CN110917847B - Reduce sulphur recovery unit SO2Discharge device and method - Google Patents

Reduce sulphur recovery unit SO2Discharge device and method Download PDF

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CN110917847B
CN110917847B CN201911019567.2A CN201911019567A CN110917847B CN 110917847 B CN110917847 B CN 110917847B CN 201911019567 A CN201911019567 A CN 201911019567A CN 110917847 B CN110917847 B CN 110917847B
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CN110917847A (en
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毛松柏
陈园园
周志斌
朱道平
杨绪甲
余勇
宋丽
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8603—Removing sulfur compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/308—Carbonoxysulfide COS

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Abstract

The invention provides a method for reducing SO discharged by a Claus sulfur recovery device aiming at a tail gas treatment technology of a hydrogenation reduction sulfur recovery device2A content device and a method belong to the atmospheric pollutant control technology in the environmental protection field. According to the tail gas hydrogenation reduction absorption process of the Claus sulfur device, the invention utilizes the characteristic that the hydrogenation tail gas has special temperature range and low temperature COS and CS when entering the quench tower2According to the requirement of the activation temperature of the hydrolysis catalyst, the hydrolysis catalyst with the height of 150-500mm is arranged at a certain tower plate number or filler height of a quenching tower, and COS and CS are hydrolyzed under the balance advantage of low-temperature hydrolysis2Reducing the sulfur content to below 5ppmv, thereby reducing the total sulfur in the purified hydrogenation tail gas and finally reducing the SO in the exhaust gas discharged by the sulfur recovery device2The concentration of (c). Meanwhile, the invention has no additional requirements on subsequent desulfurization and other equipment and operation, and is very suitable for reducing discharged SO by new and old devices2The concentration requirement.

