CN102757141A - Method for processing heavy metal nickel in stainless steel pickling mixed waste acid - Google Patents
Method for processing heavy metal nickel in stainless steel pickling mixed waste acid Download PDFInfo
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- CN102757141A CN102757141A CN2012102770280A CN201210277028A CN102757141A CN 102757141 A CN102757141 A CN 102757141A CN 2012102770280 A CN2012102770280 A CN 2012102770280A CN 201210277028 A CN201210277028 A CN 201210277028A CN 102757141 A CN102757141 A CN 102757141A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 23
- 239000010935 stainless steel Substances 0.000 title claims abstract description 23
- 239000002253 acid Substances 0.000 title claims abstract description 22
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 21
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 20
- 238000005554 pickling Methods 0.000 title abstract description 7
- 238000012545 processing Methods 0.000 title abstract description 7
- 239000010812 mixed waste Substances 0.000 title abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 29
- 239000012065 filter cake Substances 0.000 claims abstract description 20
- 239000002351 wastewater Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 9
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 9
- 239000004571 lime Substances 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005189 flocculation Methods 0.000 claims abstract description 7
- 230000016615 flocculation Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 11
- 239000010802 sludge Substances 0.000 claims description 11
- 238000011010 flushing procedure Methods 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 229910001453 nickel ion Inorganic materials 0.000 claims description 4
- 238000011084 recovery Methods 0.000 abstract description 21
- 239000002002 slurry Substances 0.000 abstract description 3
- 229920002401 polyacrylamide Polymers 0.000 abstract 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000004537 pulping Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 4
- 239000002562 thickening agent Substances 0.000 description 4
- 238000009388 chemical precipitation Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- -1 metals ion Chemical class 0.000 description 3
- 239000010801 sewage sludge Substances 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XWROUVVQGRRRMF-UHFFFAOYSA-N F.O[N+]([O-])=O Chemical compound F.O[N+]([O-])=O XWROUVVQGRRRMF-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Treatment Of Sludge (AREA)
- Removal Of Specific Substances (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
Disclosed is a method for processing heavy metal nickel in a stainless steel pickling mixed waste acid. Lime slurries are added into the stainless steel pickling mixed waste acid, the potential of hydrogen (pH) value is adjusted to 3.5, then polyacrylamide is added to generate sludges, a filter cake produced after the sludges are subjected to a filter pressing is subjected to mixed stirring, pulping and filter pressing by stainless steel factory workshop ground washing wastewater, the produced filter pressing liquor and the filter pressing liquor produced by the filter pressing of sludges are mixed, then the lime slurries are added into the mixed filter pressing liquor, the pH value is adjusted to 9.5, then the polyacrylamide is added to perform a flocculation precipitation to generate sludges, the filter cake and the filter pressing liquor are formed after the filter pressing of the sludges, the filter cake is recycled, sulfuric acid is added into the filter pressing liquor, the pH value of the filter pressing liquor is adjusted to 8, and the filter pressing liquor is directly discharged or recycled. By means of the method, the recovery ratio of heavy metal in the sludges can be improved, the recycling of the sludges is guaranteed, and the stainless steel factory workshop ground washing wastewater can be comprehensively utilized.
Description
Technical field
The present invention relates to the recovery method of heavy metal in a kind of spent acid processing, the treatment process of heavy metal nickel in particularly a kind of acid-washing stainless steel mixing spent acid.
Technical background
In steel processing enterprise, like steel plate factory, pipe mill etc., usually to use nitration mixture (nitric acid-hydrofluoric acid mixed waste liquor) to come the acid-washed metal surface to carry out surface derusting and handle, produced a large amount of spent acid that contains metals ion in the treating processes.Just be not discharged in the environment if it is not handled, spent acid solution will work the mischief to the mankind and natural, ecological.
