CN105833985A - Selective separation and recycling method for industrial solid waste slag - Google Patents
Selective separation and recycling method for industrial solid waste slag Download PDFInfo
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- CN105833985A CN105833985A CN201610173616.8A CN201610173616A CN105833985A CN 105833985 A CN105833985 A CN 105833985A CN 201610173616 A CN201610173616 A CN 201610173616A CN 105833985 A CN105833985 A CN 105833985A
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- solid waste
- selective separation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated
- B03B1/04—Conditioning for facilitating separation by altering physical properties of the matter to be treated by additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B9/00—General arrangement of separating plant, e.g. flow sheets
- B03B9/04—General arrangement of separating plant, e.g. flow sheets specially adapted for furnace residues, smeltings, or foundry slags
Abstract
Disclosed is a selective separation and recycling method for industrial solid waste slag. The selective separation and recycling method is suitable for recycling the solid waste slag generated in steel, metallurgy and chemical industries. The selective separation and recycling method is based on the systematic study of the microstructure of the industrial solid waste slag, high-selectivity chemical agents are adopted, through soaking, milling, magnetic separation, multistage sedimentation and other process steps, bonding materials between crystalline particles are dissolved or softened, and thus spatial dissociation of the crystalline particles with different components is achieved with a chemical method. Meanwhile, the surface characteristics of certain crystalline particles are changed selectively through the high-selectivity chemical agents, the differences of the sedimentation performance of different components are enhanced, separation of multistage sedimentation is completed conveniently, thus the separation efficiency is improved, energy consumption can be reduced by a large margin, and the treatment process is simplified. The selective separation and recycling method is suitable for recycling steel slag, stainless steel slag, metallurgy waste slag and the like and can also be used for recycling useful components or enrichment of certain trace elements from chemical solid waste slag.
Description
Technical field
The invention belongs to industrial solid waste residue recovery and utilization technology field, it is adaptable to iron and steel, metallurgy and chemical industry are produced
Raw solid slag reclaims the most useful metal and compound thereof.
Background technology
In the production processes such as iron and steel, metallurgy, chemical industry, often give up with a large amount of solid containing metal and oxide thereof of discharge
Slag, such as the ironmaking scum of industry, steel slag, the slag of rustless steel industry, the metallurgical slag etc. of nonferrous metallurgy industry, on the one hand,
How containing element and compounds thereof such as ferrum, nickel, chromium, manganese and minute amount of noble metal silver, berylliums in these solid slags, air storage is not only
Take a large amount of soil, and severe contamination Soil Surrounding and water body；On the other hand, metal and the compound thereof such as ferrum, nickel, silver, beryllium
It is again important metallurgy or industrial chemicals.Therefore, explore industrial solid waste residue to recycle and be one and significantly work.
From the point of view of the data grasped at present, it is " pulverizing-magnetic separation-mill-magnetic that above-mentioned solid waste recycles typical process
Choosing-screening-magnetic separation-gravity separation (or flotation) ".As CN1282633A, CN1282635A, CN1390795A, CN1492058A,
CN101391457A, CN161736099A etc..Seeing on the whole, these technology are in energy-conservation, magnetisable material recovery, tailings comprehensive utilization
Aspect achieves certain achievement, but yet suffers from notable deficiency.Firstly, since slag, metallurgical slag are through high-temperature calcination, have
The feature that hardness is high, granularity is big, pulverizes, grinds difficulty very greatly, serious to equipment attrition；Secondly, these solid wastes are mixed
Compound, crystallizes the trickleest, wants to reach relatively high separating efficiency and the response rate, granularity requirements very thin (typically 300 mesh with
On), needing repeatedly pulverize and grind, energy consumption is the highest.Further, during similar CN1282635A method dry process, deposit
In dust secondary pollution problem.Again, in prior art solid slag useful component reclaim only by " magnetic separation ", " gravity separation (or
Flotation) " etc. limited means, and many metals and oxide thereof do not have magnetic, and grain granule is mutually bonded, it is difficult to thoroughly
Dissociate, so nonmagnetic metal and oxide recovering effect thereof are the most undesirable.
Numerous studies show, major part industrial solid waste residue all contains a large amount of silicate, and wherein part silicate is micro-
Present amorphous state in sight, become the main bridge that crystalline particle or metallic particles in solid slag mutually bond；Secondly, only
There are the metal such as ferrum, chromium and partial oxide thereof more or less to possess certain magnetic, and other compositions do not have magnetic, simple magnetic mostly
The effect being difficult to reach required is reclaimed in choosing；Further, these solid slags in addition to metal or alloy granule, other major part materials
Crystalline particle is the trickleest, and general particle diameter is many between several microns to tens micron.Further, since free CaO, MgO
Etc. having water absorption behavior, in cement, these compositions exceed standard and cause building element fracture occur or split in lower meeting of exposing to the weather
Seam, threatens public and private property and user personal safety, and therefore, free CaO, MgO equal size in cement or building materials are had sternly by country
Lattice requirement, typically must not be higher than 1.5%, and the solid slags such as slag are higher than 2% more.