Description

Reduce sulphur recovery unit SO2Discharge device and method
Technical Field
The invention provides a method for reducing SO discharged by a Claus sulfur recovery device aiming at a tail gas treatment technology of a hydrogenation reduction sulfur recovery device2A content device and a method belong to the atmospheric pollutant control technology in the environmental protection field.
Background
Producing a great deal of H in the industrial processes of petroleum refining and processing, sulfur-containing natural gas purification treatment, coal gasification to synthesis gas, metallurgy coking and the like at home and abroad2S and other sulfides in industrial mixed gas is mostly recovered in the form of sulfur by various sulfides in the mixed gas through a Claus sulfur recovery device, and then SO in discharged waste gas is treated through a tail gas treatment technology2The content is lower than the environmental protection index. In order to reach the sulfide emission standard specified in GB16297-1996, GB31570-2015 and the like, the domestic and overseas sulfur recovery device basically adopts a reduction absorption type tail gas treatment process, namely, sulfides in the tail gas are firstly hydrogenated and reduced and converted into H2S, then H is2S is separated and returned to a Claus sulfur recovery device for sulfur production. For the reduction absorption process, the removal degree of the sulfide in the mixed gas after hydrogenation reduction is improved by controlling SO in the finally discharged waste gas2The key process of (2). Especially in recent years, with the implementation of strict environmental regulations, the content of sulfide in the tail gas after tail gas desulfurization and purification becomes SO in the exhaust gas discharged by the sulfur recovery device2The key influencing factor of the content.
Because the actual reaction process of the Claus sulfur recovery process is quite complex, most of the sulfides in the reducing gas after hydrogenation are H2S, but still contains a small amount of COS and CS2. On one hand, the hydrogenation reduction is carried out at 280-330 ℃, and is limited to thermodynamic equilibrium hydrogenation tail gas or trace COS and CS exist2(ii) a On the other hand, the hydrocarbon contained in the raw material acid gas and the sulfur are produced through side reaction, especially when the hydrocarbon content in the raw material acid gas is high, the residual COS and CS in the hydrogenation tail gas2The content is higher. At present, the aqueous solution of dimethylethanolamine MDEA is widely used in industry to absorb and remove H in tail gas2S, etc., although MDEA is on H2S has very good removal performance, but for COS and CS2The removal ability is very weak; most MDEA formulated solvents. Therefore, COS and CS in the hydrogenation tail gas2The total sulfur of the purified tail gas is influenced, and the SO in the exhaust gas discharged by the sulfur recovery device is improved2The content of (a). If other materials are adopted, the COS and the CS can be improved2The MDEA formula solvent with strong removal capability can improve COS and CS compared with MDEA2But the degree of removal is generally 90% lower and higher CO is easily caused2The co-absorption rate, or both, is high and not readily available.
Disclosure of Invention
1. The technical problem to be solved is as follows:
tail gas COS and CS in tail gas hydrogenation reduction absorption treatment process of Claus sulfur recovery device2The common selective desulfurization solvent is difficult to remove and purify, the total sulfur reduction of the purified tail gas is influenced, and the discharged waste gas is restricted to be subjected to standard upgrading.
2. The technical scheme is as follows:
the invention combines the characteristics of the hydrogenation tail gas reduction absorption process of the Claus sulfur recovery unit and the future more strict environmental protection requirements, and provides a method for reducing COS and CS in the purified tail gas under the conditions of no replacement of a desulfurization solvent and no change of equipment and process parameters under the existing reduction absorption process2Thereby reducing SO in the discharged exhaust gas in a manner of reducing total sulfur2The method of (1).
The invention provides a method for reducing discharged SO of Claus sulfur recovery2The device of (2), including the quench tower, be equipped with multistage filler in the quench tower, the gas inlet of quench tower is located the side below of quench tower, the gas outlet of quench tower and the gas inlet of first separator are connected, the gas outlet of first separator and the gas inlet of absorption tower are connected, the gas outlet of absorption tower and the gas inlet of second separator are connected, are equipped with low temperature COS, CS2The hydrolysis catalyst is disposed at a certain packing height.
The catalyst for hydrolyzing the COS and the CS2 at the low temperature comprises aluminum oxide, the auxiliary agent is an alkaline substance, the catalyst is prepared by an impregnation method, the mass fraction of the aluminum oxide is 90-95, and the mass fraction of the alkaline substance is 5-10. The low temperature COS and CS2The space velocity of the hydrolysis catalyst is 500/h-2500/h.
The low temperature COS and CS2The hydrolysis catalyst is arranged above the second-stage packing counted from bottom to top in the quenching tower or is away from the quenching towerThe position of the packing with the bottom of 600 mm and the thickness of 1000mm ensures that the entering hydrogenation tail gas reaches the low-temperature COS and CS2When the hydrolysis catalyst is in the position, the temperature is 110-140 ℃.
The low temperature COS and CS2The height of the hydrolysis catalyst is 150-500 mm.
The temperature of the absorption liquid entering the absorption tower is less than or equal to 40 ℃, and the temperature of rich liquid absorbed by the absorption liquid at the bottom of the absorption tower is 115-125 ℃.
The invention also provides a method for reducing discharged SO recovered from Claus sulfur2The device reduces the discharged SO of Claus sulfur recovery2The method of (1).
3. Has the beneficial effects that:
the method reduces COS and CS in the purified tail gas under the condition of not replacing a desulfurization solvent and basically not changing equipment and process parameters under the existing hydrogenation reduction absorption process2Reducing SO in the discharged waste gas by reducing the total sulfur2。
Drawings
FIG. 1 is a process flow diagram of the present invention.
Wherein: 01-a quench tower, 02-an absorption tower, 03-a filler, 04-a low-temperature COS and CS2 hydrolysis catalyst, 05-a first separator, 06-a second separator, 07-hydrogenation tail gas, 10-lean solution and 11-rich solution.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
