CN101457162A - Wet-type absorption coke oven gas desulphurization and decyanation process using ammine as alkali source - Google Patents
Wet-type absorption coke oven gas desulphurization and decyanation process using ammine as alkali source Download PDFInfo
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- CN101457162A CN101457162A CNA2007101588167A CN200710158816A CN101457162A CN 101457162 A CN101457162 A CN 101457162A CN A2007101588167 A CNA2007101588167 A CN A2007101588167A CN 200710158816 A CN200710158816 A CN 200710158816A CN 101457162 A CN101457162 A CN 101457162A
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Abstract
The invention belongs to the chemical engineering technology field relating to a wet-type absorption method gas desulfurization and decyanation process which uses ammine as alkali source and is characterized by using ammine in the gas as alkali source, employing desulphurization rich solution pressurized hydrolysis decyanation and pressurized deacidification technical method and comprising working procedures such as gas desulfurization, rich solution decyanation, rich solution deacidification, ammonia distillation and sulfur recovery or the like. The invention is a wet-type absorption method gas desulfurization and decyanation process which uses ammine as alkali source, which uses the ammine in the gas as alkali source, employs desulphurization rich solution pressurized hydrolysis decyanation and pressurized deacidification technical method to enable the gas satisfying the demand of ''coking industry admittance criteria'' without secondary pollution and obtains high-purity sulfur with simple operation.
Description
Technical field
The invention belongs to chemical technology field, relating to ammonia is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source.
Background technology
At present, domestic in the existing desulfurization and decyanation technology of coke-oven gas, it is the HPF method of alkali source that wet oxidation process adopts mostly with ammonia, and it is the ammonia sulphur cycle washing method of alkali source, i.e. AS method that the wet absorption rule adopts with ammonia.Production practice show that there is different problems separately in these two kinds of technologies.Problems such as the subject matter of HPF method is that waste liquid is difficult to handle, the ammonia loss in the regeneration overhead tail gas is many, atmosphere pollution, sulphur cream are of poor quality, sales difficulty.The AS rule exists that desulfuration efficiency is low, purified gas can not satisfy the requirement of coking industry entry criteria, processing condition require harsh, as influence normal running factor complexity, operative technique to require problems such as height, equipment corrosion and obstruction be serious.Therefore, be necessary to develop a kind of new desulfurization and decyanation technology, in the hope of thoroughly solving the problem of above-mentioned existence.
Summary of the invention
The present invention has overcome the defective of above-mentioned existence, purpose is that in " coal chemical enterprise entry criteria " the hydrogen sulfide containing requirement of coke-oven gas, sulfur removal technology itself not to be produced secondary pollution, products obtained therefrom output height, quality good for coke-oven-gas desulfurization and decyanation provides a kind of desulfuration efficiency can satisfy country, and the technology power consumption is low, reduced investment, short, the easy-operating technical process of flow process.
The present invention is the wet absorption method coke-oven-gas desulfurization and decyanation technology content Description of alkali source with ammonia:
The present invention is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, it is characterized in that: be to be alkali source with the ammonia in the coal gas, adopt pressurized hydrolysis decyanation of desulfurization rich solution and pressurization depickling technological method, form by coal gas desulfurization, rich solution decyanation, rich solution depickling, ammonia still process and sulphur recovery operation:
(1) coal gas desulfurization: 22～25 ℃ of temperature, hydrogen sulfide content 6～8g/m
3Coke-oven gas enter thionizer, with the absorption liquid counter current contact that contains ammonia 8～10g/L, rich solution is from pumping to step for regeneration with pump at the bottom of the tower; The ammoniacal liquor sweetening process is thermopositive reaction, for keeping the cold operation of desulfurization whole process, is provided with Aftercooling device at the thionizer middle part, so that the hydrogen sulfide content in the coke-oven gas behind the thionizer reaches 20mg/m
