CN110655251A - Method for removing chloride ions in desulfurization slurry - Google Patents

Method for removing chloride ions in desulfurization slurry Download PDF

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CN110655251A
CN110655251A CN201910765125.6A CN201910765125A CN110655251A CN 110655251 A CN110655251 A CN 110655251A CN 201910765125 A CN201910765125 A CN 201910765125A CN 110655251 A CN110655251 A CN 110655251A
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dechlorination
desulfurization
cobalt
desulfurization slurry
ammonia
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CN110655251B (en
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李彦龙
李银丽
金忠
鲁兴武
王长征
李俞良
程亮
庞振业
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Northwest Research Institute of Mining and Metallurgy
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/727—Treatment of water, waste water, or sewage by oxidation using pure oxygen or oxygen rich gas
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/74—Treatment of water, waste water, or sewage by oxidation with air
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treating Waste Gases (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention relates to a method for removing chloride ions in desulfurization slurry, belonging to the field of coal-fired flue gas treatment, wherein chloride ions and ammonia ions in ammonia flue gas desulfurization slurry and cobalt ions in cobalt nitrate solution form hexaammine chloride cobalt precipitate under an alkaline condition, the precipitate forms chlorine-containing wastewater, ammonia gas and cobalt hydroxide after the processes of dissolution, boiling and the like, the chlorine-containing wastewater is treated by the wastewater and then discharged after reaching the standard, filtrate and ammonia gas are returned for desulfurization, and the cobalt hydroxide is dissolved by dilute nitric acid and then returned to the dechlorination process for continuous dechlorination. After the process is adopted for treatment, the content of chloride ions in the desulfurization slurry is reduced from more than 10g/L to less than 200mg/L, and cobalt nitrate and oxygen or air are adopted as a composite dechlorinating agent in the dechlorination process, so that the process has the advantages of low cost and high dechlorination efficiency.

