CN105833985B - A kind of industrial solid waste residue Selective Separation and recoverying and utilizing method - Google Patents
A kind of industrial solid waste residue Selective Separation and recoverying and utilizing method Download PDFInfo
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- CN105833985B CN105833985B CN201610173616.8A CN201610173616A CN105833985B CN 105833985 B CN105833985 B CN 105833985B CN 201610173616 A CN201610173616 A CN 201610173616A CN 105833985 B CN105833985 B CN 105833985B
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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
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Abstract
A kind of industrial solid waste residue Selective Separation and recoverying and utilizing method, suitable for the recycling of solid slag caused by steel, metallurgy and chemical industry.The present invention is established on industrial solid waste residue microstructure system research basis, using high selectivity chemical agent, it is soaking, mill, magnetic separation, the processing step such as Multistage settling, the adhesive substance between dissolving or softening crystalline particle, realizes that heterogeneity crystalline particle space is dissociated with chemical method；Meanwhile the selection of high selectivity chemical agent sexually revises some crystalline particle surfaces characteristic, strengthens different component settling property difference, complete to separate easy to Multistage settling, so as to improve separative efficiency, energy consumption can be greatly lowered, simplify treatment process.The present invention is applicable not only to the recycling such as slag, stainless steel slag, metallurgical slag, it can also be used to which chemical industry solid slag recycles useful component or some trace element enrichments.
Description
Technical field
The invention belongs to industrial solid waste residue utilization technology field, produced suitable for steel, metallurgy and chemical industry
Raw solid slag recycles wherein useful metal and its compound.
Background technology
In the production processes such as steel, metallurgy, chemical industry, often give up with solid of the discharge largely containing metal and its oxide
Slag, such as smelts iron scum, steel slag, the slag of stainless steel industry, the metallurgical slag of nonferrous metallurgy industry of industry, on the one hand,
More containing element and its compound such as iron, nickel, chromium, manganese and minute amount of noble metal silver, beryllium in these solid slags, air storage is not only
A large amount of soils are taken, and seriously pollute Soil Surrounding and water body；On the other hand, the metal such as iron, nickel, silver, beryllium and its compound
It is important metallurgy or industrial chemicals again.Therefore, exploring industrial solid waste residue and recycling is one and significantly works.
From the point of view of the data grasped at present, above-mentioned solid waste recycles typical process as " crushing-magnetic separation-is milled-magnetic
Choosing-screening-magnetic separation-gravity separation (or flotation) ".As CN1282633A, CN1282635A, CN1390795A, CN1492058A,
CN101391457A, CN161736099A etc..See on the whole, these technologies are in energy saving, magnetisable material recycling, tailings comprehensive utilization
Aspect achieves certain achievement, but there are still significantly deficiency.Firstly, since slag, metallurgical slag have through high-temperature calcination
The characteristics of hardness is high, granularity is big, crush, grind it is difficult, it is serious to equipment attrition；Secondly, these solid wastes are mixed
Compound, crystallization is very trickle, to reach compared with high separating efficiency and the rate of recovery, granularity requirements it is very thin (generally 300 mesh with
On), it is necessary to repeatedly be crushed and ground, energy consumption is very high.Further more, during similar CN1282635A method dry process, deposit
In dust secondary pollution problem.Again, in the prior art solid slag useful component recycling only by " magnetic separation ", " gravity separation (or
Flotation) " etc. limited means, and many metals and its oxide be without magnetism, and grain particle is mutually bonded, it is difficult to thoroughly
Dissociation, so nonmagnetic metal and its oxide recovering effect are very undesirable.
Numerous studies show that most of industrial solid waste residue contains a large amount of silicates, and which part silicate is micro-
Amorphous state is presented in sight, becomes the main bridge that crystalline particle or metallic particles mutually bond in solid slag；Secondly, only
There are the metals such as iron, chromium and its partial oxide more or less to possess certain magnetism, and other compositions are mostly without magnetism, simple magnetic
Choosing recycling is difficult to reach required effect；In addition, these solid slags are in addition to metal or alloy particle, other most of materials
Crystalline particle is very trickle, and general particle diameter is more in several microns between tens microns.Further, since free CaO, MgO
Deng having a water absorption behavior, these components are exceeded in cement can cause building element to occur being broken or split in the case where exposing to the weather
Seam, threatens public and private property and user's personal safety, and therefore, there are sternly free CaO, MgO equal sizes in cement or building materials in country
Lattice requirement, must not generally be higher than 1.5%, and the solid slag such as slag is higher than 2% more.
