CN106929698B - A kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome - Google Patents
A kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome Download PDFInfo
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- CN106929698B CN106929698B CN201511023816.7A CN201511023816A CN106929698B CN 106929698 B CN106929698 B CN 106929698B CN 201511023816 A CN201511023816 A CN 201511023816A CN 106929698 B CN106929698 B CN 106929698B
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B15/00—Other processes for the manufacture of iron from iron compounds
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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
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B2200/00—Recycling of non-gaseous waste material
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- 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 invention belongs to chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome technical fields, and in particular to a kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome；The present invention uses nitration mixture enhanced leaching, leaches the Cr VI in later period addition reducing agent reducing leaching liquid and slag, and the iron and trivalent chromium in leachate carry out extraction and separation recycling, achievees the purpose that the harmless treatment of chromium slag and the synthetical recovery of iron.Using this method handle chromium slag, can by chromium slag Cr VI and trivalent chromium dissolve out as far as possible, reduce chromic wastes disposal after again occur brightness reversion risk.And synthetical recovery iron and chromium, Fe (OH)3With Cr (OH)3Purity is greater than 99.0%, obtained product iron hydroxide and chromium hydroxide purity is high.
Description
Technical field
The invention belongs to chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome technical fields, and in particular to a kind of chromium slag nitration mixture
Enhanced leaching-extraction and recovery siderochrome processing method.
Background technique
The metal simple-substance and compound of chromium are in plating casting, chemical industry metallurgical, leather manufacture, bio-pharmaceuticals and aviation
The conglomeraties such as space flight are widely used, rank most competitive one of 8 kinds of raw materials.Chromic salts is even more to hold the balance in China status,
15% product is all inseparable with its in national economy, China's chromic salts compound 2006 industrial annual value of production about 4,000,000,000.External chromium
Salt production history is more than 200 years, and annual output is more than 1200kt, and mainly there are the countries such as the United States, Russia, English, day, moral in producing region.Chinese chromic salts
Development only has 50 years, but develops rapidly, at present chromium salt production amount and the 1st, the world consumption figure Jun Ju.Chromic salts is economical to pull
It increases rapidly while play a great role, the severe toxicity for also bringing the title of " city bomb " and " fearful city malignant tumor " is secondary
Product-chromium slag.In general, the production quantity of slag of crome metal is 10 times of its output, chromic salts produces 3-5 times that the quantity of slag is its production.
Total chrome content is 1-7% in chromium slag, and Cr (VI) content accounts for 1-3%, wherein water-soluble and acid-soluble Cr (VI) ratio is about 2:
3.Soluble Cr (VI) have strong oxidizing property, mutagenicity and carcinogenicity, be internationally recognized 3 kinds of carcinogenic metallic compounds it
One.According to statistics, once there were 70 Duo Ge chromium salt production factories in the whole nation, and national production capacity is about 300kt/a, since technique is backward and chromium slag
Pollution control burden is big, and stop production and change the line of production about more than 40 families, existing chromium salt factory 25 of the whole nation.Since production technology is backward and environmental protection
Consciousness is weak, and China's left over by history chromium slag stores up total amount in 4500kt or so, and also increases every year with the quantity for being more than 800kt
Add.Currently, chromium slag is arbitrarily stored up, not only occupy large amount of land resources, and the surface water of the leachate contamination containing Cr (VI) and
Underground water, tiny flying dust can also pollute atmosphere, cause significant damage to ecological environment and people's life health.Early in 2005 10
Month, joint formulation announcement " chromium slag contaminated comprehensive improvement action scheme ", which has been formulated, was basically completed chromium slag contaminated site in 2012
The target administered and restored.To current cut-off, this target is not yet realized.Therefore, the innoxious and recycling for carrying out chromium slag is ground
Studying carefully has extremely important realistic meaning.
Summary of the invention
For the above-mentioned prior art, it is an object of that present invention to provide a kind of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome
Processing method, to chromium slag carry out harmless treatment.
