CN106086474A - A kind of method recycling magnesium from heavy metal sewage sludge - Google Patents
A kind of method recycling magnesium from heavy metal sewage sludge Download PDFInfo
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- CN106086474A CN106086474A CN201610757415.2A CN201610757415A CN106086474A CN 106086474 A CN106086474 A CN 106086474A CN 201610757415 A CN201610757415 A CN 201610757415A CN 106086474 A CN106086474 A CN 106086474A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The present invention provides a kind of method recycling magnesium from heavy metal sewage sludge, comprise the following steps: 1) heavy metal sewage sludge is mixed by a certain percentage with pure water, pH is to alkalescence in regulation, filtrate 1 it is dehydrated to obtain through filter press, filtering residue hot wash filtering means dehydration obtains filtrate 2, and filtrate 1 is 2-in-1 with filtrate and is magnesium liquid;2) taking gained magnesium liquid in a certain amount of step 1, add AR level ammonia magnesium sinking by the consumption of excess coefficient 3 ~ 8 times, fully reaction obtains magnesium hydrate precipitate;3) in step 2 products therefrom, surface modifier dodecylbenzene sodium sulfonate modified magnesium hydroxide is added;4) products therefrom in step 3 is first warming up to after 85 90 DEG C of constant temperature process 3 5h, then at 65 80 DEG C, is aged 2 6h, obtain slag specimen;5) by the dehydration of step 4 gained slag specimen vacuum pump sucking filtration, hot water and ethanol is used to replace washing, after drying, prepare the thick product of Flame Retardant Magnesium Hydroxide at 100 105 DEG C.In process of the present invention, while ensureing noble metal retrieving cobalt nickel rate and product purity, improve the primary recovery of magnesium.
Description
Technical field
The invention belongs to resource circulation utilization and technical field of wet metallurgy, more specifically to a kind of after extraction
The method of separation and recovery preparation Flame Retardant Magnesium Hydroxide in heavy metal sewage sludge.
Background technology
Industrial production magnesium hydroxide mainly has following five kinds of methods: (1) produces hydroxide with limestone and salt reaction
Magnesium;(2) with sodium hydroxide and salt, enriched bittern cake reaction hydrogen manufacturing magnesium oxide;(3) utilize burnt magnesite, dolomite and salt,
Enriched bittern cake reaction produces magnesium hydroxide;(4) utilizing MgO hydration to generate magnesium hydroxide, MgO here must be that light-burned product is to ensure
The activity of hydration;(5) with ammonia and salt, enriched bittern cake reaction hydrogen manufacturing magnesium oxide.Later stage uses surface modifier to change magnesium hydroxide
Property, use crystal seed method, the traditional method such as hydro-thermal method to prepare the flame retardant of magnesium hydroxide product meeting fire resistance.Industrial production
The raw material sources of magnesium hydroxide are extensive, but the easy etching apparatus of salt thus higher to equipment requirements, magnesite and dolomite
Calcination process energy consumption is high, and therefore conventional method prepares magnesium hydroxide industrial production magnesium hydroxide mainly following five kinds of methods:
(1) magnesium hydroxide is produced with limestone and salt reaction;(2) with sodium hydroxide and salt, enriched bittern cake reaction hydrogen manufacturing magnesium oxide;(3)
Burnt magnesite, dolomite and salt, enriched bittern cake reaction is utilized to produce magnesium hydroxide;(4) MgO hydration is utilized to generate hydroxide
Magnesium, MgO here must be that light-burned product is to ensure the activity of hydration;(5) with ammonia and salt, enriched bittern cake reaction hydrogen manufacturing oxidation
Magnesium.The traditional methods such as the later stage uses surface modifier modified to magnesium hydroxide, uses crystal seed method, hydro-thermal method prepare and meet anti-flammability
The flame retardant of magnesium hydroxide product of energy.The raw material sources of industrial production magnesium hydroxide are extensive, but the easy etching apparatus of salt because of
And higher to equipment requirements, the calcination process energy consumption of magnesite and dolomite is high, and therefore conventional method prepares magnesium hydroxide flame retardant
It is high to there is equipment requirements in agent, the shortcoming that energy consumption is high.
The magnesium that the lateritic nickel ore used in extraction cobalt nickel industry contains mass fraction about 20%, produces 1t metallic cobalt nickel,
The mud of association about 55t, magnesium is enriched in mud and does not obtain Appropriate application.Rich in valuable metals such as cobalt nickel manganese magnesium in mud,
Present stage, in order to acidleach, recycles the noble metals (material liquid prepared as ternary battery material) such as cobalt nickel manganese, acidleach process
A large amount of magnesium resources of middle generation are enriched in system circulation, magnesium the most suitably open a way (make product or outward row) therefore process
Difficulty.Owing to lacking the suitable processing method to magnesium resource, cause serious environmental pressure with the wasting of resources.
