CN113617199A - Process method for treating tail gas containing hydrogen sulfide by using double-alkali method - Google Patents
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- CN113617199A CN113617199A CN202111032342.8A CN202111032342A CN113617199A CN 113617199 A CN113617199 A CN 113617199A CN 202111032342 A CN202111032342 A CN 202111032342A CN 113617199 A CN113617199 A CN 113617199A
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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
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
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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
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- 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
- B01D53/96—Regeneration, reactivation or recycling of reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2251/00—Reactants
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Abstract
The invention relates to the technical field of sulfur-related chemical production, in particular to a method for treating tail gas containing hydrogen sulfide, and specifically relates to a process method for treating tail gas containing hydrogen sulfide by a double-alkali method, wherein a Na0H solution is used for circularly absorbing H in an absorption tower2S, feeding the ammonia gas discharged from the top of the absorption tower into a chimney to perform a denitration effect on the flue gas, feeding the neutralized liquid in the absorption tower into a regeneration tower, adding a ferrous sulfate solution to generate a ferrous sulfide precipitate, adding lime milk to generate a calcium sulfate precipitate after the reaction is finished, filtering the precipitate, wherein the obtained filtrate is a regenerated NaOH solution, and the regenerated liquid is returned to the absorption tower for use. The process is to the catalyst containing H2The tail gas of the S is absorbed and treated, and the operation is simple and easy. The equipment investment is small, the absorption efficiency of the tail gas is high, and no waste liquid is discharged. The obtained gypsumAnd the ferrous sulfide waste residue can not generate secondary pollution. The used regenerative raw materials of quicklime and ferrous sulfate are low in price and easy to purchase, and the tail gas treatment cost is very low.
Description
Technical Field
The invention relates to the technical field of chemical production related to sulfur, in particular to a method for treating tail gas containing hydrogen sulfide, and specifically relates to a process method for treating tail gas containing hydrogen sulfide by a double-alkali method.
Background
In chemical production with sulfur, the tail gas often contains a small amount of hydrogen sulfide gas. For example, in the production of separating waste sulfur into tail gas, relatively pure liquid sulfur and solid residue by heating and gasifying and then condensing the waste sulfur in a coke-oven plant, the generated tail gas contains a small amount of hydrogen sulfide gas. Some units use a treatment method of feeding the tail gas containing a small amount of hydrogen sulfide into a chimney for combustion. The method has the defects that firstly, the safety performance is poor, the tempering phenomenon is easy to generate, and the tail gas is combusted and exploded. Secondly, the emission of sulfur dioxide in the flue gas is increased. In addition, a spraying method is used for absorbing the hydrogen sulfide in the tail gas. However, absorption waste liquid has no good treatment method. Some coke plants add soda ash to the desulfurization solution, while most coke plants add ammonia to the desulfurization solution. In the purification production of the sulfur cake which is removed from soda ash desulfurization factories, the generated tail gas only contains hydrogen sulfide and does not contain ammonia. During the purification production of sulfur cakes which are removed from factories in ammonia water desulfurization, the generated tail gas contains hydrogen sulfide and ammonia gas, and the ammonia gas also needs to be purified.
Disclosure of Invention
The invention aims to effectively remove hydrogen sulfide and ammonia gas in tail gas of chemical production, and provides a process method for treating tail gas containing hydrogen sulfide by using a double-alkali method.
The invention is realized by adopting the following technical scheme: a process for treating tail gas containing hydrogen sulfide by dual-alkali method includes such steps as cyclically absorbing H in tail gas by NaOH solution in absorption tower2S, pumping the obtained neutralization solution into a regeneration tank for regeneration treatment, pumping new NaOH solution into an absorption tower for continuously and circularly absorbing H in tail gas up and down2And S, the regeneration treatment process in the regeneration tank comprises the steps of firstly adding a ferrous sulfate solution to generate a ferrous sulfide precipitate, adding lime milk after the reaction is finished to generate a calcium sulfate precipitate, finally filtering the precipitate to obtain a filtrate which is a Na0H regeneration solution, and pumping the regeneration solution into a Na0H solution tank for the absorption tower to be reserved.