In order to achieve the above object, a kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome of the present invention, packet
Include following steps:
Step 1: by chromium slag certain liquid-solid ratio and at a temperature of, a certain amount of sulfuric acid and hydrochloric acid is added by six in chromium slag
Valence chromium is dissolved out with trivalent chromium；
Step 2: the reduction that a certain amount of reducing agent carries out Cr VI is added after nitration mixture dissolution chromium slag；
Step 3: a certain amount of polyethers, which is added, after reduction stirs evenly and stand the regular hour, liquid is then carried out
Gu separation；
Step 4: obtained leachate TBP is extracted ferric iron；
Step 5: the organic phase for having extracted iron is washed with hydrochloric acid, the impurity of entrainment is washed away, concentration of hydrochloric acid is 3~
6mol/L, cleaning solution return to carry out the leaching of chromium slag；Load iron organic phase after washing is stripped with water, time of contact
1~20min, is 1:1~50:1 compared to O/A, 2~10 grades of series, obtains ferric chloride solution by 10~40 DEG C of temperature；
Step 6: it is 2~5 that the NaOH of the raffinate after extraction iron, which is adjusted pH value, trivalent chromium is extracted with P204；
Step 7: the organic phase for having extracted chromium is washed with the solution that pH value is 2~4, remaining impurity is washed away, is washed
Water returns to carry out the leaching of chromium slag；
Step 8: the load chromium organic phase acid back extraction after washing.
The liquid-solid ratio that further chromium slag described in step 1 leaches is 3:1~20:1, and temperature is 60~100 DEG C, the time
For 20~120min；The nitration mixture of addition is sulfuric acid and hydrochloric acid, and sulphuric acid is 0.1~1 times of chromium slag amount, and hydrochloric acid additional amount is
0.5~3 times of chromium slag amount.
The additional amount of reducing agent described in further step 2 is the 0.1%~5% of chromium slag amount, the reaction time 0.5
~5h.
Reducing agent described further is that glucose, sodium sulfite, sodium pyrosulfite, sodium thiosulfate are any.
Polyethers additional amount described in further step 3 is the 0.3%~3% of chromium slag amount, and the reaction time is 0.5~2h,
It is filtered after standing 12~48h.
Extractant concentration described in further step 4 is 10~30%, and diluent is sulfonated kerosene；Extraction stoste passes through
Hydrochloric acid and sodium chloride is added, guarantees that acidity is greater than 0.5mol/L, chloride content is greater than 100g/L；TBP extract iron time of contact be 1~
20min, extracts 3~9 grades of series by 10~40 DEG C of extraction temperature, extraction phase ratio O/A=1:5~5:1.
P204 concentration described in further step 6 is 10%~30%, and diluent is sulfonated kerosene, and P204 saponification degree is
20%~80%；Extraction time of contact is 1~20min, 10~40 DEG C of extraction temperature, extraction phase ratio O/A=1:5~5:1, is extracted
3~9 grades of series.
Back extraction time of contact described in further step 8 is 5~30min, and temperature is 20~40 DEG C, is compared to O/A
1:1~50:1, extraction series are 2~10 grades.
Technical solution provided in an embodiment of the present invention has the benefit that
A kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome of the present invention uses nitration mixture enhanced leaching, leaching
The Cr VI in reducing agent reducing leaching liquid and slag is added in the later period out, and the iron and trivalent chromium in leachate carry out extraction and separation and returns
It receives, the method for reaching the harmless treatment of chromium slag and the synthetical recovery of iron.
A kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome of the present invention compared with existing other methods,
Thoroughly with Cr VI dissolution, trivalent chromium is also largely dissolved, and the risk of brightness reversion occurs after reduction chromic wastes disposal again, and comprehensive
Iron and chromium are recycled, obtained product iron hydroxide and chromium hydroxide purity is high.
Specific embodiment
It elaborates With reference to embodiment to the present invention.
A kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome of the present invention, comprising the following steps:
Step 1: by chromium slag certain liquid-solid ratio and at a temperature of, a certain amount of sulfuric acid and hydrochloric acid is added by six in chromium slag
Valence chromium is dissolved out with trivalent chromium；
The liquid-solid ratio that chromium slag leaches is 3:1~20:1, and temperature is 60~100 DEG C, and the time is 20~120min；What is be added is mixed
Acid is sulfuric acid and hydrochloric acid, and sulphuric acid is 0.1~1 times of chromium slag amount, and hydrochloric acid additional amount is 0.5~3 times of chromium slag amount；
Step 2: the reduction that a certain amount of reducing agent carries out Cr VI is added after nitration mixture dissolution chromium slag；
Reducing agent used is any, additional amounts such as glucose, sodium sulfite, sodium pyrosulfite, sodium thiosulfate
It is the 0.1%~5% of chromium slag amount, the reaction time is 0.5~5h；
Step 3: a certain amount of polyethers, which is added, after reduction stirs evenly and stand the regular hour, liquid is then carried out
Gu separation；
Polyethers additional amount is the 0.3%~3% of chromium slag amount, and the reaction time is 0.5~2h, is filtered after standing 12~48h；
Step 4: obtained leachate TBP is extracted ferric iron；
Extractant concentration is 10~30%, and diluent is sulfonated kerosene；Extract stoste by the way that hydrochloric acid and sodium chloride is added, guarantees
Acidity is greater than 0.5mol/L, and chloride content is greater than 100g/L；TBP extraction iron time of contact is 1~20min, extraction temperature 10~40
DEG C, extraction phase ratio O/A=1:5~5:1 extracts 3~9 grades of series；
Step 5: the organic phase for having extracted iron is washed with hydrochloric acid, the impurity of entrainment is washed away, concentration of hydrochloric acid is 3~
6mol/L, cleaning solution return to carry out the leaching of chromium slag；
Load iron organic phase after washing is stripped with water, 1~20min of time of contact, is compared by 10~40 DEG C of temperature
O/A is 1:1~50:1,2~10 grades of series, obtains ferric chloride solution；
Step 6: it is 2~5 that the NaOH of the raffinate after extraction iron, which is adjusted pH value, trivalent chromium, P204 concentration are extracted with P204
It is 10~30%, diluent is sulfonated kerosene, and P204 saponification degree is 20%~80%；
Extraction time of contact is 1~20min, 10~40 DEG C of extraction temperature, extraction phase ratio O/A=1:5~5:1, extracts grade
3~9 grades of number；
Step 7: the organic phase for having extracted chromium is washed with the solution that pH value is 2~4, remaining impurity is washed away, is washed
Water returns to carry out the leaching of chromium slag；
Step 8: the load chromium organic phase acid back extraction after washing, acid used is hydrochloric acid or sulfuric acid, concentration 0.5mol/L~
3mol/L；
Back extraction time of contact is 5~30min, and temperature is 20~40 DEG C, is 1:1~50:1 compared to O/A, and extraction series is
2~10 grades.
Embodiment one
Certain chromium slag contains total chromium 3.12%, Cr VI 0.85%, and 6L water, the 200ml concentrated sulfuric acid, 1500ml salt is added in 1kg chromium slag
Acid after reacting 60min at 60~80 DEG C, is added 40g glucose and restores 3h at 80~90 DEG C, adds polyethers 15g stirring
30min stops stirring, and standing filters afterwards for 24 hours, obtains containing total chromium 3.56g/L, Cr VI 0.5mg/L, iron 8.7g/L.Titanium dioxide
The leachate of silicon 0.4g/L.Remaining slag dry weight 950g contains total chromium 0.23%, presses " hazardous waste judging standard-to the slag after washing
Leaching characteristic identification " (GB5085.3-2007), HJ687-2014 alkali digestion procedure, is dissolved and is detected, water soluble hexavalent chromium
Content meet as defined in " chromic salts industry pollutant emission standard ", water soluble hexavalent chromium is less than the second level of 8mg/kg in waste residue
Discharge standard.
Extract Fe3+Condition: extractant 30%TBP, diluent are sulfonated kerosene.First adjusting raw material liquid acidity with hydrochloric acid is
0.5mol, and a certain amount of NaCl is added, so that Cl in solution-Reach 100g/L.Sodium chlorate is added to aoxidize at 80 DEG C
60min, sodium chlorate additional amount are 0.3%, by ferrous oxidising for ferric iron.Extraction phase ratio O/A=2, time of contact 5min, extraction
Taking series is 6 grades, and raffinate contains Fe3+10mg/L.Iron organic phase 5mol/L salt acid elution is carried, O/A=5/1, scrubbing stage are compared
Number is 4 grades, and wash water returns to carry out the leaching of chromium slag.Load iron organic phase after washing is stripped iron with pure water, and O/A=is compared in back extraction
10, time of contact 3min, back extraction series are 5 grades, obtain the strip liquor of iron content 30g/L.