To sum up, at present to the heavy metal sewage sludge after extraction in processing procedure, there is substantial amounts of magnesium in leachate and be difficult to point
From, low as purity such as ternary battery raw material cobalt nickel manganese, in leachate, a large amount of magnesium resources cannot cause magnesium resource wave by Appropriate application
The problem taken.It is high to there is equipment requirements in fire retardant, the shortcoming that energy consumption is high.
Summary of the invention
In order to solve above-mentioned technical problem, it is an object of the invention to provide a kind of recycling magnesium from heavy metal sewage sludge
Method, by this method to extraction cobalt nickel industry in extraction after heavy metal sewage sludge (hereinafter referred to as heavy metal sewage sludge) carry out
Process, can not only shorten from heavy metal sewage sludge, reclaim cobalt nickel in magnesium, the utilization rate of raising magnesium, simultaneously guarantee heavy metal sewage sludge
Etc. having the response rate of valency noble metal subsequent treatment and higher purity to improve industry added value, and simple for process, can
Extensive industrialization.
A kind of method recycling magnesium from heavy metal sewage sludge, comprises the following steps:
Step 1, pretreatment is washed: than 8:1 ~ 15:1, heavy metal sewage sludge is added pure water with mud dry biomass according to pure water,
Heat while stirring, be heated to 80 ~ 85 DEG C and be incubated, during heated and stirred, add the dilute sulfuric acid of 0.4g/L ~ 0.6g/L
Until recording pH at 80 ~ 85 DEG C is 7.0 ~ 8.0, continue stirring 10 ~ 15min, obtain grain slag mixture and be dehydrated through filter press, obtain filter
Liquid 1 and filtering residue 1;Filtering residue 1 is used hot wash filtering means dehydration 1 ~ 3 time, obtains filtrate 2;Filtrate 1 is 2-in-1 with filtrate and gained filtrate is
For magnesium liquid;
Step 2, adds alkali liquor magnesium sinking: take gained magnesium liquid in the step 1 of certain volume, measures magnesium ion concentration in magnesium liquid, by excess
The consumption of coefficient 3 ~ 8 times multiple of ammonia theoretical value consumption (magnesium sinking need) adds AR level ammonia and reacts 30-at 30-40 DEG C
40min magnesium sinking, i.e. magnesium ion are combined formation magnesium hydrate precipitate with hydroxide ion;
Step 3, surface modification: the dodecylbenzene sodium sulfonate adding mass fraction 10-15% in step 2 products therefrom is water-soluble
Liquid 5-15mL, as surface modifier, reacts 30-40min modified magnesium hydroxide at 30-40 DEG C;
Step 4, ageing: after products therefrom in step 3 is first warming up to 85-90 DEG C of constant temperature process 3-5h older at 65-80 DEG C
Change 2-6h, obtain slag specimen;
Step 5, by the vacuum pump sucking filtration dehydration of step 4 gained slag specimen, uses the alternately washing of hot water and ethanol, at 100-105 DEG C
The thick product of Flame Retardant Magnesium Hydroxide is prepared after lower drying.
As preferably, in step 1, heavy metal sewage sludge is added pure water with mud dry biomass than 15:1 according to pure water,
Heat while stirring, be heated to 85 DEG C and be incubated, during heated and stirred, add the dilute sulfuric acid of 0.6g/L until 85 DEG C of surveys
Obtaining pH is 8.0, continues stirring 15min, obtains grain slag mixture and is dehydrated through filter press, obtains filtrate 1 and filtering residue 1;By filtering residue 1 heat
Water washing filtering means dehydration 3 times, obtains filtrate 2;Filtrate 1 is 2-in-1 with filtrate and gained filtrate is magnesium liquid.
As preferably, in step 2, in magnesium liquid, add AR level ammonia according to the consumption of excess coefficient 5 times.
As preferably, in step 2, in described magnesium liquid, magnesium ion concentration is by Japan Shimadzu atomic absorption spectrophotometer AA-
7000 record.
