CN103285722B - Highly sulfur-containing pressurized shifted gas wet-process desulphurization technique - Google Patents
Highly sulfur-containing pressurized shifted gas wet-process desulphurization technique Download PDFInfo
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Abstract
The invention provides a highly sulfur-containing pressurized shifted gas wet-process desulphurization technique which comprises the following steps of: enabling shifted gas to enter an inlet separator, enabling the shifted gas water which is separated to enter a pipeline mixer, mixing together with desulphurization solution to remove part of the hydrogen sulfide in the shifted gas, entering into a NO.1 desulphurization tower, contacting with the desulphurization solution to further remove hydrogen sulfide in the shifted gas, enabling the shifted gas to enter into a NO.2 desulphurization tower, contacting with the desulphurization solution again to remove hydrogen sulfide in the shifted gas until the hydrogen sulfide is less than 5mg/Nm<3>, separating foam through an outlet separator to the next procedure; enabling the solution to flow out of the bottom of the desulphurization tower to enter a flash tower, enabling the solution to enter a jet regeneration tank after carbon dioxide is flashed, carrying out solution regeneration through self-absorption air, enabling the regenerated desulphurization solution to enter a solution circulating tank, and pressurizing through a solution circulating pump for circulating desulphurization. According to the highly sulfur-containing pressurized shifted gas wet-process desulphurization technique, the resistance of the system is low, and the towers cannot be plugged; shifted gas with high hydrogen sulfide can be removed, and the desulphurization efficiency is high; the operation is simple, and the desulphurization and regeneration are integrally arranged; the device investment is low and takes up one quarter of a physical absorption method.
Description
Technical field
The present invention relates to sulfur removal technology, be specifically related to a kind of high sulfur-bearing pressurized shift gas wet desulfurizing process.
Background technology
Sulfur removal technology is widely used in synthetic ammonia installation, methanol device, device for producing hydrogen, belong to a major part of process for purifying, before its process station arranges decarburization after gasification, before dividing conversion, convert rear two kinds of different process, before conversion, technique is coal gas desulfurization technique, after conversion, technique is desulfuration of shift gas technique, different according to pressure, is divided into desulfurization at normal-pressure and pressurization desulfurization.
Remove H
2s is divided into two classes according to the states of matter feature difference of desulfurizing agent, i.e. dry desulfurization and wet desulphurization:
(1) dry desulfurization
Dry desulfurization adopts solid desulfurating agent, and sulfide is adsorbed and reacts on desulfurizing agent, and its sulfur capacity is large, and desulfurization precision is high, general employing three towers or two tower connection in series-parallel techniques.It utilizes the catalysed oxidn of desulfurizing agent by the H in gas
2s oxidation conversion is elemental sulfur and a small amount of water, and the elemental sulfur formed like this is deposited in the hole of desulfurizing agent carrier, makes the H of gas
2s component is converted into harmless solid elemental sulfur, is retained in desulfurizing agent, is mainly used in pole lean sulphurous gas desulfurization or deep desulfuration fine de-sulfur, the main desulfurization of inapplicable conversion gas.
(2) wet desulphurization
Wet desulphurization utilizes specific solvent contact with back flow of gas and remove H wherein
2s, C0
2, solvent, by re-starting absorption after regeneration, according to the difference of absorption mechanism, is divided into again chemical absorption method, Physical Absorption method, oxidation-reduction method.
Chemical absorption method take alkaline solution as absorbent, react with acidic components in gas and generate certain compound, absorb the solution (being called rich solution) of acidic components, under the condition of intensification step-down, make compound decomposition discharge acidic components, most representative method is MDEA method.
Physical Absorption method utilizes the difference of different component solubility in specific physical absorbent in gas and removes H
2s, then separates sucking-off H by measures such as step-down flash distillations from solvent
2s and solvent reclamation is recycled.This method is suitable for higher operating pressure, and compared with chemical absorption method, its calorific requirement is general lower.But it is more difficult comparatively speaking that physical solvent will reach high degree of purification, conventional physical solvent process comprises low-temp methanol method, polyglycol dimethyl ether process.
Oxidation-reduction method is the H absorbed with the neutrality containing oxidant or weakly alkaline solution in air-flow
2s, the carrier of oxygen in solution is by H
2s is oxidized to elemental sulfur, and solution uses with air regenesis Posterior circle.Desulfurization and sulfur recovery combine as a whole by this method, and have the advantages such as flow process is comparatively simple, investment is lower, according to the difference of sulphur oxidation catalyst, oxidation-reduction method mainly contains iron-based and vanadium base two kinds of techniques.
Low sulfur-bearing desulfuration of shift gas technique, owing to adopting coal gas desulfurization before conversion, is stripped of most of H in gas
2s, therefore H in conversion gas
2s content is not high, generally at 100-200mg/Nm
3left and right, adopts wet desulfurizing process chemiadsorption and redox adsorption method, can reach desulfurization requirement.