3
(2) rich solution decyanation: the rich solution that has absorbed hydrogen sulfide enters the rich solution groove, pressurize with high-pressure pump, enter the decyanation tower again with behind hot lean solution heat exchange to 130～140 at the bottom of the extracting tower ℃, rich solution stops 1h in the decyanation tower, with the steam heating hydrolysis of 1MPa, hydrogen cyanide content is reduced to the following decyanation rich solution of 0.2g/L and is entered extracting tower;
(3) rich solution depickling: 130～140 ℃ rich solution enters the extracting tower stage casing through after the decyanation, establish the reboiler heating at the bottom of the tower, and open steam is gone in past extracting tower bottom blowing, sour gas such as hydrogen sulfide in the rich solution and carbonic acid gas are overflowed by cat head, separate through water trap, sour gas is overflowed from the water trap top, send sulfur recovery unit production high purity sulphur; Send into from the extracting tower top without the cold rich solution of preheating 8%～10%, to absorb the ammonia in the sour gas, lean solution recycles with pumped back coal gas desulfurization operation after heat exchange, cooling at the bottom of the tower; Extracting tower is operated under the pressure of 0.4～0.5MPa, and tower top temperature is 30～40 ℃, and the hydrogen sulfide content in the depickling lean solution maintains 0.2g/L;
(4) ammonia still process: the doctor solution of extraction 10% and remained ammonia are delivered to ammonia still together and are handled, and the ammonia vapour of ammonia still process cat head returns in the preceding gas line of thionizer, and the distilled ammonia wastewater at the bottom of the tower is delivered to the wastewater containing phenol and cyanide treatment unit after heat exchange, cooling;
(5) sulfur recovery: adopt conventional Cross unit to produce the high-quality sulphur of purity 99.9%, sulfur recovery rate can reach 97%, and the tail gas of Cross unit can be blended in the gas line of negative pressure system.
The present invention is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, be to be alkali source with the ammonia in the coal gas, adopt pressurized hydrolysis decyanation of desulfurization rich solution and pressurization depickling technological method, with the requirement of satisfying purified gas and can reach " coking industry permit standard ", do not produce secondary pollution, simple to operate, can obtain high purity sulphur.
Description of drawings
Fig. 1 is to be the wet absorption method coal gas desulfurization novel process synoptic diagram of alkali source with ammonia
Fig. 2 is to be the wet absorption method coke oven gas desulfurization process flow chart of alkali source with ammonia
Embodiment
The present invention is that the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source is achieved in that to do below in conjunction with accompanying drawing and specifies with ammonia.See Fig. 1, Fig. 2, with ammonia is the wet absorption method coal gas desulfurization decyanation technology of alkali source, be to be alkali source, adopt pressurized hydrolysis decyanation of desulfurization rich solution and pressurization depickling technological method, form by operations such as coal gas desulfurization, rich solution decyanation, rich solution depickling, ammonia still process and sulphur recovery with the ammonia in the coal gas.
(1) coal gas desulfurization operation.22～25 ℃ of temperature, hydrogen sulfide content 6～8g/m
3Coke-oven gas enter thionizer, with the absorption liquid counter current contact that contains ammonia 8～10g/L, rich solution is from pumping to step for regeneration with pump at the bottom of the tower.The ammoniacal liquor sweetening process is thermopositive reaction, in order to keep the cold operation of desulfurization whole process, is provided with Aftercooling device at the thionizer middle part, so that the hydrogen sulfide content in the coke-oven gas behind the thionizer reaches 20mg/m
3Level.
(2) rich solution decyanation operation.The rich solution that has absorbed hydrogen sulfide enters the rich solution groove, with high-pressure pump pressurization, enter the decyanation tower again with behind hot lean solution heat exchange to 130～140 at the bottom of the extracting tower ℃, rich solution stops 1h in the decyanation tower, with the steam heating hydrolysis of 1MPa, hydrogen cyanide content is reduced to the following decyanation rich solution of 0.2g/L and is entered extracting tower.