Summary of the invention
The present invention is directed to prior art exist drawback, on the basis of industrial solid waste residue microstructure systematic study it
On, a kind of industrial solid waste residue Selective Separation and recoverying and utilizing method are proposed so that it is hardness can be retained in solid slag relatively
Big crystalline particle or the initial pattern of alloy agglomerated particle, can be greatly reduced again energy consumption, reduces treatment process, it is achieved high selection
Property separate.
Technical scheme is as follows:
A kind of industrial solid waste residue Selective Separation and recoverying and utilizing method, is characterized in that the method comprises the steps:
1) preparation mixed chemical medicament, this mixed chemical medicament is to be mixed by following three class materials:
Acid: 10-70%
Interfacial agent: 5-10%
Auxiliary agent: 20-80%；
2) mixed chemical medicament, solid slag and water are mixed into serosity, put in fermentation vat and soak, make mixing rear slurry
Solid content be 20-50wt%；Mixed chemical medicament mass content in serosity is 1-10%；
3), after soaking rear slurry feeding mill attrition grinding, magnetic separator is entered；
4), after magnetisable material isolated by magnetic separator, serosity flows into cone tank；
5) Multistage settling groove is entered containing short grained serosity by the overflow of cone tank top, containing oarse-grained serosity in taper
Trench bottom is enriched with and returns mill to be continued to grind；
6) overflow slurry has settled separation in Multistage settling groove difference section, and after sedimentation, clear liquid returns as circulation fluid and soaks
Pond recycles；
7) after precipitum is discharged respectively by the outlet of Multistage settling trench bottom, filter respectively, dry, obtain multiple different product
Thing.
In technique scheme, described acid is the one in hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid, oxalic acid and acetic acid
Or several mixture；Described interfacial agent is polyoxyethylene ether, sodium stearyl sulfonate, oleic acid, cetyl bromination
One or more mixture in ammonium, 18-amine., triethanolamine, imidazoline and cationic-type polyacrylamide；Described auxiliary agent
For one or more mixture in sodium hexametaphosphate, sodium metasilicate, sodium silicate, ethylene glycol and glycerol.
Preferably, step 2) described in fermentation vat soak time be 0.5-6 hour.
Preferably, described magnetic separator uses multistage wet magnetic separator.
The technical characteristic of the present invention also resides in: described Multistage settling groove, width the elongated tank not waited forms, and is divided into three
To six sections, bottom of gullet is equipped with slurry discharge ports；The 5-50 second initial segment time of staying, water velocity 1-3 meter per second；From second segment
Starting, next period of time of staying is the preceding paragraph 2-3 times, and water velocity is the preceding paragraph 1/1st to three/2nd.
The present invention has the following advantages and the technique effect of salience:
First the present invention uses high selective chemical agent soften the material between crystalline particle or dissolve, auxiliary
Mill with stirring, it is achieved dissociating (great majority are amorphous silicate) in heterogeneity crystalline particle space, pulverizes with conventional mechanical
Grinding is compared, and the chemical method space granule percentage rate that dissociates is higher, dissociates more thorough.
Secondly, chemical method particle space is dissociated and is remained granule primary morphology to greatest extent, eliminates attrition grinding, thus
Energy consumption (and prior art this energy consumption typically constitute from always process energy consumption 40-50%) is greatly reduced.From recycling in terms of angle, granule
Metal and oxide thereof that difference in size is bigger have no adverse effects to recycling, as reclaimed steel scrap granular size difference in slag
Very big, big to several even tens centimetres, little to hundreds of micron, but this has no effect on waste steel recycling and utilizes；On the other hand, gold
Belonging to and composition outside oxide, crystalline particle own is the trickleest, can form relatively fine powder, be just suitable as water after separation
The higher fineness requirement of mud building materials.Therefore, retain granule primary morphology in solid slag, neither affect recycling, also reach
Energy-saving and cost-reducing purpose.