If the tail gas contains NH, the process method for treating the tail gas containing the hydrogen sulfide by the double-alkali method3NH discharged from the top of the absorption column3And (4) feeding the flue gas into a chimney by using a pipeline to denitrate the flue gas.
In the above-mentioned process for treating tail gas containing hydrogen sulfide by using double-alkali method, the pH value of NaOH solution is required to be in the range of 8-9, and after the pH value is lower than the pH value, the obtained neutralized solution is fed into regeneration tank. And stirring by using a stirrer in the regeneration treatment process in the regeneration tank. And (3) feeding the materials in the regeneration tank into a centrifuge for precipitate filtration, automatically feeding the filtrate into a Na0H filtrate tank, and feeding the solution in the Na0H filtrate tank into a Na0H solution tank for the absorption tower to be reserved. Preparing lime milk by digestion reaction, putting quantitative quicklime into a digestion tank, then injecting a proper amount of water, filtering the materials after the reaction is finished, filtering out impurities to obtain pure lime milk, and pumping the lime milk into a lime milk tank for later use by a sewage pump. The preparation process of the ferrous sulfate solution comprises the following steps: injecting a certain amount of water into the ferrous sulfate solution tank, slowly adding a proper amount of ferrous sulfate raw materials, stirring the mixture, and preparing a ferrous sulfate solution with a certain concentration after the added raw materials are completely dissolved. The preparation process of the sodium hydroxide solution comprises the following steps: a certain amount of water is injected into a Na0H solution tank, then a proper amount of solid caustic soda is slowly added, the mixture is stirred, and after all the added caustic soda is dissolved, a Na0H solution with a certain concentration is prepared.
The process is to the catalyst containing H2The tail gas of the S is absorbed and treated, and the operation is simple and easy. The equipment investment is small, the absorption efficiency of the tail gas is high, and no waste liquid is discharged. The obtained gypsum and ferrous sulfide waste residue can not generate secondary pollution. The used regenerative raw materials of quicklime and ferrous sulfate are low in price and easy to purchase, and the tail gas treatment cost is very low. In the chemical production, if tail gas is generated and the content of hydrogen sulfide gas in the tail gas is not too much, the process for treating the tail gas is simple and easy to implement and is very practical.
Drawings
FIG. 1 is a process flow diagram of a double alkali process for treating tail gas containing hydrogen sulfide.
FIG. 2 is a process flow diagram of a double alkali process for treating tail gas containing hydrogen sulfide and ammonia gas.
In the figure: 1-tail gas sent by a fan, 2-an absorption tower, 3-a tail gas outlet of the absorption tower, 4-Na0H solution tank, 5-a circulating pump, 6-a lime milk tank, 7-a digestion tank, 8-a regeneration tank, 9-a ferrous sulfate solution tank, 10-Na0H filtrate tank, 11-a centrifugal machine, 12-a milk pump, 13-a slurry pump, 14-a solution pump, 15-a stirrer, 16-a chimney and 17-a fan; the first valve, the second valve, the third valve, the fourth valve, the fifth valve and the sixth valve.
Detailed Description
A process for treating tail gas containing hydrogen sulfide by using a double alkali method is shown in figure 1.
The circulating liquid outlet of the absorption tower 2 is connected with the inlet of a circulating pump 5 through a pipeline, the pipeline is provided with a first valve, the outlet of the circulating pump 5 is connected with the circulating liquid inlet of the absorption tower 1 through a pipeline, the pipeline is provided with a third valve, the outlet of the circulating pump 5 is also connected with a regeneration tank 8 through a pipeline, the pipeline is provided with a fourth valve, a Na0H solution tank 4 is connected with the inlet of the circulating pump 5 through a pipeline, the pipeline is provided with a second valve, a lime milk tank 6 is connected with the inlet of a milk pump 12 through a pipeline, the outlet of the milk pump 12 is connected with the regeneration tank 8 through a pipeline, a ferrous sulfate solution tank 9 is connected with the regeneration tank 8 through a pipeline, the pipeline is also provided with a sixth valve, the regeneration tank 8 is connected with the inlet of a pulp pump 13 through a pipeline, the outlet of the pulp pump 13 is connected with a centrifugal machine 11 through a pipeline, the centrifugal machine 11 is connected with a Na0H filtrate tank 10 through a pipeline, the Na0H filtrate tank 10 is connected to the inlet of the solution pump 14 via a pipe, the pipe is also provided with a fifth valve, and the outlet of the solution pump 14 is also connected to the Na0H solution tank 4 via a pipe.