Beneficial effects of the present invention:
1) heavy metal sewage sludge passes through pretreatment water-washing process, and wherein most magnesium enter magnesium liquid after washing out, and in magnesium liquid, magnesium accounts for weight
In metal sludge, the ratio of magnesium reaches more than 99%;Meanwhile, in filtrate, the content of Ni is less than 0.6mg/L, and Co, Mn, Zn do not detect,
The content of Cu is less than 0.2mg/L, thus ensure that the high-recovery of noble metal cobalt nickel in the filtering residue of recovery.2) hydrogen prepared
The thick product of magnesium oxide fire retardant: in product, the primary recovery (product magnesium accounts for the ratio of magnesium in heavy metal sewage sludge) of magnesium reaches
More than 86.9%, reach as high as 90.2%;Product purity >=96.7%, specific surface area (BET)≤17.6m/g, 101 microcosmic planted agents
Become η≤2.9x10-3;SEM result shows that magnesium hydroxide particle is hexagonal flake, has well-regulated pattern, it is simple to as fire retardant
Easily disperse during interpolation.
3) synthetical recovery of valuable metal magnesium in heavy metal sewage sludge is effectively achieved, it is to avoid existing recovery process exists
Magnesium circulates in system, the deficiency of suitable open circuit is (with the cobalt nickel manganese together conduct leached in magnesium leachate after acidleach
Material liquid, the recycling to cobalt nickel manganese interferes);
4) recycled in its entirety rational technology is easy, efficiency is high, has considerable economic worth.
Accompanying drawing explanation
Fig. 1 is the technique course diagram of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of method recycling magnesium from heavy metal sewage sludge, comprises the following steps:
1. pretreatment washing: heavy metal sewage sludge is added pure water with mud dry biomass than 8:1 according to pure water, opens electric furnace liter
Temperature, finally stable at 80 DEG C by dilute sulfuric acid aqueous solution regulation pH to the 7.0(temperature of 0.4g/L while stirring, pH=7.0 is at this
At a temperature of record), continue stirring 10min, obtain grain slag mixture through filter press be dehydrated, obtain filtrate 1 and filtering residue 1;Filtering residue 1 is used
80-90 DEG C of hot wash filtering means dehydration 1 time, obtains filtrate 2.Filtrate 1 is 2-in-1 with filtrate and gained filtrate is magnesium liquid.Magnesium in magnesium liquid
The ratio of magnesium in heavy metal sewage sludge that accounts for reaches more than 99%, and the content of Ni is 0.5mg/L, and Co, Mn, Zn do not detect, and the content of Cu is
0.1mg/L, Na, Ca, although but Cl-content is higher harmless to preparing magnesium hydroxide.
2. add alkali liquor magnesium sinking: take gained magnesium liquid 2000ml in step 1, use Japan's Shimadzu atomic absorption spectrophotometer
AA-7000 measures magnesium ion concentration in magnesium liquid, according to the use of the excess coefficient 3 times multiple of ammonia theoretical value consumption (magnesium sinking need)
Amount adds AR level ammonia regulation pH value in 2000mL magnesium liquid, reacts 30-40min magnesium sinking, i.e. magnesium ion and hydrogen at 30-40 DEG C
Oxygen radical ion combines and forms magnesium hydrate precipitate.
3. surface modification: add the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 15% in step 2 products therefrom
5mL, as surface modifier, reacts 30min modified magnesium hydroxide at 30 DEG C;
4. ageing: products therefrom in step 3 is first warming up to 90 DEG C of constant temperature and processes 3h, then be aged 2h at 65 DEG C, make generation
Magnesium hydroxide particle further growth, to reach to meet the standard of preparation Flame Retardant Magnesium Hydroxide, obtains slag specimen.
5. step 4 gained slag specimen vacuum pump sucking filtration is dehydrated, uses the alternately washing of hot water and ethanol, at 100-105 DEG C
The prepared thick product of Flame Retardant Magnesium Hydroxide after drying under (have only to dry moisture to constant weight, therefore temperature is without the highest).
Flame Retardant Magnesium Hydroxide needs to meet 3 points (reference standard HGT 4531-2013 magnesium hydroxide for fire retardant): produce
Product purity >=93.0%, specific surface area (BET)≤20.0m/g, 101 microcosmic internal strain η≤3.0x10-3;Additionally need to produce
Product magnesium hydroxide particle has well-regulated pattern, it is simple to easily disperse when adding as fire retardant.
In the present embodiment, the response rate (product magnesium accounts for the ratio of magnesium in heavy metal sewage sludge) of magnesium can reach 86.9%, product
Purity can reach 96.9%(and be recorded by the U.S.'s graceful ICP-OES Inductively coupled plasma optical emission spectrometer of profit), particle diameter is distributed in
Between 0.8-9.2 μm, mean diameter 6.32 μm (is recorded by Malvern 2000 laser particle analyzer), and BET result is that 17.6m/g(is beautiful
State NOVA full-automatic N2 adsorption specific surface tester records), SEM result shows that granule is that hexagonal flake (is surveyed by U.S.'s FEI Electronic Speculum
), 101 microcosmic internal strains η: 2.9x10-3(full-automatic X-ray diffractometer D/max-IIIA records), below to the equipment of measurement
Do not repeat.
