CN110054201A - A kind of technique that remained ammonia depickling production purification ammonium hydroxide realizes heat coupling simultaneously - Google Patents

A kind of technique that remained ammonia depickling production purification ammonium hydroxide realizes heat coupling simultaneously Download PDF

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Publication number
CN110054201A
CN110054201A CN201910300066.5A CN201910300066A CN110054201A CN 110054201 A CN110054201 A CN 110054201A CN 201910300066 A CN201910300066 A CN 201910300066A CN 110054201 A CN110054201 A CN 110054201A
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ammonia
tower
ammonium hydroxide
remained
heat
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CN201910300066.5A
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CN110054201B (en
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李昊阳
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Acre Coking and Refractory Engineering Consulting Corp MCC
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Acre Coking and Refractory Engineering Consulting Corp MCC
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/10Separation of ammonia from ammonia liquors, e.g. gas liquors

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Water Treatments (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to a kind of remained ammonia depicklings to produce the technique that purification ammonium hydroxide realizes heat coupling simultaneously, remained ammonia exchanges heat with distilled ammonia wastewater and enters extracting tower after mixing with acid solution, free ammonia in remained ammonia becomes fixed ammonia, for acid gas by escaping at the top of extracting tower, a part of ammonium hydroxide after removing acid gas, which mixes to enter from the top of ammonia still with lye, carries out ammonia still process processing;Another part ammonium hydroxide enters the condenser of ammonia still process tower top, and depickling tower bottom is returned after heating and carries out heat supply to extracting tower;Fixed ammonia under the action of lye in ammonium hydroxide becomes free ammonia, and ammonia escapes at the top of ammonia still, becomes ammonolysis product after condenser is concentrated.The present invention inhibits ammonia evolution, effectively recycling ammonolysis product by carrying out acid adding operation in extracting tower;It is higher than extracting tower column bottom temperature by control ammonia still process column overhead temperatures, makes the condenser of ammonia still process column overhead while completing that ammonia is concentrated, additionally it is possible to is desulfurizing tower heat supply, reduce technique entirety energy consumption in such a way that heat couples.