(3) rich solution deacidification process.130～140 ℃ rich solution enters the extracting tower stage casing through after the decyanation, establish the reboiler heating at the bottom of the tower, and open steam is gone in past extracting tower bottom blowing, sour gas such as hydrogen sulfide in the rich solution and carbonic acid gas are overflowed by cat head, separate through water trap, sour gas is overflowed from the water trap top, send sulfur recovery unit production high purity sulphur.Because contained ammonia is unfavorable for the recovery of sulphur in the sour gas.For reducing the ammonia quantity in the sour gas, generally be to send into from the extracting tower top without the cold rich solution of preheating, to absorb the ammonia in the sour gas with 8%～10%.Lean solution recycles with pumped back coal gas desulfurization operation after heat exchange, cooling at the bottom of the tower.Extracting tower is operated under the pressure of 0.4～0.5MPa, and tower top temperature is 30～40 ℃.Require extracting tower to remove sour gas as much as possible, maintain 0.2g/L, thereby improve the desulfuration efficiency of coal gas to guarantee the hydrogen sulfide content in the depickling lean solution.
(4) ammonia still process.Doctor solution descends desulfuration efficiency because of impurity salts such as accumulation thiocyanate-and thiosulphates in working cycle and causes equipment corrosion, must extract 10% doctor solution and remained ammonia out delivers to ammonia still together and handles, the ammonia vapour of ammonia still process cat head returns in the preceding gas line of thionizer, and the distilled ammonia wastewater at the bottom of the tower is delivered to the wastewater containing phenol and cyanide treatment unit after heat exchange, cooling.
(5) sulfur recovery process.Because contain a spot of prussic acid and ammonia in the sour gas that the depickling cat head is overflowed, hydrogen sulfide and carbonic acid gas then account for more than 90%.Therefore, can adopt conventional Cross unit to produce the high-quality sulphur of purity 99.9% fully, sulfur recovery rate can reach 97%.The tail gas of Cross unit can be blended in the gas line of negative pressure system.
The characteristics of the wet absorption method coal gas desulfurization decyanation technology of the present invention take ammonia as alkali source are: (1) When the carbon dioxide content in coke-stove gas is 5～10 times of hydrogen sulfide, take ammonia as alkali source Absorption liquid absorbing hydrogen sulphide as much as possible in desulfurizing tower, and few absorbing carbon dioxide. So The design of desulfurizing tower should be accomplished to lack big, the high gas speed of mass transfer area and time of contact as far as possible, makes liquid Distribute to drip shape, be conducive to selective absorbing hydrogen sulphide.
(2) the pre-decyanation device of sulfur removing pregnant solution is set before extracting tower, can makes with pressurized hydrolysis and take off Hydrogen cyanide content in the sulphur rich solution is reduced to below the 0.2g/L. One of its purpose is to improve coal gas Decyanation efficient makes the hydrogen cyanide content＜200mg/m in the coal gas behind the tower3, secondly be to reduce desulfurization The corrosivity of rich solution is achieved the operation of depickling under pressure.
(3) adopt depickling under the pressure, can not only improve the deacidification efficiency of extracting tower, and can make Sour gas in the sulfur removing pregnant solution can separate preferably with ammonia, to guarantee the sulfuration in the depickling lean solution Hydrogen content＜0.2g/L, and can improve the desulfuration efficiency of desulfurizing tower makes behind the desulfurizing tower in the coal gas Hydrogen sulfide content satisfies the requirement of " coal chemical enterprise entry criteria ", also can make in the sour gas Ammon amount maintain reduced levels, be conducive to the normal operating of Cross unit.
(4) sour gas can be produced high-purity sulphur, Cross unit in sulfur recovery unit Tail gas can return in the negative pressure system of converting coke-stove gas, whole desulphurization system does not have waste liquid and produces, Can not produce secondary pollution yet.
Before the wet type suction method desulfuration and decyanation device of the present invention take ammonia as alkali source should be placed on air blast Carry out negative-pressure operation, can make the flow process of whole gas cleaning system reach the shortest, thermograde It is more reasonable to change. This process using ammonia is alkali source, does not use catalyst. The pressurization of sulfur removing pregnant solution Hydrolysis decyanation and pressurization depickling can improve deacidification efficiency, and the desulfurization that also can increase substantially coal gas is taken off Cyanogen efficient, sulfur purity height, the quality of production are good, and flow process is simple, and non-secondary pollution is Desirable coke-oven-gas desulfurization and decyanation technology.