Embodiment 2
A kind of method recycling magnesium from heavy metal sewage sludge, comprises the following steps:
1. pretreatment washing: heavy metal sewage sludge is added pure water with mud dry biomass than 15:1 according to pure water, opens electric furnace liter
Temperature, finally stable at 85 DEG C by dilute sulfuric acid aqueous solution regulation pH to the 8.0(temperature of 0.6g/L while stirring, pH=8.0 is at this
At a temperature of record), continue stirring 15min, obtain grain slag mixture through filter press be dehydrated, obtain filtrate 1 and filtering residue 1;Filtering residue 1 is used
80-90 DEG C of hot wash filtering means dehydration 3 times, obtains filtrate 2.Filtrate 1 is 2-in-1 with filtrate and gained filtrate is magnesium liquid.Magnesium in magnesium liquid
The ratio of magnesium in heavy metal sewage sludge that accounts for reaches more than 99%, and the content of Ni is 0.6mg/L, and Co, Mn, Zn do not detect, the content of Cu
0.2mg/L, Na, Ca, although but Cl-content is higher harmless to preparing magnesium hydroxide.
2. add alkali liquor magnesium sinking: take gained magnesium liquid 2000ml in step 1, use Japan's Shimadzu atomic absorption spectrophotometer
AA-7000 measures magnesium ion concentration in magnesium liquid, according to the use of the excess coefficient 5 times multiple of ammonia theoretical value consumption (magnesium sinking need)
Amount adds AR level ammonia regulation pH value in 2000mL magnesium liquid, reacts 30-40min magnesium sinking, i.e. magnesium ion and hydrogen at 30-40 DEG C
Oxygen radical ion combines and forms magnesium hydrate precipitate.
3. surface modification: add the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 10% in step 2 products therefrom
10mL, as surface modifier, reacts 40min modified magnesium hydroxide at 40 DEG C.
4. ageing: products therefrom in step 3 is first warming up to 85 DEG C of constant temperature and processes 4h, then be aged 4h at 70 DEG C, make raw
The magnesium hydroxide particle further growth become, to reach to meet the standard of preparation Flame Retardant Magnesium Hydroxide, obtains slag specimen.
5. step 4 gained slag specimen vacuum pump sucking filtration is dehydrated, uses the alternately washing of hot water and ethanol, at 100-105 DEG C
The prepared thick product of Flame Retardant Magnesium Hydroxide after drying under (have only to dry moisture to constant weight, therefore temperature is without the highest).
In the present embodiment, the response rate (product magnesium accounts for the ratio of magnesium in heavy metal sewage sludge) of magnesium can reach 90.2%, product
Purity can reach 97.3%, and particle diameter is distributed between 1.0-9.5 μm, mean diameter 6.57 μm, and BET result is 16.9m/g,
SEM result shows that granule is hexagonal flake, 101 microcosmic internal strains η: 2.8x10-3。
Embodiment 3
A kind of method recycling magnesium from heavy metal sewage sludge, comprises the following steps:
1. pretreatment washing: heavy metal sewage sludge is added pure water with mud dry biomass than 10:1 according to pure water, opens electric furnace liter
Temperature, finally stable at 82 DEG C by dilute sulfuric acid aqueous solution regulation pH to the 7.5(temperature of 0.5g/L while stirring, pH=7.5 is at this
At a temperature of record), continue stirring 12min, obtain grain slag mixture through filter press be dehydrated, obtain filtrate 1 and filtering residue 1;Filtering residue 1 is used
80-90 DEG C of hot wash filtering means dehydration 2 times, obtains filtrate 2.Filtrate 1 is 2-in-1 with filtrate and gained filtrate is magnesium liquid.Magnesium in magnesium liquid
The ratio of magnesium in heavy metal sewage sludge that accounts for reaches more than 99%, and the content of Ni is 0.3mg/L, and Co, Mn, Zn do not detect, the content of Cu
0.1mg/L, Na, Ca, although but Cl-content is higher harmless to preparing magnesium hydroxide.
2. add alkali liquor magnesium sinking: take gained magnesium liquid 2000ml in step 1, use Japan's Shimadzu atomic absorption spectrophotometer
AA-7000 measures magnesium ion concentration in magnesium liquid, according to the use of the excess coefficient 8 times multiple of ammonia theoretical value consumption (magnesium sinking need)
Amount adds AR level ammonia regulation pH value in 2000mL magnesium liquid, reacts 30-40min magnesium sinking, i.e. magnesium ion and hydrogen at 30-40 DEG C
Oxygen radical ion combines and forms magnesium hydrate precipitate.