High sulfur-bearing desulfuration of shift gas technique, appear at pressing gas metallization processes, coal gas directly carries out shift conversion step, without desulfurization process before conversion, H in conversion gas
2s content significantly improves, generally at 1000-2000mg/Nm
3left and right, main employing Physical Absorption method low-temperature rectisol wet processing, and low-temp methanol washing process plant investment is large, the investment of more than one hundred million units, apparatus is many, has multi-stage flash system, refrigeration system, sulfur recovery system etc., and complicated operation, operating cost is higher.Because in pressurized shift gas, carbon dioxide content is high, under pressurization operating mode, gas flow rate is low, according to conventional wet sulfur removal technology chemiadsorption and redox adsorption method, then affect desulfurization regeneration, tower is blocked up in easy appearance, cannot produce, therefore need to develop a kind of high sulfur-bearing pressurized shift air humidity method new desulfurization process.
Summary of the invention
Technical problem to be solved by this invention be overcome existing desulfuration of shift gas technology above-mentioned defect and a kind of high sulfur-bearing pressurized shift gas wet desulfurizing process is provided, be specially adapted to high sulfur-bearing pressurized shift desulfurization.
For realizing the object of the invention, this high sulfur-bearing pressurized shift gas wet desulfurizing process comprises the following steps:
1-5MPa, sulfide hydrogen 500-5000mg/Nm is come from shift conversion step
3conversion gas enter import separator, conversion gas after Separation of Water enters pipe-line mixer, mix with doctor solution to remove in conversion gas and enter 1# desulfurizing tower after part hydrogen sulfide, contact with doctor solution from top to down, remove hydrogen sulfide in conversion gas further, conversion gas enters 2# desulfurizing tower, contacts with doctor solution from top to down again, removes hydrogen sulfide extremely little≤5mg/Nm in conversion gas
3, operation after discharge knockout drum separation foam goes; Bottom 1# desulfurizing tower and 2# desulfurizing tower, out solution enters flash column, after flashed carbon dioxide gas, solution enters jet regeneration tank, air self-suction carries out regeneration of waste liquor, after regeneration, doctor solution enters solution circulation groove, again through the desulfurization of solution circulation pump pressurization Posterior circle, regeneration is separated out elemental sulfur foam and is entered sulphur foam tank, after the pressurization of sulphur foam pump, go filter press to reclaim sulphur, pressing filtering liquid gravity flow back dissolving liquid circulating slot.
Adopt layer 2-4 plastics dumped packing in described 1# desulfurizing tower and 2# desulfurizing tower, gas system resistance is less than 0.05MPa, and desulfuration efficiency reaches more than 99%.
Described flash column is a pressure vessel, and after all desulfurization, solution enters this container flash distillation entirely, and flashing pressure controls as 0.5-0.6MPa, and the solution after flashed carbon dioxide all enters jet regeneration tank and carries out regeneration of waste liquor.
Compared with prior art, the invention has the advantages that:
1, SR is low, controls at 0.05MPa, and not stifled tower, pipe-line mixer is set before desulfurizing tower and absorbs H
2s, arranges a solution flash column, optimizes desulfurization regeneration operating mode after desulfurizing tower.
2, desulfuration efficiency is high, adopts pipeline to absorb and absorbs combination technique with packed tower, can take off the high conversion gas of sulfur-bearing, H
2s reaches 500-5000 mg/Nm
3, desulfuration efficiency reaches 99%, and can organic sulfide removal.
3, device is simple to operate, and desulfurization regeneration integration, do not need additionally to regenerate source of the gas, do not need low-temperature receiver, operating cost is lower.
4, plant investment is low, compared with low-temperature rectisol method, can reduce investment outlay 3/4ths, not have refrigeration system, not establish ad hoc sulfur recovery unit, do not need multistage flash evaporation.
Adopt foregoing invention to be applied to high sulfur-bearing pressurized shift desulfurization technology, possess skills, many-sided comprehensive advantage such as economy, fund.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
1: import separator; 2: pipe-line mixer; 3:1# desulfurizing tower; 4:2# desulfurizing tower; 5: discharge knockout drum; 6: flash column; 7: jet regeneration tank; 8: solution circulation groove; 9: solution circulation pump; 10: sulphur foam tank; 11: sulphur foam pump; 12: filter press.
Detailed description of the invention
The present invention is described in detail with regard to specific embodiment below in conjunction with accompanying drawing.