Further, chemical method achieves high Selective Separation.Mixed chemical pharmacy effect does not terminate in solid slag difference
Divide crystalline particle space to dissociate, also reside in some granular boundary of Selective activation, strengthen heterogeneity settlement difference, for sedimentation point
From having established solid foundation.Mixed chemical medicament has the strongest selectivity to different crystalline particle interfaces, and interface selective is lived
Change, cause variable grain settling property equal in magnitude, that proportion is close to present larger difference, be conducive to by Multistage settling mode
Realize separating.Experiment shows, the present invention not only has good separating effect to various slags, metallurgical slag, and to Fluorite slag
In the recovery of middle calcium fluoride, beryllium element enrichment and Zn smelting wastes, silver enrichment etc. also have good effect.
It addition, the harmless treatment of free CaO, MgO in industrial solid waste residue also taken into account by mixed chemical medicament of the present invention,
Free CaO, MgO remaining quantity add up to less than 1%, comply fully with the Standard such as clinker.
In a word, instant invention overcomes the drawbacks such as traditional handicraft high energy consumption, secondary pollution, inferior separating effect, and have extensively
The suitability, cannot be only used for the steel slag and iron slag of steel industry, stainless steel slag, is also applied for the nonferrous metallurgy solids such as Zn smelting wastes
Waste residue, it may also be used for after the fluorite flotation of fluorination work, tailings recycles.
Accompanying drawing explanation
Fig. 1 is a kind of concrete technology flow chart of industrial solid waste residue Selective Separation and recycling.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment the present invention is described further.
Fig. 1 is that the present invention proposes a kind of industrial solid waste residue Selective Separation and the process chart of recoverying and utilizing method,
It specifically includes following steps:
1) first preparation mixed chemical medicament: following three class materials are mixed in proportion, will 10-70% acid,
5-10% interfacial agent and 20-80% auxiliary agent mix homogeneously, be configured to mixed chemical medicament, and wherein said acid is
The mixture of one or more in hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid, oxalic acid and acetic acid；Described interfacial agent is polyoxy second
Alkene ether, sodium stearyl sulfonate, oleic acid, cetyl ammonium bromide, 18-amine., triethanolamine, imidazoline and cationic poly third
One or more mixture in acrylamide；Described auxiliary agent is sodium hexametaphosphate, sodium metasilicate, sodium silicate, ethylene glycol and third
One or more mixture in triol.
2) mixed chemical medicament, solid slag and water are mixed into serosity, put in fermentation vat and soak, typically at fermentation vat
Middle soak time is 0.5-6 hour；The solid content making mixing rear slurry is 20-50wt%；Mixed chemical medicament is in serosity
Mass content is 1-10wt%；
3), after soaking rear slurry feeding mill attrition grinding, magnetic separator is entered；This magnetic separator uses multistage wet magnetic separation
Machine；
4), after magnetisable material isolated by magnetic separator, serosity flows into cone tank；
5) Multistage settling groove is entered containing short grained serosity by the overflow of cone tank top, containing oarse-grained serosity in taper
Trench bottom is enriched with and returns mill to be continued to grind；Described Multistage settling groove, width the elongated tank not waited forms, and is divided into three
To six sections, bottom of gullet is equipped with slurry discharge ports；The 5-50 second initial segment time of staying, water velocity 1-3 meter per second；From second segment
Starting, next period of time of staying is the preceding paragraph 2-3 times, and water velocity is the preceding paragraph 1/1st to three/2nd.
6) overflow slurry has settled separation in Multistage settling groove difference section, and after sedimentation, clear liquid returns as circulation fluid and soaks
Pond recycles；
7) after precipitum is discharged respectively by the outlet of Multistage settling trench bottom, filter respectively, dry, obtain multiple different product
Thing.