3. surface modification: add the sodium dodecyl benzene sulfonate aqueous solution of mass fraction 8% in step 2 products therefrom
15mL, as surface modifier, reacts 35min modified magnesium hydroxide at 35 DEG C;
4. ageing: products therefrom in step 3 is first warming up to 87 DEG C of constant temperature and processes 5h, then be aged 6h at 85 DEG C, make generation
Magnesium hydroxide particle further growth, to reach to meet the standard of preparation Flame Retardant Magnesium Hydroxide, obtains slag specimen.
5. step 4 gained slag specimen vacuum pump sucking filtration is dehydrated, uses the alternately washing of hot water and ethanol, at 100-105 DEG C
The prepared thick product of Flame Retardant Magnesium Hydroxide after drying under (have only to dry moisture to constant weight, therefore temperature is without the highest).
In the present embodiment, the response rate (product magnesium accounts for the ratio of magnesium in heavy metal sewage sludge) of magnesium can reach 87.7%, product
Purity can reach 96.7%, and particle diameter is distributed between 1.1-9.5 μm, mean diameter 6.62 μm, and BET result is 16.6m/g,
SEM result shows that granule is hexagonal flake, 101 microcosmic internal strains η: 2.7x10-3。
Claims (4)
1. the method recycling magnesium from heavy metal sewage sludge, it is characterised in that comprise the following steps:
Step 1, pretreatment is washed: than 8:1 ~ 15:1, heavy metal sewage sludge is added pure water with mud dry biomass according to pure water,
Heat while stirring, be heated to 80 ~ 85 DEG C and be incubated, during heated and stirred, add the dilute sulfuric acid of 0.4g/L ~ 0.6g/L
Until recording pH at 80 ~ 85 DEG C is 7.0 ~ 8.0, continue stirring 10 ~ 15min, obtain grain slag mixture and be dehydrated through filter press, obtain filter
Liquid 1 and filtering residue 1;Filtering residue 1 is used hot wash filtering means dehydration 1 ~ 3 time, obtains filtrate 2;Filtrate 1 is 2-in-1 with filtrate and gained filtrate is
For magnesium liquid;
Step 2, adds alkali liquor magnesium sinking: take gained magnesium liquid in the step 1 of certain volume, measures magnesium ion concentration in magnesium liquid, by excess
The consumption that coefficient is 3 ~ 8 times adds AR level ammonia and reacts 30-40min magnesium sinking, i.e. magnesium ion and hydroxide ion knot at 30-40 DEG C
Close and form magnesium hydrate precipitate;
Step 3, surface modification: the dodecylbenzene sodium sulfonate adding mass fraction 10-15% in step 2 products therefrom is water-soluble
Liquid 5-15mL, as surface modifier, reacts 30-40min modified magnesium hydroxide at 30-40 DEG C;
Step 4, ageing: after products therefrom in step 3 is first warming up to 85-90 DEG C of constant temperature process 3-5h older at 65-80 DEG C
Change 2-6h, obtain slag specimen;
Step 5, by the vacuum pump sucking filtration dehydration of step 4 gained slag specimen, uses the alternately washing of hot water and ethanol, at 100-105 DEG C
The thick product of Flame Retardant Magnesium Hydroxide is prepared after lower drying.
2. according to the method recycling magnesium from heavy metal sewage sludge described in claim, it is characterised in that:
In step 1, heavy metal sewage sludge is added pure water with mud dry biomass than 15:1 according to pure water, heats while stirring,
It is heated to 85 DEG C and is incubated, during heated and stirred, adding the dilute sulfuric acid of 0.6g/L until recording pH at 85 DEG C is 8.0, continuing
Stirring 15min, obtains grain slag mixture and is dehydrated through filter press, obtain filtrate 1 and filtering residue 1;By filtering residue 1 hot wash filtering means dehydration
3 times, obtain filtrate 2;Filtrate 1 is 2-in-1 with filtrate and gained filtrate is magnesium liquid.
3. according to the method recycling magnesium from heavy metal sewage sludge described in claim, it is characterised in that:
In step 2, in magnesium liquid, add AR level ammonia according to the consumption of excess coefficient 5 times.
4. according to the method recycling magnesium from heavy metal sewage sludge described in claim, it is characterised in that:
In step 2, in described magnesium liquid, magnesium ion concentration is recorded by Japan Shimadzu atomic absorption spectrophotometer AA-7000.
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