Description

A kind of technique that remained ammonia depickling production purification ammonium hydroxide realizes heat coupling simultaneously
Technical field
The present invention relates to coke oven gas purification and recovering ammonia technique field more particularly to a kind of remained ammonia depickling production essences The technique that ammonium hydroxide processed realizes heat coupling simultaneously.
Background technique
During coke oven production, condensate liquid and circulation ammonia of the raw coke oven gas after cyclic ammonia water sprinkling is cooling, in raw coke oven gas Water mixes, and wherein most is recycled as cyclic ammonia water, and remainder is sent to ammonia still process workshop section as remained ammonia, Ammonia distillation is carried out after filtering out oil.Contain a certain amount of free ammonia and fixed ammonia and a small amount of cyaniding in remained ammonia Hydrogen, hydrogen sulfide and carbon dioxide, existing remained ammonia treatment process is by adding alkali in rational position, by acidic components and ammonia one It rises and distills out, the distilled ammonia wastewater of tower bottom enters sewage treatment plant and carries out purified treatment, but contains one in the ammonia product of tower top Quantitative hydrogen cyanide, hydrogen sulfide and carbon dioxide.With the increasingly strict of ring national requirements for environmental protection, flue gas desulfurization and denitration technique becomes Conventional process, the demand of ammonolysis product also gradually increase therewith, but contain acidity in the ammonia product as made from remained ammonia It forms on the high side, significantly limits the application of this kind of ammonolysis product.In addition, often to be expended during remained ammonia deacidifion big The energy is measured, greatly affected social benefit and Business Economic Benefit.
Summary of the invention
The present invention provides a kind of remained ammonia depickling produce purification ammonium hydroxide simultaneously realize heat coupling technique, by Extracting tower carries out acid adding operation, and the substep of hydrogen sulfide and ammonia is completed in existing form, inhibition ammonia evolution to transformation ammonia in the liquid phase Desorption, effectively recycling ammonolysis product;It is higher than extracting tower column bottom temperature by control ammonia still process column overhead temperatures, makes the cold of ammonia still process column overhead Condenser is while completing that ammonia is concentrated, additionally it is possible to be desulfurizing tower heat supply, reduce technique entirety energy in such a way that heat couples Consumption.
In order to achieve the above object, the present invention is implemented with the following technical solutions:
A kind of remained ammonia depickling production purification ammonium hydroxide realizes the technique of heat coupling simultaneously, includes the following steps:
1) by condensation air blast workshop section Lai remained ammonia and distilled ammonia wastewater exchange heat through heat exchanger, then after being mixed with acid solution At the top of into extracting tower;
2) depickling tower bottom carries out heat supply by the condenser of ammonia still process tower top, due to the addition of acid solution, so that remaining ammonia Free ammonia in water becomes fixed ammonia, so that ammonia be inhibited to escape;Acid gas is sent to desulfurization workshop section upstream by evolution at the top of extracting tower Raw coke oven gas pipeline;
3) the extracting tower bottom liquid phase after removing acid gas is ammonium hydroxide, and after aqua ammonia pump is pressurized, a part of ammonium hydroxide and lye are mixed It closes to enter from the top of ammonia still and carries out ammonia still process processing;Another part ammonium hydroxide enters the condenser of ammonia still process tower top, returns after heating Depickling tower bottom carries out heat supply to extracting tower;
4) operating pressure is 0.15Mpa (a)~1Mpa (a) at the top of the ammonia still, and ammonia still top pressure is greater than depickling Tower bottom pressure;For ammonia still process tower bottom by heat supply, fixed ammonia under the action of lye in ammonium hydroxide becomes free ammonia, ammonia It is escaped at the top of from ammonia still, and the condenser for entering tower top carries out concentration;
5) the gas phase evolution after condenser is concentrated becomes ammonolysis product, and liquid phase returns to ammonia still as reflux;
6) ammonia still tower bottom discharge distilled ammonia wastewater is sent outside after heat exchanger and remained ammonia heat exchange to sewage treatment plant.
The acid solution is added in residual ammonia water pipeline before remained ammonia enters extracting tower, or in extracting tower Top and remained ammonia enter extracting tower simultaneously.
The lye is added in ammonia water pipeline before extracting tower tower bottom ammonium hydroxide enters ammonia still ammonia still process, or in ammonia still Top and ammonium hydroxide enter ammonia still simultaneously.
Steam of the heat source of the ammonia still process tower bottom from ammonia still process tower reboiler or external steam pipeline.
Compared with prior art, the beneficial effects of the present invention are:
1) by carrying out acid adding operation in extracting tower, transformation ammonia in the liquid phase complete by existing form, inhibition ammonia evolution The desorption of the substep of hydrogen sulfide and ammonia, effectively recycling ammonolysis product;
2) by improving ammonia still tower top pressure, so that ammonia still process column overhead temperatures are higher than extracting tower column bottom temperature, ammonia still The condenser of tower top also carries out heat supply to desulfurizing tower as the reboiler of desulfurizing tower while ammonia is concentrated;
3) in such a way that heat couples, technique entirety energy consumption is reduced;
4) extracting tower no setting is required reboiler, area needed for ammonia still tower bottom reboiler are reduced.
Detailed description of the invention
Fig. 1 is a kind of remained ammonia depickling production purification ammonium hydroxide of the present invention while the stream for realizing the technique that heat couples Cheng Tu.
In figure: 1. extracting tower, 2. heat exchanger, 3. ammonia still, 4. aqua ammonia pump, 5. distilled ammonia wastewater pumps 6. condenser, 7. ammonia still process Tower reboiler
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing:
As shown in Figure 1, a kind of remained ammonia depickling production purification ammonium hydroxide of the present invention realizes the work of heat coupling simultaneously Skill includes the following steps:
1) by condensation air blast workshop section Lai remained ammonia and distilled ammonia wastewater exchange heat through heat exchanger 2, then mixed with acid solution Enter 1 top of extracting tower afterwards;
2) 1 bottom of extracting tower by 3 tower top of ammonia still 6 heat supply of condenser, due to the addition of acid solution, so that remaining ammonia Free ammonia in water becomes fixed ammonia, so that ammonia be inhibited to escape;Acid gas is sent to desulfurization workshop section upstream by escaping at the top of extracting tower 1 Raw coke oven gas pipeline;
3) the extracting tower bottom liquid phase after removing acid gas is ammonium hydroxide, and after the pressurization of aqua ammonia pump 4, a part of ammonium hydroxide and lye are mixed It closes to enter from the top of ammonia still 3 and carries out ammonia still process processing;Another part ammonium hydroxide enters the condenser 6 on the top of ammonia still 3, returns after heating 1 bottom of acid tower carries out heat supply to extracting tower 1 back off;
4) the 3 top operating pressure of ammonia still is 0.15Mpa (a)~1Mpa (a), and 3 top pressure of ammonia still is greater than de- 1 base pressure of acid tower;For 3 bottom of ammonia still by heat supply, fixed ammonia under the action of lye in ammonium hydroxide becomes free ammonia, Ammonia escapes at the top of ammonia still 3, and the condenser 6 for entering tower top carries out concentration;
5) the gas phase evolution after the concentration of condenser 6 becomes ammonolysis product, and liquid phase returns to ammonia still 3 as reflux;
6) 3 tower bottom of ammonia still discharge distilled ammonia wastewater is sent outside after heat exchanger 2 and remained ammonia heat exchange to sewage treatment work Section.
The acid solution is added in residual ammonia water pipeline before remained ammonia enters extracting tower 1, or in depickling Top of tower and remained ammonia enter extracting tower 1 simultaneously.
The lye is added in ammonia water pipeline before 1 tower bottom ammonium hydroxide of extracting tower enters 3 ammonia still process of ammonia still, or in ammonia still process Top of tower and ammonium hydroxide enter ammonia still 3 simultaneously.
Steam of the heat source from ammonia still process tower reboiler 7 or external steam pipeline of 3 bottom of ammonia still.
A kind of remained ammonia depickling production purification ammonium hydroxide of the present invention realizes the emphasis behaviour of the technique of heat coupling simultaneously It is as step, first is that acid solution is added in remained ammonia before remained ammonia depickling, second is that in extracting tower tower bottom ammonia Before water ammonia still process, lye is added in ammonium hydroxide.
A kind of concrete composition mode of system of technique of the present invention is that by shown in Fig. 1, which includes de- Acid tower 1, ammonia still 3, condenser 6, ammonia still process tower reboiler 7, heat exchanger 2, aqua ammonia pump 4 and distilled ammonia wastewater pump 5.1 top of extracting tower Equipped with acid gas outlet, remained ammonia and acid solution entry to mixed solution, lower part sets liquid phase return port, and bottom sets ammonium hydroxide discharge Mouthful;Wherein, the remained ammonia of extracting tower 1 and acid solution entry to mixed solution pass through the first of mixed liquor pipeline connection heat exchanger 2 Heat transferring medium outlet, and set acid solution inlet on this section of mixed liquor pipeline and be connected with acid solution conveyance conduit;Heat exchanger 2 First heat transferring medium entrance connects remained ammonia conveyance conduit;The second heat transferring medium entrance connection distilled ammonia wastewater pump 5 of heat exchanger 2 Outlet, the entrance of distilled ammonia wastewater pump 5 is connected by distilled ammonia wastewater pipeline with the distilled ammonia wastewater outlet at ammonia still bottom, heat exchanger 2 the second heat transferring medium outlet connection distilled ammonia wastewater conveyance conduit.
The top of ammonia still 3 is equipped with ammonia outlet, and top sets ammonia inlet and phegma entrance, and lower part is equipped with ammonia still process Tower reboiler 7, bottom set distilled ammonia wastewater outlet;Wherein, the entrance of distilled ammonia wastewater outlet and distilled ammonia wastewater pump 5 passes through ammonia still process Waste pipe connection;The ammonium hydroxide outlet of 1 bottom of extracting tower is connect by ammonia water pipeline with the entrance of aqua ammonia pump 4, aqua ammonia pump 4 Outlet is separately connected the ammonia inlet of ammonia still 3 and the first heat transferring medium entrance of condenser 6, ammonia still 3 by ammonia water pipeline Alkali liquor inlet connection lye conveyance conduit is set in preceding ammonia water pipeline;The first heat transferring medium outlet connection extracting tower 1 of condenser 6 The liquid phase return port of lower part.The ammonia outlet of ammonia still 3 passes through the second heat transferring medium entrance of ammonia pipeline and condenser 6 Connection, the second heat transferring medium outlet connection ammonia product pipeline of condenser 6.The condensate outlet of condenser 6 passes through condensate liquid Pipeline connects the phegma entrance at 3 top of ammonia still.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (4)