Claims (6)
1, a kind of is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, it is characterized in that with the ammonia in the coal gas be alkali source, adopt pressurized hydrolysis decyanation of desulfurization rich solution and pressurization depickling technological method, form by coal gas desulfurization, rich solution decyanation, rich solution depickling, ammonia still process and sulphur recovery operation.
2, according to claim 1 is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, it is characterized in that described coal gas desulfurization: 22～25 ℃ of temperature, hydrogen sulfide content 6～8g/m
3Coke-oven gas enter thionizer, with the absorption liquid counter current contact that contains ammonia 8～10g/L, rich solution is from pumping to step for regeneration with pump at the bottom of the tower; The ammoniacal liquor sweetening process is thermopositive reaction, for keeping the cold operation of desulfurization whole process, is provided with Aftercooling device at the thionizer middle part, so that the hydrogen sulfide content in the coke-oven gas behind the thionizer reaches 20mg/m
3
3, according to claim 1 is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, it is characterized in that: described rich solution decyanation: the rich solution that has absorbed hydrogen sulfide enters the rich solution groove, pressurize with high-pressure pump, enter the decyanation tower again with behind hot lean solution heat exchange to 130～140 at the bottom of the extracting tower ℃, rich solution stops 1h in the decyanation tower, with the steam heating hydrolysis of 1MPa, hydrogen cyanide content is reduced to the following decyanation rich solution of 0.2g/L and is entered extracting tower.
4, according to claim 1 is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, it is characterized in that: described rich solution depickling: 130～140 ℃ rich solution enters the extracting tower stage casing through after the decyanation, establish the reboiler heating at the bottom of the tower, and open steam is gone in past extracting tower bottom blowing, sour gas such as hydrogen sulfide in the rich solution and carbonic acid gas are overflowed by cat head, separate through water trap, sour gas is overflowed from the water trap top, send sulfur recovery unit production high purity sulphur; Send into from the extracting tower top without the cold rich solution of preheating 8%～10%, to absorb the ammonia in the sour gas, lean solution recycles with pumped back coal gas desulfurization operation after heat exchange, cooling at the bottom of the tower; Extracting tower is operated under the pressure of 0.4～0.5MPa, and tower top temperature is 30～40 ℃, and the hydrogen sulfide content in the depickling lean solution maintains 0.2g/L.
5, according to claim 1 is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, it is characterized in that: described ammonia still process: the doctor solution of extraction 10% and remained ammonia are delivered to ammonia still together and are handled, the ammonia vapour of ammonia still process cat head returns in the preceding gas line of thionizer, and the distilled ammonia wastewater at the bottom of the tower is delivered to the wastewater containing phenol and cyanide treatment unit after heat exchange, cooling.
6, according to claim 1 is the wet absorption method coke-oven-gas desulfurization and decyanation technology of alkali source with ammonia, it is characterized in that: described sulfur recovery: adopt conventional Cross unit to produce the high-quality sulphur of purity 99.9%, the rate of recovery can reach 97%, and the tail gas of Cross unit can be blended in the gas line of negative pressure system.