Description

Method for removing chloride ions in desulfurization slurry
Technical Field
The invention belongs to the field of coal-fired flue gas treatment, relates to dechlorination treatment of ammonia-process desulfurization slurry, and particularly relates to a method for removing chloride ions in the desulfurization slurry.
Background
The ammonia desulfurization is a common method for coal-fired flue gas desulfurization treatment, and the method is characterized in that ammonia is used as an absorbent to absorb free sulfur dioxide in flue gas to form ammonium sulfate or ammonium sulfite which enters a desulfurization solution. Because the content of chlorine in the fire coal is too high or the content of chlorine in ammonia is higher, the desulfurization slurry contains a large amount of chlorine, and along with the circulation of the system, the chlorine is continuously accumulated in the desulfurization slurry, the concentration is increased, and along with the increase of the concentration of the chlorine, the corrosion rate of desulfurization system equipment is accelerated, thereby causing great threat to the stable operation of the system equipment.
In order to ensure that the desulfurization system can safely and efficiently operate, some enterprises reduce the chlorine content in the desulfurization ore pulp by adopting a stone washing mode, but the method can increase the discharge amount of wastewater and cause the increase of production cost. In addition, some manufacturers adopt ozone as an oxidant to oxidize chlorine in the desulfurization slurry into chlorine gas to be discharged into the atmosphere, and the chlorine gas is discharged into the air to cause environmental pollution, and the chlorine gas has toxicity and great potential safety hazard although the method solves the problem of high chlorine content in the solution. And in addition, part of enterprises adopt a abandoning method to perform dechlorination, part of desulfurized slurry is subjected to purification treatment, and a mixture of ammonium chloride and ammonium sulfate is formed after evaporation and concentration for discharge treatment. Therefore, the problem how to more effectively control the content of chloride ions in the desulfurization slurry is an urgent need to be solved while strictly controlling the discharge of the desulfurization wastewater.
Disclosure of Invention
The invention provides a method for removing chloride ions in desulfurization slurry aiming at ammonia desulfurization slurry, which can effectively reduce the content of chlorine in the desulfurization slurry, ensure that a desulfurization system operates safely and efficiently and reduce the discharge amount of wastewater.
The technical scheme adopted by the invention is as follows: a method for removing chloride ions in desulfurization slurry specifically comprises the following steps:
step (1), oxidation dechlorination: taking ammonia desulfurization slurry, and adding a composite dechlorinating agent cobalt nitrate solution and an oxidant into a reactor filled with the slurry to form hexaammine cobalt chloride precipitate;
step (2), filtering: carrying out filter pressing on the solution obtained in the step (1) for solid-liquid separation to obtain dechlorination solution and dechlorination slag, and feeding the dechlorination solution (the content of chloride ions is lower than 200 mg/L) back to an absorption tower for flue gas desulfurization;
and (3) boiling and dissolving dechlorination slag under micro pressure: dissolving the dechlorinated slag obtained in the step (2) by using dilute ammonia water with the concentration of 0.1-1.0mol/L, and boiling under the micro-pressure condition of 1.1-1.5 times of atmospheric pressure to obtain cobalt hydroxide, ammonia gas and chlorine-containing wastewater; wherein, cobalt hydroxide is dissolved by dilute nitric acid with the concentration of 0.1-1.0mol/L to form cobalt nitrate solution, the cobalt nitrate solution is returned to the reactor in the step (1) for dechlorination, ammonia gas is absorbed by the aqueous solution and then returned to the absorption tower for desulfurization, and chlorine-containing wastewater is discharged after reaching the standard after being sent to wastewater treatment.
Preferably, in the step (1), the ammonia desulfurization slurry is desulfurization slurry with the chloride ion content not less than 10g/L, the concentration of the cobalt nitrate solution is 1-10 mol/L, and the molar ratio of the cobalt ions in the cobalt nitrate solution to the chloride ions in the desulfurization slurry is more than 0.5.
Preferably, the oxidizing agent is hot sparged air or oxygen.
Compared with the prior art, the invention has the advantages that: the invention selects cobalt nitrate and oxygen or air as a composite dechlorinating agent to remove chloride ions of ammonia desulphurization slurry, the obtained dechlorinating solution directly returns to a desulphurization system for liquid preparation, the chlorine residue is subjected to the working procedures of dissolution, micro-pressure boiling and the like to obtain cobalt nitrate solution and chlorine-containing solution, the chlorine-containing solution is discharged after reaching the standard after being treated by waste water, and the cobalt nitrate is used as a dechlorinating agent raw material, which comprises the following steps:
1. oxidation dechlorination: taking the ammonia desulfurization slurry as a target solution, adding a cobalt nitrate solution into a dechlorination reactor filled with the desulfurization slurry, and simultaneously blowing oxygen (hot air) to form hexaammine cobalt trichloride. The reaction is as follows:
Co(NO3)2+2NH4Cl=2CoCl2+2NH4NO3
4CoCl2+4NH4Cl+20NH3+O2=4Co(NH3)6)Cl3+2H2O
the desulfurization slurry is dechlorinated by adopting a dechlorinating agent cobalt nitrate and an oxidant compressed air or oxygen to form a composite dechlorinating agent, so that the slurry is directly dechlorinated, the cost is low, and the dechlorinating efficiency is high.