Embodiment 1
Weigh 50 kilograms of blast furnace slags, add 100 grams of sulphuric acid, cetyl ammonium bromide 11 grams, sodium silicate (45 °, modulus
3.0) 100 grams, mix and blend 30 minutes, stand 4 hours；Then start rod mill, be passed through circulation fluid with 30 liters/min of speed and (open
Stage beginning is passed through clear water), it is continuously added to mixed serum, overflowing liquid enters three grades of magnetic separators, the solids mixing magneticly elected, and dehydration is dried
Dry；Magnetic separation rear slurry enters taper overflow settler, and bottom precipitum returns rod mill to be continued to grind, and upper strata overflow flows into precision
Subsider, subsider water channel is divided into three sections, and the time of staying is respectively 10 seconds, 50 seconds and 19 minutes, total residence time 20 minutes, sinks
After fall, clear liquid returns rod mill recycling.Three sections of water channels are deposited to the solid slurry of bottom and draw from bottom, carry out respectively
Filter and drying；After finally immersion material all adds, equipment stops after continuing to run with 30 minutes, samples weighing after drying, according to
Relevant national standard method carries out component analysis.Experimental result is as follows:
1, experimental raw analysis result: component content is wt%
2, product analysis result: component content is WT%
Embodiment 2
Weigh 50 kilograms of stainless steel smelting waste residues, add 1:1:1 nitric acid, hydrochloric acid, acetic acid mixture 100 grams, the miaow of 1:1:1
Oxazoline, oleic acid, triethanolamine mixed liquor 20 grams, the sodium sulfate of 1:1:1, sodium metasilicate, sodium silicate (45 °, modulus 3.0) mixture
100 grams, mix and blend 30 minutes, stand 6 hours；Then start rod mill, be passed through circulating clear liquid with 20 liters/min of speed and (start
Stage is passed through clear water), it is continuously added to mixed serum, overflowing liquid enters three grades of magnetic separators, the solids mixing magneticly elected, and dehydration is dried
Dry；Magnetic separation rear slurry enters taper overflow settler, and bottom precipitum returns rod mill to be continued to grind, and upper strata overflow flows into precision
Subsider, subsider water channel is divided into four sections, and the time of staying is respectively 10 seconds, 20 seconds, 30 seconds and 19 minutes, total residence time 20 points
Clock, after sedimentation, clear liquid returns rod mill recycling.Five sections of water channels are deposited to the solid slurry of bottom and draw from bottom, enter respectively
Row filters and dries；After finally immersion material all adds, equipment stops after continuing to run with 30 minutes, samples weighing after drying,
Component analysis is carried out according to relevant national standard method.Experimental result is as follows:
1, experimental raw analysis result: component content is WT%
2, product analysis result: component content is WT%
Test result indicate that, metallic iron, chromium primarily enter magnetic separation product, ferrum and chromated oxide and mainly settle at first paragraph,
Nickel settles at second segment, and manganese is the 3rd section of sedimentation, and the 4th section is settled into silicates.
Embodiment 3
Weigh 50 kilograms of metallic zinc melting waste slags, add 1:1:1 formic acid, acetic acid, benzoic acid mixed liquor 100 grams, 1:1:1's
Cetyl ammonium bromide, oleic acid, PAMC mixed liquor 20 grams, the glycerol of 1:1:1, sodium hexametaphosphate, flower bulb
Alkali (45 °, modulus 3.0) 100 grams of mixture, mix and blend 30 minutes, stand 3 hours；Then ball mill is started, with 10 liters/min
Speed is passed through circulating clear liquid (incipient stage is passed through clear water), is continuously added to mixed serum, and overflowing liquid enters three grades of magnetic separators, magnetic separation
The solids mixing gone out, dewatered drying；Magnetic separation rear slurry enters taper overflow settler, and bottom precipitum returns ball mill to be continued to grind
Mill, upper strata overflow flows into accurate subsider, and subsider water channel is divided into three sections, and the time of staying is respectively 30 seconds, 60 seconds and 18.5 points
Clock, total residence time 20 minutes, after sedimentation, clear liquid returns ball mill recycling.Five sections of water channels are deposited to the solid slurry of bottom
Draw from bottom, filter respectively and dry；After finally immersion material all adds, equipment stops after continuing to run with 30 minutes
Only, samples weighing after drying, carry out component analysis according to relevant national standard method.Experimental result is as follows:
1, experimental raw analysis result: component content is WT%
2, product analysis result: component content is WT%
Test result indicate that, metallic iron primarily enters magnetic separation product, ferrum and chromated oxide and mainly settles at first paragraph, and silver exists
Second segment sedimentation enrichment, aluminum and silicate are mainly the 3rd section of sedimentation.
Embodiment 4
Weigh 50 kilograms of fluorite flotation tailings, add 1:1:1 hydrochloric acid, nitric acid, sulfuric acid mixture liquid 100 grams, the ten of 1:1:1
Six alkyl bromination ammoniums, 18-amine., imidazoline mixed liquor 20 grams, the ammonium fluoride of 1:1:1, sodium hexametaphosphate, sodium silicate (45 °, modulus
3.0) 100 grams of mixture, mix and blend 30 minutes, stand 1 hour；Then start ball mill, be passed through circulation with 5 liters/min of speed
Clear liquid (incipient stage is passed through clear water), is continuously added to mixed serum, and overflowing liquid enters three grades of magnetic separators, and the solid magneticly elected mixes
Close, dewatered drying；Magnetic separation rear slurry enters taper overflow settler, and bottom precipitum returns ball mill to be continued to grind, and overflows in upper strata
Stream flows into accurate subsider, and subsider water channel is divided into three sections, and the time of staying is respectively 60 seconds, 15 minutes and 4 minutes, when always stopping
Between 20 minutes, after sedimentation clear liquid return ball mill recycle.Three sections of water channels are deposited to the solid slurry of bottom and draw from bottom,
Filter respectively and dry；After finally immersion material all adds, equipment stops after continuing to run with 30 minutes, sample after drying
Weigh, carry out component analysis according to relevant national standard method.Experimental result is as follows:
1, experimental raw analysis result: component content is WT%
2, product analysis result: component content is WT%
Test result indicate that, metallic iron primarily enters magnetic separation product, and calcium fluoride mainly settles at first paragraph, and silicate is the
Two-stage nitration settles, and beryllium then forms enrichment at the 3rd section.