1. a kind of technique that remained ammonia depickling production purification ammonium hydroxide realizes heat coupling simultaneously, which is characterized in that including as follows Step:
1) by condensation air blast workshop section Lai remained ammonia and distilled ammonia wastewater exchange heat through heat exchanger, then enter after being mixed with acid solution At the top of extracting tower;
2) depickling tower bottom carries out heat supply by the condenser of ammonia still process tower top, due to the addition of acid solution, so that in remained ammonia Free ammonia become fixed ammonia, so that ammonia be inhibited to escape;Acid gas is sent to the famine of desulfurization workshop section upstream by evolution at the top of extracting tower Gas piping;
3) the extracting tower bottom liquid phase after removing acid gas is ammonium hydroxide, and after aqua ammonia pump is pressurized, a part of ammonium hydroxide mixes certainly with lye Enter at the top of ammonia still and carries out ammonia still process processing;Another part ammonium hydroxide enters the condenser of ammonia still process tower top, returns to depickling after heating Tower bottom carries out heat supply to extracting tower;
4) operating pressure is 0.15Mpa (a)~1Mpa (a) at the top of the ammonia still, and ammonia still top pressure is greater than extracting tower bottom Portion's pressure;For ammonia still process tower bottom by heat supply, fixed ammonia under the action of lye in ammonium hydroxide becomes free ammonia, and ammonia is from steaming The evolution of ammonia top of tower, and the condenser for entering tower top carries out concentration;
5) the gas phase evolution after condenser is concentrated becomes ammonolysis product, and liquid phase returns to ammonia still as reflux;
6) ammonia still tower bottom discharge distilled ammonia wastewater is sent outside after heat exchanger and remained ammonia heat exchange to sewage treatment plant.
2. a kind of remained ammonia depickling production purification ammonium hydroxide according to claim 1 realizes the technique of heat coupling simultaneously, It is characterized in that, the acid solution is added in residual ammonia water pipeline before remained ammonia enters extracting tower, or de- Enter extracting tower simultaneously with remained ammonia at the top of acid tower.
3. a kind of remained ammonia depickling production purification ammonium hydroxide according to claim 1 realizes the technique of heat coupling simultaneously, It is characterized in that, the lye is added in ammonia water pipeline before extracting tower tower bottom ammonium hydroxide enters ammonia still ammonia still process, or steaming Ammonia top of tower and ammonium hydroxide enter ammonia still simultaneously.
4. a kind of remained ammonia depickling production purification ammonium hydroxide according to claim 1 realizes the technique of heat coupling simultaneously, It is characterized in that, steam of the heat source of the ammonia still process tower bottom from ammonia still process tower reboiler or external steam pipeline.
CN201910300066.5A 2019-04-15 2019-04-15 Process for producing refined ammonia water by deacidifying residual ammonia water and simultaneously realizing heat coupling Active CN110054201B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112023651A (en) * 2020-09-08 2020-12-04 四川省达州钢铁集团有限责任公司 Method and system for desulfurization and denitrification of coke oven flue gas by using residual ammonia water
CN112551793A (en) * 2020-12-10 2021-03-26 天津大学 Ammonia distillation method and device for ammonia-containing wastewater
CN114212850A (en) * 2021-12-27 2022-03-22 中冶焦耐(大连)工程技术有限公司 High-efficiency energy-saving thermal coupling ammonia distillation process