2. The invention carries out solid-liquid separation on the solution containing hexaammine cobalt trichloride to obtain dechlorination liquid and dechlorination slag with the chloride ion content lower than 200mg/L, the dechlorination liquid directly returns to the desulfurization, the dechlorination slag is dissolved by dilute ammonia water and is boiled under the condition of micro pressure to obtain cobalt hydroxide, ammonia gas and chlorine-containing wastewater. Cobalt hydroxide is dissolved by dilute nitric acid and then returns to dechlorination, ammonia gas is directly sent to be desulfurized, and chlorine-containing wastewater is sent to be treated and then is discharged after reaching the standard:
the reaction is as follows: 2[ Co (NH)3)6]Cl3+6NH3·H2O=2Co(OH)3+12NH3+ 6NH4Cl；
Co(OH)3+3HNO3=Co(NO3)3+3H2O
After dechlorination slag is treated, ammonium chloride solution is sent to wastewater for treatment and then is discharged after reaching standards, ammonia gas and water are directly prepared into desulfurization solution to participate in desulfurization, cobalt hydroxide can return to a dechlorination system for dechlorination and dechlorination on one hand, and can be sold as a battery material on the other hand.
The method reduces the chloride ion content in the desulfurization slurry from more than 10g/L to less than 200mg/L, and the dechlorinating agent adopted in the dechlorinating process can be recycled.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and examples;
example 1
A method for removing chloride ions in desulfurization slurry specifically comprises the following steps:
dissolving desulfurized slurry with the chloride ion content of 10g/L and 1mol/L cobalt nitrate into a dechlorination reactor to be mixed according to the volume ratio of 1.5:1, and continuously blowing hot air into the reactor to carry out dechlorination reaction;
step (2), after the reaction is finished, carrying out solid-liquid separation to obtain dechlorination liquid and chlorine-containing slag, and sending the chlorine ion content of 183 mg/L in the dechlorination liquid back to the absorption tower for desulfurization;
dissolving the chlorine-containing residues by using dilute ammonia water with the concentration of 1.0mol/L, boiling in a micro-pressure reactor under the boiling pressure of 1.5 times of atmospheric pressure, releasing ammonia gas, absorbing the ammonia gas by using an aqueous solution, and returning the ammonia gas to an absorption tower for desulfurization; and carrying out solid-liquid separation to obtain a cobalt hydroxide solution and an ammonium chloride solution, sending the ammonium chloride solution to wastewater treatment and then discharging the solution after reaching the standard, mixing and dissolving the cobalt hydroxide and 0.1 mol/L dilute nitric acid to form a cobalt nitrate solution, and returning the cobalt nitrate solution to the dechlorination reactor to continue dechlorination.
Example 2
A method for removing chloride ions in desulfurization slurry specifically comprises the following steps:
mixing the desulfurization slurry with the chloride ion content of 15g/L and 2mol/L cobalt nitrate solution in a dechlorination reactor according to the volume ratio of 2:1, and continuously blowing hot air into the reactor to perform dechlorination.
And (2) after the reaction is finished, carrying out solid-liquid separation to obtain dechlorination liquid and chlorine-containing slag, and sending the dechlorination liquid with the chloride ion content of 179mg/L back to the absorption tower for desulfurization.
And (3) dissolving the chlorine-containing residues by using dilute ammonia water with the concentration of 0.5mol/L, boiling in a micro-pressure reactor under the boiling pressure of 0.1 time of atmospheric pressure, releasing ammonia gas, absorbing the ammonia gas by using an aqueous solution, and returning the ammonia gas to the absorption tower for desulfurization. And carrying out solid-liquid separation to obtain a cobalt hydroxide solution and an ammonium chloride solution, sending the ammonium chloride solution to wastewater treatment and then discharging the solution after reaching the standard, mixing and dissolving the cobalt hydroxide and 0.5mol/L dilute nitric acid to form a cobalt nitrate solution, and returning the cobalt nitrate solution to the dechlorination reactor to continue dechlorination.
Example 3
A method for removing chloride ions in desulfurization slurry specifically comprises the following steps:
mixing the desulfurization slurry with the chloride ion content of 20g/L and 10mol/L cobalt nitrate solution in a dechlorination reactor according to the volume ratio of 5:1, and continuously blowing hot oxygen into the reactor to perform dechlorination.
And (2) after the reaction is finished, carrying out solid-liquid separation to obtain dechlorination liquid and chlorine-containing slag, and sending the dechlorination liquid with the chloride ion content of 150mg/L back to the absorption tower for desulfurization.
And (3) dissolving the chlorine-containing residues by using dilute ammonia water with the concentration of 1.0mol/L, boiling in a micro-pressure reactor under the boiling pressure of 1.1 times of atmospheric pressure, releasing ammonia gas, absorbing the ammonia gas by using an aqueous solution, and returning the ammonia gas to the absorption tower for desulfurization. And carrying out solid-liquid separation to obtain a cobalt hydroxide solution and an ammonium chloride solution, sending the ammonium chloride solution to wastewater treatment and then discharging the solution after reaching the standard, mixing and dissolving the cobalt hydroxide and 1.0mol/L dilute nitric acid to form a cobalt nitrate solution, and returning the cobalt nitrate solution to the dechlorination reactor to continue dechlorination.