As shown in Figure 1, from shift conversion step come 1.85MPa, 40 DEG C, carbon dioxide 40%, hydrogen sulfide 1500mg/Nm
3conversion gas enter import separator 1, conversion gas after Separation of Water enters pipe-line mixer 2, mix with doctor solution to remove in conversion gas and enter 1# desulfurizing tower 3 after part hydrogen sulfide, contact with doctor solution from top to down, remove hydrogen sulfide in conversion gas further, conversion gas enters 2# desulfurizing tower 4, contacts with doctor solution from top to down again, remove hydrogen sulfide in conversion gas, 1.81MPa, 45 DEG C, carbon dioxide 40%, hydrogen sulfide 5mg/Nm
3conversion gas through discharge knockout drum 5 be separated foam go after operation; Bottom 1# desulfurizing tower 3 and 2# desulfurizing tower 4, out solution enters flash column 6, flash tank Stress control is at 0.5-0.6MPa, after flashed carbon dioxide gas, solution enters jet regeneration tank 7, air self-suction carries out regeneration of waste liquor, after regeneration, doctor solution enters solution circulation groove 8, then to pressurize Posterior circle desulfurization through solution circulation pump 9, and regeneration is separated out elemental sulfur foam and entered sulphur foam tank 10, after sulphur foam pump 11 is pressurizeed, filter press 12 is gone to reclaim sulphur, pressing filtering liquid gravity flow back dissolving liquid circulating slot 8.
Claims (3)
1. a high sulfur-bearing pressurized shift gas wet desulfurizing process, is characterized in that comprising following flow process: come 1-5MPa, sulfide hydrogen 500-5000mg/Nm from shift conversion step
3conversion gas enter import separator (1), conversion gas after Separation of Water enters pipe-line mixer (2), mix with doctor solution to remove in conversion gas and after part hydrogen sulfide, enter the first desulfurizing tower (3), contact with doctor solution from top to down, remove hydrogen sulfide in conversion gas further, conversion gas enters the second desulfurizing tower (4), contacts with doctor solution from top to down again, to remove in conversion gas hydrogen sulfide to≤5mg/Nm
3, operation after discharge knockout drum (5) separation foam goes; Wherein the first desulfurizing tower (3) and the second desulfurizing tower (4) bottom out solution enter flash column (6), after flashed carbon dioxide gas, solution enters jet regeneration tank (7), air self-suction carries out regeneration of waste liquor, after regeneration, doctor solution enters solution circulation groove (8), again through the desulfurization of solution circulation pump (9) pressurization Posterior circle, regeneration is separated out elemental sulfur foam and is entered sulphur foam tank (10), goes filter press (12) to reclaim sulphur, pressing filtering liquid gravity flow back dissolving liquid circulating slot (8) after sulphur foam pump (11) pressurization.
2. one according to claim 1 high sulfur-bearing pressurized shift gas wet desulfurizing process, it is characterized in that: in described first desulfurizing tower (3) and the second desulfurizing tower (4), adopt layer 2-4 plastics dumped packing, its gas system resistance is less than 0.05MPa, and desulfuration efficiency reaches more than 99%.
3. one according to claim 1 high sulfur-bearing pressurized shift gas wet desulfurizing process, it is characterized in that: described flash column (6) is a pressure vessel, after all desulfurization, solution enters this container flash distillation entirely, flashing pressure controls as 0.5-0.6MPa, and the solution after flashed carbon dioxide all enters jet regeneration tank (7) and carries out regeneration of waste liquor.
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| CN104174273B (en) * | 2014-08-12 | 2016-09-07 | 天津大学 | A kind of solar energy directly drives the integrated system and method that carbon dioxide flash distillation desorbs |
| CN106335876B (en) * | 2016-08-22 | 2019-01-08 | 中国神华能源股份有限公司 | The purification device of sulfur-bearing conversion gas |
| CN111905549B (en) * | 2019-05-08 | 2022-06-17 | 北京化工大学 | Absorb H2S desulfurization solution, desulfurization system and desulfurization method |
| CN114292672A (en) * | 2021-12-27 | 2022-04-08 | 湖南金牛化工有限公司 | Variable-pressure wet desulphurization process for high-sulfur-content gas |
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| CN1088131A (en) * | 1993-09-12 | 1994-06-22 | 浙江大学 | Remove high-concentration hydrogen sulfide and dithiocarbonic anhydride waste gas and reclaim the method and system of sulphur |
| CN1279147C (en) * | 2003-05-09 | 2006-10-11 | 湖北宜化化工股份有限公司 | Multistage desulfurizing method for synthetic ammonia system |
| CN101402884A (en) * | 2008-11-16 | 2009-04-08 | 李大路 | Process and apparatus for removing and recovering sulphur in coke oven gas |
| CN102872713B (en) * | 2012-10-25 | 2016-06-22 | 北京三聚环保新材料股份有限公司 | A kind of utilize gas transmission pipeline elimination the desulfurization of hydrogen sulfide, regenerating unit |
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