Existing people is applied to the processing of waste acid from stainless steel acid washing and the extraction of heavy metal with methods such as electroosmose process, ion exchange membrane, roasting method, distillation method, fluiddized-bed roasting method, spray roasting, chemical precipitation methods both at home and abroad at present.The advantage of electroosmose process is that equipment is simple, and organic efficiency is high, can reclaim spent acid and extract iron; Its shortcoming is that current consumption is higher.Roasting method, distillation method require height because of high-temperature operation to equipment material, and equipment life is shorter, and acid gas, dust and the air pollution problems inherent of Yin Gaowen generation, make environment be difficult for keeping, and need blowing out maintenance equipment in every month, and maintenance cost is higher; The shortcoming of fluiddized-bed roasting method and spray roasting is that equipment cost is high, the scale restriction is arranged, and air pollutant emission is arranged; Chemical precipitation method has that treatment effect is good, less investment, advantage such as easy and simple to handle, but maximum shortcoming is that sludge quantity is big, the sludge dewatering difficulty, and be difficult to recycle, thereby influenced its application and development.In recent years along with the technological development of Metal smelting; The sludge disposal that makes the nickel grade reach more than 5% has had reasonable outlet; Therefore just how to adopt chemical precipitation method to improve the grade of mud efficiently; Reach the requirement of smelting, promote that the heavy metal recovery just becomes a problem demanding prompt solution in the mud.
The amount * 100 of the amount/mud of heavy metal in the grade of mud (%)=mud, therefore improving sewage sludge quality is mainly reflected in two aspects: improve heavy metal content and the amount that reduces mud in the mud.
The amount of heavy metal in the amount/water inlet of heavy metal in the heavy metal recovery (%)=mud, therefore improve heavy metal especially the recovery of nickel be mainly reflected in the content that reduces nickel in the no recovery value mud.
Summary of the invention
But the technical problem that the present invention will solve provides a kind ofly can improve the heavy metal recovery in the mud, guarantee the mud recycle value, and the treatment process of heavy metal nickel in the acid-washing stainless steel mixing spent acid of comprehensive utilization stainless steel plant mill floor flushing waste water.
For solving this technical problem, the technical scheme that the present invention adopts is:
The treatment process of heavy metal nickel in a kind of acid-washing stainless steel mixing spent acid is characterized in that may further comprise the steps:
A, one-level deposition: in containing the acid-washing stainless steel mixing spent acid of bivalent nickel ion, add the lime white of 20% (quality percentage composition), regulating its pH value is 3.5; Add-on according to 5g/ ton water adds SEPIGEL 305 (PAM), carries out flocculation sediment, and the mud of generation (staple of said mud is an ironic hydroxide, chromium hydroxide, verditer, Calcium Fluoride (Fluorspan) deposition) forms filter cake and pressing filtering liquid after the press filtration;
B, one-level precipitate and separate: filter cake among the step a and stainless steel plant's mill floor flushing waste water are mixed stirring, slurrying by solid-liquid volume ratio 1:5, carry out press filtration again, form filter cake and pressing filtering liquid;
C, the filtrating among filtrating among the step a and the step b is mixed;
D, two-stage precipitation: in through step c blended pressing filtering liquid, add 20% (quality percentage composition) lime white; Regulating its pH value is 9.5; Add-on according to 5g/ ton water adds SEPIGEL 305; Carry out flocculation sediment, the mud of generation (staple of said mud is verditer, nickel hydroxide precipitate) forms filter cake and pressing filtering liquid after the press filtration.Cupric ion, nickel ion were realized deposition completely during this pH value was filtrated down, had ensured the up to standard of water outlet, and the extraction and the recovery of nickel are carried out in the filter cake outward transport;
Add volumetric concentration in e, the pressing filtering liquid that in the d step, forms and be 10% sulfuric acid, regulating its pH value is 8, directly discharges or reuse.