The technological process includes feeding tail gas containing hydrogen sulfide into the absorption tower 2 with blower, setting ceramic ring stuffing in the upper part of the absorption tower 2, spraying with spraying device and circulating water solution of NaOH. The spraying liquid from top to bottom and the tail gas from bottom to top flow in the reverse direction, and the gas phase and the liquid phase are subjected to sufficient mass transfer action under the action of the ceramic ring. The hydrogen sulfide in the gas phase and NaOH in the liquid phase are subjected to neutralization reaction, so that the hydrogen sulfide in the tail gas is sufficiently chemically absorbed.
After the absorption reaction is carried out for a certain period of time, the alkalinity of the absorption solution is reduced. The neutralization reaction is carried out in the absorption column 2. The reaction equation is:
H2s ten 2NaOH = Na2S+2H20。
The pH of the absorption liquid is required to be in the range of 8 to 9. After the value is lower than the above value, the neutralized liquid in the absorption tower can be fed into the regeneration tank 8 by three operations. And the caustic soda solution in the Na0H solution tank 4 is driven into the absorption tower through operation one. The absorption work is started by operation two.
And 5, preparing lime milk in a lime milk tank 6 for later use by operating five.
The ferrous sulfate solution is prepared in the ferrous sulfate solution tank 9 for standby through operation six.
The neutralization solution was regenerated by operation three.
The Na0H filtrate obtained by regeneration was returned to the Na0H solution tank 4 for further use in operation IV.
The preparation of the sodium hydroxide solution was carried out by operation seven. So as to meet the requirement of the absorption liquid.
The reactions taking place in the regeneration tank 8 are:
S2-ten Fe2+ =FeS↓
Na2S04Ten Ca (0H)2=CaS04↓ + ten 2Na0H
Ca2+Ten S04 2-=CaS04↓
The first operation is that the first valve and the fourth valve are closed, the second valve and the third valve are opened and the circulating pump 5 is started, and the solution in the Na0H solution tank 4 is pumped into the absorption tower 2.
And the second operation is to close the second valve and the fourth valve, open the first valve and the third valve and the circulating pump 5, circulate the solution in the absorption tower 2 up and down, and absorb the tail gas by the absorption tower 2.
And thirdly, closing the second valve and the third valve, opening the first valve and the fourth valve, starting the circulating pump 5, and pumping the neutralized liquid in the absorption tower into the regeneration tank 8. The stirrer 15 is started, the sixth valve is opened, and a proper amount of ferrous sulfate solution is slowly put into the regeneration tank 8. According to Na in a regeneration tank2The content of S determines the input amount of the ferrous sulfate solution. So that most of the sulfur ions and iron ions in the regeneration tank generate ferrous sulfide precipitate, but the input amount cannot be excessive. After the feeding is finishedClosing the sixth valve. Stirring is continued. After the reaction for generating ferrous sulfide is completed, the milk pump 12 is started, and a proper amount of lime milk is put into the regeneration tank 8. A reaction occurs in which calcium ions react with sulfate ions to form calcium sulfate precipitates. The input amount of the lime milk is accurately determined according to the sulfate radical content in the regeneration tank 8. After the reaction of generating calcium sulfate is finished, starting a slurry pump 13 to pump the materials in the regeneration tank into a centrifuge 11 for filtration in several times. The filtrate automatically flows into the Na0H filtrate tank 10.
Operation four, opening the fifth valve, starting the solution pump 14, then pumping the solution in the Na0H filtrate tank 10 into the Na0H solution tank 4 for the absorption tower to be ready.
The filter cake of the centrifuge is gypsum and ferrous sulfide.
Fifthly, preparing lime milk through digestion reaction. Quantitative quicklime is put into the digestion tank 7, and then a proper amount of water is injected, so that the reaction is vigorously carried out. The reactions that occur are:
Ca0+H20=Ca(0H)2。
after the reaction is finished, the materials are simply filtered, and impurities are filtered out. Obtaining purer lime milk. Pumping the lime milk into a lime milk tank 6 by a sewage pump for later use.