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4240808A (en) * 1977-10-03 1980-12-23 Metallgesellschaft Aktiengesellschaft Processing aqueous effluent liquors from degasification or gasification of coal
CN101717096A (en) * 2009-12-29 2010-06-02 中钢集团天澄环保科技股份有限公司 Technology for preparing desulfurizing agent ammonia water in sintering flue gas desulfurization by coking residual ammonia water

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4240808A (en) * 1977-10-03 1980-12-23 Metallgesellschaft Aktiengesellschaft Processing aqueous effluent liquors from degasification or gasification of coal
CN101717096A (en) * 2009-12-29 2010-06-02 中钢集团天澄环保科技股份有限公司 Technology for preparing desulfurizing agent ammonia water in sintering flue gas desulfurization by coking residual ammonia water

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112023651A (en) * 2020-09-08 2020-12-04 四川省达州钢铁集团有限责任公司 Method and system for desulfurization and denitrification of coke oven flue gas by using residual ammonia water
CN112551793A (en) * 2020-12-10 2021-03-26 天津大学 Ammonia distillation method and device for ammonia-containing wastewater
CN114212850A (en) * 2021-12-27 2022-03-22 中冶焦耐(大连)工程技术有限公司 High-efficiency energy-saving thermal coupling ammonia distillation process
CN114212850B (en) * 2021-12-27 2024-04-26 中冶焦耐(大连)工程技术有限公司 Efficient energy-saving type thermal coupling ammonia distillation process

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