tables 1 and 2, compared with the classical desulfurization process (comparative example 1) combining two-stage Claus + SCOT + sodium desulfurization, the energy consumption of example 1 is also significantly reduced (by 66%), thereby further illustrating that the scheme of the present invention greatly reduces the energy consumption while efficiently purifying the sulfur-making tail gas;
(2) no acidic water discharge
Example 1 desulfurization by oxidative adsorption avoids the prior art hydrogenation reduction (reduction of sulfur content in the sulfur production tail gas to H)2S) carrying out quenching absorption to generate a desulfurization process of acidic water, so that the generation of the acidic water is avoided, the environment is protected, and the acidic corrosion to equipment is reduced;
(3) fresh water does not need to be supplemented basically in the washing process, and alkali residue is not discharged
In the embodiment 1, the secondary process gas is circularly washed by arranging an evaporator, a quenching washing tower and the like, and the water content in the secondary process gas can reach gas-liquid phase balance by adjusting the conditions of quenching washing temperature and the like in the circulating washing process, and fresh water is basically not required to be supplemented; in addition, two stagesThe desulfurizer particles carried in the process gas are alkaline and can be dissolved with SO2The acid-base neutralization is realized by the washing liquid of the acidic gas, so that the tail gas is fully purified, the use of alkali liquor is avoided, and no alkali residue is discharged;
(4) low investment and good profit
Taking a sulfur recovery device with the capacity of 10 ten thousand tons/year as an example, referring to the conventional price of each reagent, the engineering cost of the embodiment 1 is obviously lower than that of the comparative example 1, and the yield of the embodiment 1 is better than that of the comparative example 1 by calculating the conventional output-consumption cost, thereby further explaining that the desulfurization process has important practical significance.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made without departing from the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A method for desulfurizing a sulfur production tail gas, comprising:
carrying out a first reaction on the sulfur production tail gas and oxygen-containing gas in a converter to obtain a first-stage process gas; wherein the first reaction satisfies: oxidizing sulfur-containing components in the sulfur production tail gas to sulfur oxides by the oxygen-containing gas;
the primary process gas from the converter enters a reactor, and undergoes a second reaction with a desulfurizer in the reactor to respectively obtain a secondary process gas and a desulfurizer to be generated; wherein the second reaction satisfies: allowing the sulfur oxides in the primary process gas to be adsorbed by a desulfurizing agent and converted into sulfates;
washing and electrically dedusting the secondary process gas from the reactor to obtain purified tail gas; wherein, washing and electric precipitation treatment include: the second-stage process gas enters an evaporator to exchange heat with the filtered waste liquid and then enters a quenching washing tower to contact with washing liquid for quenching washing to respectively obtain a third-stage process gas and a non-gas-phase material; feeding the three-stage process gas from the quenching washing tower into an electric precipitation section for electric precipitation treatment to obtain the purified tail gas; the non-gas phase material enters a filter for solid-liquid separation to respectively obtain waste residues and filtered waste liquid; part of the filtered waste liquid is cooled by a cooler and then returns to a quenching washing tower to be used as the washing liquid; part of the filtered waste liquid enters the evaporator to exchange heat with secondary process gas entering the evaporator, in the heat exchange process, the secondary process gas is cooled, meanwhile, the filtered waste liquid is evaporated and concentrated to respectively obtain concentrated solution and steam generated by the evaporation and concentration, and the steam returns to the quenching washing tower;
after the to-be-generated desulfurizer is output from the reactor, at least part of the to-be-generated desulfurizer enters a regenerator for regeneration to obtain a regenerated desulfurizer; and the regenerated desulfurizer returns to the reactor to participate in the second reaction.
2. The desulfurization method of claim 1, wherein the secondary process gas from the reactor is subjected to the washing and electric dust removal treatment after sequentially passing through a steam superheater, a waste heat boiler, a first heat exchanger and a preheater;
the oxygen-containing gas exchanges heat with a secondary process gas flowing through the preheater to obtain a preheated oxygen-containing gas; the preheated oxygen-containing gas is mixed with the sulfur production tail gas to obtain mixed gas;
the mixed gas exchanges heat with a secondary process gas flowing through the first heat exchanger, and then enters the converter to generate the first reaction;
the deaerated water enters a waste heat boiler to exchange heat with secondary process gas flowing through the waste heat boiler to generate medium-pressure steam; the medium-pressure steam enters the steam superheater to exchange heat with secondary process gas flowing through the steam superheater.