Sixthly, preparing a ferrous sulfate solution. A certain amount of water is poured into the ferrous sulfate solution tank 9, and then a proper amount of ferrous sulfate raw material is slowly poured into the tank, so that the raw material is stirred. After the added raw materials are completely dissolved, a ferrous sulfate solution with a certain concentration is prepared.
Seventhly, preparing a sodium hydroxide solution. A certain amount of water is poured into the Na0H solution tank 4, and then a proper amount of solid caustic soda is slowly added, so that the mixture is stirred. After all the added caustic soda is dissolved, Na0H solution with a certain concentration is prepared.
Most coking plants adopt ammonia water for desulfurization, and the produced solid waste sulfur contains a small amount of ammonium salt. When the waste sulfur is heated, gasified and purified by using combustion gas, the generated tail gas contains a small amount of ammonia gas in addition to a small amount of hydrogen sulfide. The absorption treatment process of the hydrogen sulfide in the tail gas is the same as the process described above, but the absorption tower only absorbs the hydrogen sulfide and does not absorb ammonia gas, and the ammonia gas is discharged from the top of the absorption tower and then is sent into a chimney by a pipeline. The ammonia gas is used for denitration of flue gas generated by heating waste sulfur burning coal gas. The denitration reaction formula is as follows:
4NH3+02ten 4NO =4N2+6H2O
4NH3+02+2N02=3N2Ten 6H20。
The process flow diagram is shown in figure 2.
The process carries out desulfurization treatment on tail gas and carries out denitration treatment on flue gas.
In the embodiment, the waste sulfur is indirectly heated by burning coal gas, and the waste sulfur liquid starts to be gasified when the temperature reaches more than 450 ℃. Gas phase is condensed to obtain relatively pure liquid sulfur, and the produced tail gas contains a small amount of H2S and NH3. For the waste sulfur purification production line of 30 tons of sulfur produced per day, H is contained in the produced tail gas2The discharge of S is about 100 Kg/day, NH3The discharge amount of (2) is about 20 Kg/day. Absorbing H in the tail gas2S, consumption of the caustic soda flakes Na0H235 Kg/day. The input amount of ferrous sulfate in the regeneration tank is 433 Kg/day, and the generated precipitate ferrous sulfide is 235 Kg/day. The input amount of lime milk in the regeneration tank is 96 kg/day, and calcium sulfate precipitate 383 kg/day is generated. The waste residue filtered out is about 636 Kg/day, and the regenerated Na0H is about 226 Kg/day. The consumption flow of the quicklime in the digestion tank is about 80 Kg/day.
The steps for treating the tail gas are as follows:
1, preparing equipment, namely an absorption tower, namely a spray tower, which is commercially available equipment. A spray tower with a diameter of 1.5 meters and a height of more than 8 meters is selected. The Na0H solution tank was fabricated to have a size of 1.5m (long) × 1.5m () × 2m (high). The regeneration tank is manufactured according to the size of 2m (width) X3 m (length) X2m (height). The Na0H filtrate tank was made in the size of 2m (length) x2m (width) x 1m (height). The ferrous sulfate solution tank is made into a round tank with the height of 2 meters and the diameter of 1.5 meters. The digestion tank is made in the size of 2m (long) x 1m (wide) x2m (high). Are welded from a 304 stainless steel plate 8 mm thick.
The material conveying pump is purchased from the market.
2, equipment installation, namely installing the equipment according to the attached figure 2.
3, tail gas treatment operation, namely injecting 3 cubic meters of water into a Na0H solution tank, and then adding 250Kg of caustic soda flakes into the water under continuous stirring. The resulting Na0H solution was pumped into an absorption column by operation one. And the tail gas absorption work is started through the second operation.
80Kg of quicklime is put into a digestion tank, and then a proper amount of water is injected to complete the reaction. Filtering to remove impurities, pumping into a lime milk tank by a sewage pump for later use.
2-3 cubic meters of water is injected into a ferrous sulfate solution tank, and then 433Kg of ferrous sulfate corresponding crystals with crystal water are slowly put into the water, and then the mixture is stirred. To prepare ferrous sulfate solution for later use.