Step a, d use lime as precipitation agent, and chemical equation is: 2OH-+M
2+→ M (OH)
2↓
Technique scheme because after acid-washing stainless steel mixings spent acid composition confirmed, metal content was basically confirmed in the sewage, therefore mainly is through controlling appropriate condition, and (requirement that also is qualified discharge) fully precipitates heavy metal; For reducing sludge quantity, mainly concentrate on: will have recovery value mud and no recovery value mud to separate, and dispose respectively, just fractional precipitation;
Enrichment, deposition and recovery that the characteristics of this method are to fully utilize fractionation precipitation, the methods such as recovery, comprehensive treating process that stir realize heavy metal nickel will have recovery value mud and no recovery value mud to separate simultaneously.For the problem that one-level precipitating sludge amount in the precipitation process is big, grade is not high; The control of one-level deposition pH in the real reaction; Requirement can guarantee lower nickel rate of loss; Can not react mud nickel grade to two-stage precipitation again and produce bigger detrimentally affect, therefore need to reduce the isoionic concentration of copper, iron, chromium and fluorine of first order reaction water outlet, so control first order reaction pH value is 3.5; Second order reaction pH value is controlled to be 9.5, under alkaline condition, adds milk of lime (staple is a calcium hydroxide) coprecipitated nickel hydroxide ion, generates nickel hydroxide precipitate, realizes each ionic qualified discharge simultaneously.This method combines with the use of autoclave diaphragm plate-and-frame filter press simultaneously, has further improved the nickel recovery of whole technology, and comprehensive treating process the workshop waste water that produces in the daily production in stainless steel plant.This recovery method, technology is simple and convenient, easy to operate, the nickel cost recovery is low, nickel recovery is higher, and the discharging of waste water is up to state standards (electroplate pollutant emission standard (GB21900-2008)), has favorable economic benefit and social benefit.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
Certain stainless steel plant's pickling mixing acid-spending strength and mill floor flushing waste water influent quality index are seen table 1, table 2:
Table 1 pickling mixing spent acid influent quality
Table 2 mill floor flushing waste water influent quality
Referring to Fig. 1, the treatment process of heavy metal nickel in a kind of acid-washing stainless steel mixing spent acid is 3.5 to be example with one-level deposition pH value, comprises the steps:
A, one-level deposition: pickling the mixings spent acid of pickling workshop, stainless steel plant discharging (water: hydrofluoric acid: the entering equalizing tank of nitric acid=6:1.5:1); In this equalizing tank with PLC (programmable logic controller) by 300 kilograms of/hour lime whites that add 20% (quality percentage composition), regulating its pH value is 3.5; Through the add-on adding SEPIGEL 305 (PAM) of PLC according to 5g/ ton water; Carry out flocculation sediment; The mud that generates (staple of said mud is an ironic hydroxide, chromium hydroxide, verditer, Calcium Fluoride (Fluorspan) deposition) uses spiral pump to be delivered into sludge thickener and carries out the concentrated moisture percentage in sewage sludge that reduces of mud; Mud in the sludge thickener after preliminary the concentrating is delivered into the autoclave diaphragm sheet frame by mortar pump and carries out press filtration; Form filter cake and pressing filtering liquid, the filter cake outward transport is disposed, and filtrating gets in the pressing filtering liquid outlet sump;
B, one-level precipitate and separate: the ground flushing waste water of workshop, stainless steel plant discharging (said mill floor wash-down water is to adopt the tap water flushing to contain the ground of mixing spent acid by daily production to produce) gets into the flushing waste water intermediate pool; And filter cake among the step a and stainless steel plant's mill floor flushing waste water used machine mixer mixing stirring by solid-liquid volume ratio 1:5; Slurrying; And adopt the autoclave diaphragm sheet frame that slurries are carried out press filtration, and forming filter cake and pressing filtering liquid, the filter cake outward transport is disposed;
Pressing filtering liquid among c, the step b flows back in the outlet sump of the pressing filtering liquid that step a autoclave diaphragm sheet frame produces automatically;
D, two-stage precipitation: add 20% lime white through PLC by 50 kilograms/hour in the pressing filtering liquid outlet sump in step a; Regulating its pH value is 9.5; Through PLC, add SEPIGEL 305 (PAM) 0.005g/L, carry out flocculation sediment; The mud (staple of said mud is verditer, nickel hydroxide precipitate) that generates; Use spiral pump to be delivered into sludge thickener and carry out the concentrated moisture percentage in sewage sludge that reduces of mud, the mud in the sludge thickener after preliminary the concentrating is delivered into the autoclave diaphragm sheet frame by mortar pump and carries out press filtration, forms filter cake and pressing filtering liquid.Cupric ion, nickel ion were realized deposition completely during this pH value was filtrated down, had ensured the up to standard of water outlet, and the extraction and the recovery of nickel are carried out in the filter cake outward transport;
Adding 35 kilograms/hour through PLC in e, the filtrating that in the d step, forms, to add volumetric concentrations be 10% sulfuric acid, and regulating its pH value is 8, directly discharges.