Cr3+Extraction: extractant be 10%P204+10% n-octyl alcohol+sulfonated kerosene, saponification degree 50%.Use sodium hydroxide
Adjusting has extracted ferric remaining phase, and adjusting pH value is 3.Extraction phase ratio O/A=2, time of contact 5min, extraction series are 10 grades,
Raffinate contains Cr3+1.5mg/L.The water washing that chromium organic phase pH value is 3 is carried, O/A=3 is compared, series is 3 grades.After washing
It carries chromium organic phase to be stripped with 1mol/L sulfuric acid, compares O/A=1/20, series is 4 grades, obtains the Cr of 35g/L3+Solution.
Claims (8)
1. a kind of processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome, which is characterized in that this method includes following step
It is rapid:
Step 1: by chromium slag certain liquid-solid ratio and at a temperature of, a certain amount of sulfuric acid and hydrochloric acid is added by the Cr VI in chromium slag
It is dissolved out with trivalent chromium；
Step 2: the reduction that a certain amount of reducing agent carries out Cr VI is added after nitration mixture dissolution chromium slag；
Step 3: a certain amount of polyethers, which is added, after reduction stirs evenly and stand the regular hour, then carries out liquid and divide admittedly
From；
Step 4: obtained leachate TBP is extracted ferric iron；
Step 5: the organic phase for having extracted iron is washed with hydrochloric acid, the impurity of entrainment is washed away, concentration of hydrochloric acid is 3~6mol/
L, cleaning solution return to carry out the leaching of chromium slag；Load iron organic phase after washing is stripped with water, time of contact 1~
20min, is 1:1~50:1 compared to O/A, 2~10 grades of series, obtains ferric chloride solution by 10~40 DEG C of temperature；
Step 6: it is 2~5 that the NaOH of the raffinate after extraction iron, which is adjusted pH value, trivalent chromium is extracted with P204；
Step 7: the organic phase for having extracted chromium is washed with the solution that pH value is 2~4, remaining impurity is washed away, wash water returns
Go back to carry out the leaching of chromium slag；
Step 8: the load chromium organic phase acid back extraction after washing.
2. the processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome according to claim 1, which is characterized in that
The liquid-solid ratio that chromium slag described in step 1 leaches is 3:1~20:1, and temperature is 60~100 DEG C, and the time is 20~120min；Add
The nitration mixture entered is sulfuric acid and hydrochloric acid, and sulphuric acid is 0.1~1 times of chromium slag amount, and hydrochloric acid additional amount is the 0.5~3 of chromium slag amount
Times.
3. the processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome according to claim 1, which is characterized in that
The additional amount of reducing agent described in step 2 is the 0.1%~5% of chromium slag amount, and the reaction time is 0.5~5h.
4. the processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome according to claim 2, which is characterized in that
The reducing agent be glucose, sodium sulfite, sodium pyrosulfite, sodium thiosulfate any one.
5. the processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome according to claim 1, which is characterized in that
Polyethers additional amount described in step 3 is the 0.3%~3% of chromium slag amount, and the reaction time is 0.5~2h, after standing 12~48h
Filtering.
6. the processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome according to claim 1, which is characterized in that
Extractant concentration described in step 4 is 10~30%, and diluent is sulfonated kerosene；Extract stoste by the way that hydrochloric acid and chlorination is added
Sodium guarantees that acidity is greater than 0.5mol/L, and chloride content is greater than 100g/L；TBP extraction iron time of contact is 1~20min, extraction temperature
10~40 DEG C, extraction phase ratio O/A=1:5~5:1, extract 3~9 grades of series.
7. the processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome according to claim 1, which is characterized in that
P204 concentration described in step 6 is 10%~30%, and diluent is sulfonated kerosene, and P204 saponification degree is 20%~80%；Extraction
Time of contact is 1~20min, 10~40 DEG C of extraction temperature, extraction phase ratio O/A=1:5~5:1, extracts 3~9 grades of series.
8. the processing method of chromium slag nitration mixture enhanced leaching-extraction and recovery siderochrome according to claim 1, which is characterized in that
Back extraction time of contact described in step 8 is 5~30min, and temperature is 20~40 DEG C, is 1:1~50:1, extraction compared to O/A
Series is 2~10 grades.
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| CN109536708B (en) * | 2018-12-17 | 2021-08-06 | 江苏永葆环保科技有限公司 | A kind of separation method of chromium and iron in pickling waste liquid |
| CN113477666A (en) * | 2021-07-05 | 2021-10-08 | 东北大学 | Method for removing hexavalent chromium from chromium slag |
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