After the absorption operation was carried out for 24 hours, the neutralization solution was regenerated by the third operation. The neutralized solution is added into a regeneration tank, and then the prepared ferrous sulfate solution is added into regeneration and stirred. And after the reaction for generating the ferrous sulfide is finished, adding the prepared lime milk into the regeneration tank. The mixture is put in and stirred. After the reaction of generating calcium sulfate is finished, the materials in the regeneration pool are fed into a centrifuge in batches for filtering. The prepared Na0H filtrate returns to the absorption tower to continue absorption work.
The above work is a workday. The operation is repeated, and the absorption work is continuously carried out day after day. And NH discharged from the top of the absorption tower3And (4) conveying the flue gas into a chimney by using a pipeline to perform denitration reaction on the flue gas.
Claims (2)
1. A process method for treating tail gas containing hydrogen sulfide by a double alkali method is characterized by comprising the following steps: h in tail gas is absorbed by NaOH solution in the absorption tower (2) in a vertical circulation manner2S, the obtained neutralization solution is pumped into a regeneration tank (8) for regeneration treatment, and new NaOH solution is pumped into an absorption tower (2) for continuously and circularly absorbing H in tail gas up and down2S, the regeneration treatment process in the regeneration tank (8) comprises the steps of firstly adding a ferrous sulfate solution to generate a ferrous sulfide precipitate, adding lime milk after the reaction is finished to generate a calcium sulfate precipitate, finally filtering the precipitate to obtain a filtrate, namely a Na0H regeneration solution, and adding the regeneration solution into a Na0H solution tank (4) for the absorption tower (2) to be reserved.
2. The process of claim 1, wherein the double alkali method is used for treating tail gas containing hydrogen sulfide, and the process comprises the following steps: if the tail gas contains NH3And then the tail gas discharged from the top of the absorption tower is sent into a chimney by a pipeline to denitrate the flue gas.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115090096A (en) * | 2022-06-06 | 2022-09-23 | 武汉天源环保股份有限公司 | Landfill leachate deodorization method and system |
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| JPH07268357A (en) * | 1994-03-31 | 1995-10-17 | Sekiyu Sangyo Kasseika Center | Method for treating hydrogen sulfide-containing gas |
| RU2199374C1 (en) * | 2001-06-13 | 2003-02-27 | Казанское открытое акционерное общество "Органический синтез" | Method of alkali purification of pyrolysis gases |
| CN104556147A (en) * | 2014-12-18 | 2015-04-29 | 成都华西堂投资有限公司 | Process for preparing SCR reducing agent from coking residual ammonia wastewater as raw material |
| CN105664712A (en) * | 2016-03-28 | 2016-06-15 | 济南冶金化工设备有限公司 | Coking flue gas denitration and ammonia-containing tail gas purifying system |
| CN206986110U (en) * | 2017-01-13 | 2018-02-09 | 久泰能源内蒙古有限公司 | A kind of Denitration in Boiler system using ammonia-contaminated gas as denitrfying agent |
| CN109824165A (en) * | 2017-11-23 | 2019-05-31 | 上海江柘环境工程技术有限公司 | A kind of sulfur-containing waste water treatment process |
| CN209619062U (en) * | 2019-01-23 | 2019-11-12 | 湖南北控威保特环境科技股份有限公司 | A kind of sulfur-containing waste water processing system |
-
2021
- 2021-09-03 CN CN202111032342.8A patent/CN113617199A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07268357A (en) * | 1994-03-31 | 1995-10-17 | Sekiyu Sangyo Kasseika Center | Method for treating hydrogen sulfide-containing gas |
| RU2199374C1 (en) * | 2001-06-13 | 2003-02-27 | Казанское открытое акционерное общество "Органический синтез" | Method of alkali purification of pyrolysis gases |
| CN104556147A (en) * | 2014-12-18 | 2015-04-29 | 成都华西堂投资有限公司 | Process for preparing SCR reducing agent from coking residual ammonia wastewater as raw material |
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| CN206986110U (en) * | 2017-01-13 | 2018-02-09 | 久泰能源内蒙古有限公司 | A kind of Denitration in Boiler system using ammonia-contaminated gas as denitrfying agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115090096A (en) * | 2022-06-06 | 2022-09-23 | 武汉天源环保股份有限公司 | Landfill leachate deodorization method and system |
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