Claims (7)
1. an industrial solid waste residue Selective Separation and recoverying and utilizing method, it is characterised in that the method comprises the steps:
1) preparation mixed chemical medicament, this mixed chemical medicament is to be mixed by following three class materials:
Acid: 10-70%
Interfacial agent: 5-10%
Auxiliary agent: 20-80%；
2) mixed chemical medicament, solid slag and water are mixed into serosity, put in fermentation vat and soak, make consolidating of mixing rear slurry
Content is 20-50wt%；Mixed chemical medicament mass content in serosity is 1-10wt%；
3), after soaking rear slurry feeding mill attrition grinding, magnetic separator is entered；
4), after magnetisable material isolated by magnetic separator, serosity flows into cone tank；
5) Multistage settling groove is entered containing short grained serosity by the overflow of cone tank top, containing oarse-grained serosity at the bottom of cone tank
Portion is enriched with and returns mill and continues to grind；
6) overflow slurry has settled separation in Multistage settling groove difference section, and after sedimentation, clear liquid follows as circulation fluid return fermentation vat
Ring uses；
7) after precipitum is discharged respectively by the outlet of Multistage settling trench bottom, filter respectively, dry, obtain multiple different product.
2. a kind of industrial solid waste residue Selective Separation as claimed in claim 1 and recoverying and utilizing method, it is characterised in that: institute
The acid stated is the mixture of one or more in hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid, oxalic acid and acetic acid.
3. a kind of industrial solid waste residue Selective Separation as claimed in claim 1 and recoverying and utilizing method, it is characterised in that: institute
The interfacial agent stated is polyoxyethylene ether, sodium stearyl sulfonate, oleic acid, cetyl ammonium bromide, 18-amine., three ethanol
One or more mixture in amine, imidazoline and cationic-type polyacrylamide.
4. a kind of industrial solid waste residue Selective Separation as claimed in claim 1 and recoverying and utilizing method, it is characterised in that: institute
The auxiliary agent stated is one or more mixture in sodium hexametaphosphate, sodium metasilicate, sodium silicate, ethylene glycol and glycerol.
5. a kind of industrial solid waste residue Selective Separation as described in claim 1-4 any claim and recycling side
Method, it is characterised in that: step 2) described in fermentation vat soak time be 0.5-6 hour.
6. a kind of industrial solid waste residue Selective Separation as described in claim 1-4 any claim and recycling side
Method, it is characterised in that: described magnetic separator uses multistage wet magnetic separator.
7. a kind of industrial solid waste residue Selective Separation as described in claim 1-4 any claim and recycling side
Method, it is characterised in that: the elongated tank that described Multistage settling groove is not waited by width forms, and is divided into three to six sections, and bottom of gullet fills
There is slurry discharge ports；The initial segment time of staying is the 5-50 second, and water velocity is 1-3 meter per second；From the beginning of second segment, next section is stopped
Stay the time to be the preceding paragraph 2-3 times, water velocity is 1st/1st to three/2nd of the preceding paragraph.
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| CN201610173616.8A CN105833985B (en) | 2016-03-24 | 2016-03-24 | A kind of industrial solid waste residue Selective Separation and recoverying and utilizing method |
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| CN201610173616.8A CN105833985B (en) | 2016-03-24 | 2016-03-24 | A kind of industrial solid waste residue Selective Separation and recoverying and utilizing method |
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| CN109608062A (en) * | 2018-12-12 | 2019-04-12 | 盐城市国泰混凝土有限公司 | A kind of Silicon-rich magnesium nickel dreg concrete reinforcing agent and nickel slag enhance concrete material |
| CN113441287A (en) * | 2021-07-09 | 2021-09-28 | 淮北市协力重型机器有限责任公司 | System for be used for preparing concentrate |
| CN115626788A (en) * | 2021-11-24 | 2023-01-20 | 山东大学 | Device for acidifying and carbonizing modified steel slag |
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| CN105833985B (en) | 2018-05-11 |
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