3. The desulfurization method according to claim 2,
the temperature of the preheated oxygen-containing gas is 130-170 ℃; and/or the presence of a gas in the gas,
the temperature of the mixed gas after heat exchange with a secondary process gas flowing through the first heat exchanger is 250-400 ℃; and/or the presence of a gas in the atmosphere,
the medium-pressure steam is 3.6 MPa-4.4 MPa steam.
4. The desulfurization method according to any one of claims 1 to 3,
the primary process gas is output from an outlet of the converter and then enters a heater, and after the temperature of the primary process gas in the heater is raised to 600-750 ℃, the primary process gas enters the reactor and reacts with a desulfurizer for the second time; wherein the outlet temperature of the converter is 400-600 ℃.
5. The desulfurization method according to claim 1, wherein the pH of the scrubbing solution is 6.5 to 6.8, and the temperature of the top of the quenching scrubber is 55 to 75 ℃.
6. The desulfurization method according to claim 1, wherein the regeneration process comprises: the to-be-regenerated desulfurizer entering the regenerator is subjected to a regeneration reaction with a reducing agent to obtain the regenerated desulfurizer; wherein the regeneration reaction satisfies: reducing the sulfur element in the sulfate to hydrogen sulfide by the reducing agent.
7. The desulfurization method according to claim 6, wherein the reducing agent comprises hydrogen and/or methane.
8. The desulfurization method according to claim 1 or 6,
the oxygen-containing gas comprises air; and/or the presence of a gas in the gas,
the temperature of the regeneration reaction is 500-650 ℃.
9. The desulfurization method according to claim 6,
after the regeneration reaction, the regenerated desulfurizer and the regeneration gas containing the hydrogen sulfide are obtained, and the regeneration gas from the regenerator enters a filter for filtering after passing through a second heat exchanger to obtain the filtered regeneration gas;
and the reducing agent enters the second heat exchanger, exchanges heat with the regenerated gas flowing through the second heat exchanger, enters the regenerator, and performs the regeneration reaction with the to-be-regenerated desulfurizer entering the regenerator.
10. A desulfurization apparatus, comprising:
the converter is provided with a feeding inlet and a primary process gas outlet;
the heater is provided with a process gas outlet and a process gas inlet communicated with the primary process gas outlet of the converter;
the reactor is provided with a spent agent circulating inlet, a secondary process gas outlet, a spent agent outlet and a primary process gas inlet communicated with the process gas outlet of the heater;
the regenerator is provided with a reducing agent inlet, a regeneration gas outlet, a spent agent inlet communicated with a spent agent outlet of the reactor, and a regeneration agent outlet communicated with a spent agent circulating inlet of the reactor;
the second heat exchanger is provided with a regeneration gas channel and a reducing agent channel, and the reducing agent channel is communicated with a reducing agent inlet of the regenerator;
the regeneration gas outlet of the regenerator, the regeneration gas channel of the second heat exchanger and the filter are communicated in sequence;
the steam superheater is provided with a first process gas channel and a steam channel;
the waste heat boiler is provided with a second process gas channel and a steam/water channel, and the steam channel of the steam superheater is communicated with the steam/water channel of the waste heat boiler;
the first heat exchanger is provided with a third process gas channel and a feeding channel;
the preheater is provided with a fourth process gas channel and an oxygen-containing gas channel;
the evaporator is provided with a fifth process gas channel and a filtered waste liquid channel, and the filtered waste liquid channel is provided with a filtered waste liquid inlet and a steam outlet;
the oxygen-containing gas channel of the preheater, the feeding channel of the first heat exchanger and the feeding inlet of the converter are communicated in sequence;
a secondary process gas outlet of the reactor, a first process gas channel of the steam superheater, a second process gas channel of the waste heat boiler, a third process gas channel of the first heat exchanger, a fourth process gas channel of the preheater and a fifth process gas channel of the evaporator are communicated in sequence;
the quenching washing tower is provided with a washing liquid inlet, a third-stage process gas outlet, a non-gas-phase material outlet, a steam inlet communicated with the steam outlet of the evaporator and a second-stage process gas inlet communicated with the fifth process gas channel;
the filter is provided with a filtered waste liquid outlet and a feed liquid inlet communicated with the non-gas-phase material outlet of the quenching washing tower, and the filtered waste liquid outlet is communicated with the filtered waste liquid inlet of the filtered waste liquid channel of the evaporator;
a cooler provided with a filtered waste liquid inlet communicated with the filtered waste liquid outlet of the filter and a washing liquid outlet communicated with the washing liquid inlet of the quenching washing tower;
and the electric dust removal section is communicated with a three-stage process gas outlet of the quenching washing tower.
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