Table 3 experiment records each index value of water outlet
Adopting the one-level deposition to regulate the pH value is 3.5; The mill floor wash-down water mixed with the one-level precipitating sludge stir press filtration and reclaim pressing filtering liquid, two-stage precipitation pH value is that the processing cost of this waste water is 58.840 yuan/ton under 9.5 the method; Processing cost is lower; The recovery of nickel is 86.05%, and better results for the recovery, and water outlet each item index meets country's plating pollutant emission standard (GB21900-2008).
Claims (1)
1. the treatment process of heavy metal nickel in the acid-washing stainless steel mixing spent acid is characterized in that may further comprise the steps:
A, one-level deposition: in containing the acid-washing stainless steel mixing spent acid of bivalent nickel ion, add 20% lime white, regulating its pH value is 3.5; Add-on according to 5g/ ton water adds SEPIGEL 305, carries out flocculation sediment, and the mud of generation forms filter cake and pressing filtering liquid after press filtration;
B, one-level precipitate and separate: filter cake among the step a and stainless steel plant's mill floor flushing waste water are mixed stirring, slurrying by solid-liquid volume ratio 1:5, carry out press filtration again, form filter cake and pressing filtering liquid;
C, the filtrating among filtrating among the step a and the step b is mixed;
D, two-stage precipitation: in through step c blended pressing filtering liquid, add 20% lime white; Regulating its pH value is 9.5, and the add-on adding SEPIGEL 305 according to 5g/ ton water carries out flocculation sediment; Form filter cake and pressing filtering liquid behind the sludge press filtration that generates, filter cake is recycled;
Add sulfuric acid in e, the pressing filtering liquid that in the d step, forms, regulating its pH value is 8, directly discharging or reuse.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012102770280A CN102757141A (en) | 2012-08-06 | 2012-08-06 | Method for processing heavy metal nickel in stainless steel pickling mixed waste acid |
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| CN2012102770280A CN102757141A (en) | 2012-08-06 | 2012-08-06 | Method for processing heavy metal nickel in stainless steel pickling mixed waste acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896426A (en) * | 2014-01-09 | 2014-07-02 | 湛江市聚鑫新能源有限公司 | Wastewater treatment method after purification of lithium ion battery negative material spherical graphite |
| CN104310647A (en) * | 2014-10-21 | 2015-01-28 | 徐超群 | Recycling method for treating stainless steel pickling acid pickle and wastewater |
| CN105565547A (en) * | 2016-02-01 | 2016-05-11 | 浙江大学 | Method for treating heavy metal wastewater through organic flocculant |
| CN110002567A (en) * | 2019-03-22 | 2019-07-12 | 浦项(张家港)不锈钢股份有限公司 | A kind of method that stainless steel annealing pickling waste waters neutralizes and sludge is applied flexibly |
| CN116027712A (en) * | 2023-01-12 | 2023-04-28 | 中国科学院赣江创新研究院 | A kind of rare earth enrichment, extraction method and application of rare earth in waste acid of zirconium smelting |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896426A (en) * | 2014-01-09 | 2014-07-02 | 湛江市聚鑫新能源有限公司 | Wastewater treatment method after purification of lithium ion battery negative material spherical graphite |
| CN104310647A (en) * | 2014-10-21 | 2015-01-28 | 徐超群 | Recycling method for treating stainless steel pickling acid pickle and wastewater |
| CN105565547A (en) * | 2016-02-01 | 2016-05-11 | 浙江大学 | Method for treating heavy metal wastewater through organic flocculant |
| CN110002567A (en) * | 2019-03-22 | 2019-07-12 | 浦项(张家港)不锈钢股份有限公司 | A kind of method that stainless steel annealing pickling waste waters neutralizes and sludge is applied flexibly |
| CN116027712A (en) * | 2023-01-12 | 2023-04-28 | 中国科学院赣江创新研究院 | A kind of rare earth enrichment, extraction method and application of rare earth in waste acid of zirconium smelting |
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Application publication date: 20121031 |