The invention provides a method for reducing discharged SO of Claus sulfur recovery2The device of (2), including quench tower 1, be equipped with multistage filler 3 in the quench tower 1, the gas inlet of quench tower 1 is located quench tower 1's side below, the gas outlet of quench tower 1 and the air inlet of first separator 5 are connected, the gas outlet of first separator 5 and the air inlet of absorption tower 2 are connected, the gas outlet of absorption tower 2 and the air inlet of second separator 6 are connected, are equipped with low temperature COS, CS2The hydrolysis catalyst 4 is arranged at a certain packing level.
COS and CS in hydrogenation tail gas2Low-temperature hydrolysis: according to claus sulphur device tail gas hydrogenation reduction absorption workerIn the process, after the tail gas 7 after hydrogenation is subjected to heat recovery by a waste heat boiler, the temperature of the tail gas 7 after hydrogenation is reduced to 140-170 ℃ from 280-330 ℃, and then the tail gas enters a quenching tower 1, is cooled to the atmospheric temperature-40 ℃ by water, and then enters an absorption tower 2.
The quenching tower 1 has a special temperature range and low temperature COS and CS when the hydrogenation tail gas 7 enters the quenching tower 12The hydrolysis catalyst 4 is arranged in an activation temperature interval, and low-temperature COS and CS are arranged at the position of a certain filler 3 of the quenching tower 12 Hydrolysis catalyst 4 by low temperature COS and CS2Hydrolyzing catalyst 4 COS and CS2Reducing the sulfur content to below 5ppmv, thereby reducing the total sulfur in the purified hydrogenation tail gas 7 and finally reducing the SO in the exhaust gas discharged by the sulfur recovery device2Can realize SO2In a concentration of less than 50mg/Nm3。
Specifically, the second filler 3 from bottom to top is changed into a second filler filled with low-temperature COS and CS with the height of 150-500mm2Hydrolyzing catalyst 4, or filling 150-500mm high low-temperature COS and CS at 600-1000mm filler position at the bottom of the clean cooling tower 12The hydrolysis catalyst ensures that the entering hydrogenation tail gas reaches the low-temperature COS and CS2When the hydrolysis catalyst is at the position of 4, the temperature is 110-140 ℃. The other devices are not changed and,
the catalyst 4 for low-temperature COS and CS2 hydrolysis comprises aluminum oxide, the auxiliary agent is an alkaline substance, the catalyst is prepared by an immersion method, the mass fraction of the aluminum oxide is 90-95, and the mass fraction of the alkaline substance is 5-10. 2, low temperature COS, CS2The space velocity of the hydrolysis catalyst 4 is 500/h-2500/h.
The existing alcohol amine absorption process can be applied to the absorption process or is appropriately changed, and the absorption solvent can be MDEA or other solvents with good selective desulfurization performance; the main absorption process parameters are characterized in that the temperature of absorption liquid entering the absorber 2 is less than or equal to 40 ℃, and the optimal temperature is 15-35 ℃; the temperature of the rich solution which is absorbed by the absorption liquid and is removed from the bottom of the absorption tower 2 is 115-125 ℃; one or more of a plate tower, a packed tower, a super-gravity rotating bed and a micro-cyclone absorber can be used in series-parallel connection on the absorber selection type.
The invention also provides a method for reducing discharged SO recovered from Claus sulfur2The device reduces gramDischarged SO from Laos sulfur recovery2The method comprises the following steps: the first step is as follows: hydrogenation tail gas 7 enters from the gas inlet of the quenching tower 1; the second step is that: the hydrogenation tail gas 7 is in countercurrent contact with quenching liquid sprayed from the top of the quenching tower 1 and passes through COS and CS2Low temperature hydrolysis catalyst 4 of COS and CS2Hydrolysis to H2S、CO2And then flows out from the gas outlet of the quenching tower 1; the third step: and in the second step, the gas from the gas outlet of the quenching tower 1 enters from the gas inlet of the absorption tower 2 after passing through the first separator 5, is in countercurrent contact with the barren solution 10 sprayed from the top of the absorption tower 2, and is then sent to the second separator 6 to separate entrained droplets and then is led out of the system.
In the second step, low-temperature COS and CS are performed2Hydrolyzing COS and CS in catalyst 4-back hydrogen tail gas2By hydrolysis to H2S、CO2The hydrolysis rate of (2) is more than 95%.
The temperature of the gas coming out of the gas outlet of the quenching tower 1 is 20-35 ℃.
Comparative example 1:
the quenching tower 1 is not filled with low-temperature COS and CS2 A hydrolysis catalyst 4. The pressure of the simulated hydrogenation tail gas 7 used in the test is 5kPa, the simulated hydrogenation tail gas enters the quenching tower 1 at the temperature of 140 ℃, wherein COS and CS2100mg/Nm in terms of sulfur3，H2S2.0% volume fraction. An aqueous solution with the mass fraction of 35% prepared from MDEA is used as an absorption liquid, the temperature of the absorption liquid entering an absorption tower is 30-35 ℃, and the temperature of a rich solution is 115-120 ℃. The results of the tests are shown in the MDEA section of table 2.
Example 1:
the quenching tower 1 is filled with low-temperature COS and CS with the height of 200mm2A hydrolysis catalyst 4. The pressure of the simulated hydrogenation tail gas 7 used in the test is 5kPa, the simulated hydrogenation tail gas enters a quenching tower 1 at the temperature of 140 ℃, wherein COS and CS2100mg/Nm in terms of sulfur3，H2S2.0% volume fraction. An aqueous solution with the mass fraction of 35% prepared from MDEA is used as an absorption liquid, the temperature of the absorption liquid entering an absorption tower is 30-35 ℃, and the temperature of a rich solution is 115-120 ℃. The results of the tests are shown in the MDEA section of table 2.
Example 2:
the quenching tower 1 is filled with low-temperature COS and CS with the height of 400mm2A hydrolysis catalyst 4. The pressure of the simulated hydrogenation tail gas 7 used in the test is 5kPa, the simulated hydrogenation tail gas enters a quenching tower 1 at the temperature of 140 ℃, wherein COS and CS are2100mg/Nm in terms of sulfur3，H2S2.0% volume fraction. An aqueous solution with the mass fraction of 35% prepared from MDEA is used as an absorption liquid, the temperature of the absorption liquid entering an absorption tower is 30-35 ℃, and the temperature of a rich solution is 115-120 ℃. The results of the tests are shown in the MDEA section of table 2.
Example 3:
the quenching tower 1 is filled with low-temperature COS and CS with the height of 300mm2A hydrolysis catalyst 4. The pressure of the simulated hydrogenation tail gas 7 used in the test is 5kPa, the simulated hydrogenation tail gas enters the quenching tower 1 at 160 ℃, wherein COS and CS2100mg/Nm in terms of sulfur3，H2S2.0% volume fraction. An aqueous solution with the mass fraction of 35% prepared from MDEA is used as an absorption liquid, the temperature of the absorption liquid entering an absorption tower is 30-35 ℃, and the temperature of a rich solution is 115-120 ℃. The results of the tests are shown in the MDEA section of table 2.
Example 4:
the quenching tower 1 is filled with low-temperature COS and CS with the height of 300mm2 A hydrolysis catalyst 4. The pressure of the simulated hydrogenation tail gas 7 used in the test is 5kPa, the simulated hydrogenation tail gas enters a quenching tower at the temperature of 150 ℃, wherein COS and CS are introduced2200mg/Nm in terms of sulfur3，H2S2.0% volume fraction. An aqueous solution with the mass fraction of 35% prepared from MDEA is used as an absorption liquid, the temperature of the absorption liquid entering an absorption tower is 30-35 ℃, and the temperature of a rich solution is 115-120 ℃. The results of the tests are shown in the MDEA section of table 2.
TABLE 2 test results of comparative examples and examples
Figure 840797DEST_PATH_IMAGE001
。
From the test results shown in Table 2, it is clear that the examples using the proposed process of the present invention are compared with the comparative examples, MDEA solution, COS and CS2The removal rate of the catalyst is greatly improved, SO that the total sulfur in the purified tail gas is obviously reduced, and if the purified hydrogenation tail gas is guided to be burned, SO in the discharged waste gas is discharged2The concentration is lower than 30mg/Nm3Is significantly lower than that of the comparative example 125 mg/Nm3. Namely the method proposed by the inventionThe method can fully utilize the characteristics of the hydrogenation tail gas, the total cost of the newly added low-temperature COS and CS2 hydrolysis catalyst section is low, no special requirements are basically required for production operation, and the MDEA solvent widely used for selective desulfurization can be used. Therefore, the technical scheme of the invention shows better effect and obvious advantages.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. Reduce discharged SO of Claus sulphur recovery2The device comprises a quenching tower (1), wherein a plurality of stages of packing (3) are arranged in the quenching tower (1), a gas inlet of the quenching tower (1) is positioned below the side of the quenching tower (1), a gas outlet of the quenching tower (1) is connected with a gas inlet of a first separator (5), a gas outlet of the first separator (5) is connected with a gas inlet of an absorption tower (2), a gas outlet of the absorption tower (2) is connected with a gas inlet of a second separator (6), and the device is characterized in that: is provided with low temperature COS and CS2The hydrolysis catalyst (4) is arranged at a certain filler height, the low-temperature COS and CS2 hydrolysis catalyst (4) is arranged above a second-stage filler (3) in the quenching tower (1) from bottom to top or at a position 600-1000mm away from the bottom of the quenching tower (1) at the filler (3), and the entering hydrogenation tail gas (7) is ensured to reach the low-temperature COS and CS2The temperature of the hydrolysis catalyst (4) is 110-140 ℃.
2. The method of claim 1 for reducing Claus sulfur recovery efflux SO2The device of (2), characterized in that: the low temperature COS and CS2The hydrolysis catalyst (4) comprises aluminum oxide, the auxiliary agent is an alkaline substance, the hydrolysis catalyst is prepared by adopting an immersion method, the mass fraction of the aluminum oxide is 90-95, the mass fraction of the alkaline substance is 5-10, and the low-temperature COS and CS are obtained by low-temperature COS and CS2Hydrolysis catalyst (A)4) The space velocity is 500/h-2500/h.
3. The method of claim 1 for reducing Claus sulfur recovery efflux SO2The device is characterized in that: the low temperature COS and CS2The height of the hydrolysis catalyst (4) is 150-500 mm.
4. The method of any one of claims 1 to 3 for reducing SO emitted from Claus sulphur recovery2The device of (2), characterized in that: the temperature of the absorption liquid entering the absorption tower is less than or equal to 40 ℃, and the temperature of the rich liquid (11) absorbed by the absorption liquid at the bottom of the absorption tower is 115-125 ℃.
5. The method of any one of claims 1 to 3 for reducing Claus sulphur recovery efflux SO2The device is characterized in that: the absorption tower (2) is one or more of a plate tower, a packed tower, a super-gravity rotating bed and a micro-cyclone absorber which are connected in series and in parallel.
6. Use of a composition according to any one of claims 1 to 5 for reducing the emission of SO from Claus sulphur recovery2The device reduces the discharged SO of Claus sulfur recovery2The method comprises the following steps: the first step is as follows: hydrogenation tail gas (7) enters from the gas inlet of the quenching tower (1); the second step is that: the hydrogenation tail gas (7) is in countercurrent contact with quenching liquid sprayed from the top of the quenching tower (1) and passes through COS and CS2COS and CS in the low-temperature hydrolysis catalyst (4)2Hydrolysis to H2S、CO2And the gas outlet of the quenching tower (1); the third step: and in the second step, the gas from the gas outlet of the quenching tower (1) enters from the gas inlet of the absorption tower (2) after passing through the first separator (5), is in countercurrent contact with the lean solution (10) sprayed from the top of the absorption tower (2), and is then conveyed to the second separator (6) to separate entrained fog droplets and is led out of the system.
7. The method of claim 6, wherein: in the second step, the catalyst is subjected to COS and CS2After the low-temperature hydrolysis catalyst (4), COS and CS in the hydrogen tail gas2Hydrolysis to H2S、CO2The hydrolysis rate of (2) is more than 95%.
8. The method of claim 6, wherein: the temperature of the high-temperature hydrogenation tail gas (7) entering the quenching tower for hydrogenation reduction is 140-170 ℃.
9. The method of claim 6, wherein: in the second step, the temperature of the gas coming out of the gas outlet of the quenching tower (1) is 20-35 ℃.
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CN111620310B (en) * 2020-06-08 2022-02-01 山东华星石油化工集团有限公司 Reduce SO in sulphur tail gas2Method of discharging concentration of
CN114632409B (en) * 2022-02-23 2023-03-31 国能龙源环保有限公司 Carbonyl sulfide and hydrogen sulfide removal system suitable for different concentrations and use method thereof