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Cited By (9)
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| CN102101006A (en) * | 2011-01-21 | 2011-06-22 | 内蒙古庆华集团庆华煤化有限责任公司 | Process for removing SO2 in smoke from boiler of coking plant by utilizing residual coked ammonia water |
| CN103264991A (en) * | 2013-06-04 | 2013-08-28 | 枣庄德信环保技术有限公司 | Method for processing sulfur paste as coke oven gas desulfuration by-product |
| CN103820171A (en) * | 2014-03-12 | 2014-05-28 | 邯郸市裕泰燃气有限公司 | Coal gas desulfurization device |
| CN105238449A (en) * | 2015-09-29 | 2016-01-13 | 山东钢铁股份有限公司 | Desulfurization method of coke oven gas |
| CN105694988A (en) * | 2016-03-03 | 2016-06-22 | 金能科技股份有限公司 | Process for solving coal gas desulfuration liquid expansion in coking industry and system for process |
| CN105985814A (en) * | 2015-02-09 | 2016-10-05 | 上海同特化工科技有限公司 | Treatment technology for removing hydrogen sulfide, hydrogen cyanide and ammonia in coal gas |
| CN106244249A (en) * | 2016-08-29 | 2016-12-21 | 中冶焦耐(大连)工程技术有限公司 | A kind of coke-oven-gas desulfurization and decyanation alkali wash section base extraction technique and device |
| CN108384582A (en) * | 2018-02-22 | 2018-08-10 | 中冶焦耐(大连)工程技术有限公司 | A kind of system and technique for strengthening deacidifion desorption |
| CN115196809A (en) * | 2022-08-04 | 2022-10-18 | 广西钢铁集团有限公司 | Method for removing hydrogen cyanide in rich solution by using pressurization type AS (acrylonitrile-styrene) desulfurization process in coking plant |
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| CN1227253A (en) * | 1998-12-30 | 1999-09-01 | 宝山钢铁(集团)公司 | Desulfurizing and decyanating method for coke oven gas |
| CN100384516C (en) * | 2003-12-09 | 2008-04-30 | 南化集团研究院 | Improved method for removing sulfur by vanadium based wet-type oxidization |
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- 2007-12-12 CN CN2007101588167A patent/CN101457162B/en not_active Expired - Fee Related
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| CN102101006B (en) * | 2011-01-21 | 2013-08-28 | 内蒙古庆华集团庆华煤化有限责任公司 | Process for removing SO2 in smoke from boiler of coking plant by utilizing residual coked ammonia water |
| CN102101006A (en) * | 2011-01-21 | 2011-06-22 | 内蒙古庆华集团庆华煤化有限责任公司 | Process for removing SO2 in smoke from boiler of coking plant by utilizing residual coked ammonia water |
| CN103264991A (en) * | 2013-06-04 | 2013-08-28 | 枣庄德信环保技术有限公司 | Method for processing sulfur paste as coke oven gas desulfuration by-product |
| CN103264991B (en) * | 2013-06-04 | 2014-10-08 | 枣庄德信环保技术有限公司 | Method for processing sulfur paste as coke oven gas desulfuration by-product |
| WO2014194791A1 (en) * | 2013-06-04 | 2014-12-11 | 枣庄德信环保技术有限公司 | Method for processing sulphur paste as by-product from coke oven coal gas desulphuration |
| CN103820171B (en) * | 2014-03-12 | 2016-03-16 | 邯郸市裕泰燃气有限公司 | Gas desulfurizer |
| CN103820171A (en) * | 2014-03-12 | 2014-05-28 | 邯郸市裕泰燃气有限公司 | Coal gas desulfurization device |
| CN105985814A (en) * | 2015-02-09 | 2016-10-05 | 上海同特化工科技有限公司 | Treatment technology for removing hydrogen sulfide, hydrogen cyanide and ammonia in coal gas |
| CN105985814B (en) * | 2015-02-09 | 2019-02-01 | 上海同特化工科技有限公司 | The treatment process of hydrogen sulfide, hydrogen cyanide and ammonia is removed from coal gas |
| CN105238449A (en) * | 2015-09-29 | 2016-01-13 | 山东钢铁股份有限公司 | Desulfurization method of coke oven gas |
| CN105694988A (en) * | 2016-03-03 | 2016-06-22 | 金能科技股份有限公司 | Process for solving coal gas desulfuration liquid expansion in coking industry and system for process |
| CN106244249A (en) * | 2016-08-29 | 2016-12-21 | 中冶焦耐(大连)工程技术有限公司 | A kind of coke-oven-gas desulfurization and decyanation alkali wash section base extraction technique and device |
| CN108384582A (en) * | 2018-02-22 | 2018-08-10 | 中冶焦耐(大连)工程技术有限公司 | A kind of system and technique for strengthening deacidifion desorption |
| CN108384582B (en) * | 2018-02-22 | 2024-02-13 | 中冶焦耐(大连)工程技术有限公司 | System and process for strengthening deacidification, ammonia distillation and desorption |
| CN115196809A (en) * | 2022-08-04 | 2022-10-18 | 广西钢铁集团有限公司 | Method for removing hydrogen cyanide in rich solution by using pressurization type AS (acrylonitrile-styrene) desulfurization process in coking plant |
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