Claims (3)

1. A method for removing chloride ions in desulfurization slurry is characterized by comprising the following steps: the method specifically comprises the following steps:
step (1), oxidation dechlorination: taking ammonia desulfurization slurry, and adding a composite dechlorinating agent cobalt nitrate solution and an oxidant into a reactor filled with the slurry to form hexaammine cobalt chloride precipitate;
step (2), filtering: carrying out filter pressing on the solution obtained in the step (1) for solid-liquid separation to obtain dechlorination solution and dechlorination slag, and feeding the dechlorination solution back to the absorption tower for flue gas desulfurization;
and (3) boiling and dissolving dechlorination slag under micro pressure: dissolving the dechlorinated slag obtained in the step (2) by using dilute ammonia water with the concentration of 0.1-1.0mol/L, and boiling under the micro-pressure condition of 1.1-1.5 times of atmospheric pressure to obtain cobalt hydroxide, ammonia gas and chlorine-containing wastewater; and (2) dissolving cobalt hydroxide by using dilute nitric acid with the concentration of 0.1-1.0mol/L to form a cobalt nitrate solution, returning to the reactor in the step (1) for continuous dechlorination, absorbing ammonia gas by using an aqueous solution, returning to an absorption tower for desulfurization, and delivering chlorine-containing wastewater to treat the wastewater to reach the standard and then discharging the wastewater.
2. The method for removing chloride ions from desulfurization slurry according to claim 1, wherein: in the step (1), the ammonia desulfurization slurry is the desulfurization slurry with the chloride ion content not lower than 10g/L, and the concentration of the cobalt nitrate solution is 1-10 mol/L.
3. The method for removing chloride ions from desulfurization slurry according to claim 1 or 2, wherein: the oxidant is hot bubbling air or oxygen.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111137964A (en) * 2020-01-14 2020-05-12 福建永荣科技有限公司 Coal-fired boiler ammonia desulfurization slurry dechlorination treatment process
CN117049718A (en) * 2023-06-28 2023-11-14 北京清新环境技术股份有限公司 Method for removing chloride ions from desulfurization slurry

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CN109647152A (en) * 2019-01-29 2019-04-19 中南大学 A kind of purification method and its purification device containing chlorine or/and sulphur-containing exhaust gas

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CA2699572A1 (en) * 2007-09-20 2009-03-26 Skyonic Corporation Removing carbon dioxide from waste streams through co-generation of carbonate and/or bicarbonate minerals
CN102423613A (en) * 2011-08-23 2012-04-25 武汉兴能环保技术有限公司 Ammonia desulfurization method for effectively removing chlorine and fluorine ions and heavy metal ions
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111137964A (en) * 2020-01-14 2020-05-12 福建永荣科技有限公司 Coal-fired boiler ammonia desulfurization slurry dechlorination treatment process
CN117049718A (en) * 2023-06-28 2023-11-14 北京清新环境技术股份有限公司 Method for removing chloride ions from desulfurization slurry
CN117049718B (en) * 2023-06-28 2024-04-09 北京清新环境技术股份有限公司 Method for removing chloride ions from desulfurization slurry

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