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CN101721884A (en) * 2009-12-10 2010-06-09 攀枝花新钢钒股份有限公司 Smoke desulphurization agent and smoke desulphurization method
CN102600850A (en) * 2012-01-13 2012-07-25 昆明理工大学 Method for preparing catalyst capable of being subjected to carbon oxysulfide removal and carbon disulfide removal simultaneously
CN108367237A (en) * 2015-08-06 2018-08-03 氟石科技公司 Improve the system and method that sulphur is recycled from Claus process tail gases
CN108993133A (en) * 2017-06-06 2018-12-14 中国石油化工股份有限公司 COS, CS in a kind of promotion natural gas2The method of removing

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101721884A (en) * 2009-12-10 2010-06-09 攀枝花新钢钒股份有限公司 Smoke desulphurization agent and smoke desulphurization method
CN102600850A (en) * 2012-01-13 2012-07-25 昆明理工大学 Method for preparing catalyst capable of being subjected to carbon oxysulfide removal and carbon disulfide removal simultaneously
CN108367237A (en) * 2015-08-06 2018-08-03 氟石科技公司 Improve the system and method that sulphur is recycled from Claus process tail gases
CN108993133A (en) * 2017-06-06 2018-12-14 中国石油化工股份有限公司 COS, CS in a kind of promotion natural gas2The method of removing

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