The content of the invention
The present invention is directed to drawback existing in the prior art, on the basis of industrial solid waste residue microstructure system research
On, propose a kind of industrial solid waste residue Selective Separation and recoverying and utilizing method, make its can retain in solid slag hardness compared with
Big crystalline particle or the initial pattern of alloy agglomerated particle, and energy consumption can be greatly reduced, treatment process is reduced, realizes high selection
Property separation.
Technical scheme is as follows：
A kind of industrial solid waste residue Selective Separation and recoverying and utilizing method, it is characterized in that this method comprises the following steps：
1) mixed chemical medicament is prepared, which formed by following three classes material mixing：
Acid：10-70%
Interfacial agent：5-10%
Auxiliary agent：20-80%；
2) mixed chemical medicament, solid slag and water are mixed into slurries, are put into fermentation vat and soak, make mixing rear slurry
Solid content be 20-50wt%；Mass content of the mixed chemical medicament in slurries is 1-10%；
3) after soaking rear slurry feeding grinding mill attrition grinding, into magnetic separator；
4) after magnetic separator isolates magnetisable material, slurries flow into cone tank；
5) Multistage settling groove is entered by overflow at the top of cone tank containing short grained slurries, the slurries containing bulky grain are in taper
Trench bottom, which is enriched with and returns to grinding mill, to be continued to grind；
6) overflow slurry settles in Multistage settling groove difference section and completes separation, and clear liquid is returned as circulation fluid and soaked after sedimentation
Pond recycles；
7) after sediment exports discharge respectively by Multistage settling trench bottom, filter, dry respectively, obtain a variety of different productions
Thing.
In above-mentioned technical proposal, the acid is one kind in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid and acetic acid
Or several mixture；The interfacial agent is polyoxyethylene ether, sodium stearyl sulfonate, oleic acid, cetyl bromination
One or more of mixtures in ammonium, octadecylamine, triethanolamine, imidazoline and cationic-type polyacrylamide；The auxiliary agent
For one or more of mixtures in sodium hexametaphosphate, sodium metasilicate, sodium silicate, ethylene glycol and glycerine.
Preferably, when soaking time is 0.5-6 small in fermentation vat described in step 2).
Preferably, the magnetic separator is using multistage wet magnetic separator.
The technical characteristic of the present invention also resides in：The Multistage settling groove, the elongated sink not waited by width form, and are divided into three
To six sections, bottom of gullet is equipped with slurry discharge ports；5-50 seconds initial segment residence time, water velocity 1-3 meter per seconds；From second segment
Start, next section of residence time is 2-3 times of the preceding paragraph, and water velocity is the preceding paragraph half to 1/3rd.
The present invention has the following advantages and the technique effect of high-lighting：
The present invention is softened or is dissolved to the material between crystalline particle using the chemical agent of high selectivity first, auxiliary
Milled with stirring, realize heterogeneity crystalline particle space dissociation (most of is amorphous silicate), crushed with conventional mechanical
Grinding is compared, chemical method space dissociation particle percentage higher, and dissociation is more thorough.
Secondly, chemical method particle space dissociation remains particle primary morphology to greatest extent, eliminates attrition grinding, so that
Energy consumption (and the prior art this energy consumption typically constitute from always handling energy consumption 40-50%) is greatly reduced.In terms of recycling angle, particle
The larger metal of difference in size and its oxide have no adverse effects to recycling, as recycled steel scrap granular size difference in slag
It is very big, it is small to hundreds of microns greatly to several or even tens centimetres, but this has no effect on waste steel recycling utilization；On the other hand, it is golden
Component outside category and its oxide, crystalline particle itself is just very trickle, can be formed compared with fine powder after separation, just be suitable as water
The higher fineness requirement of mud building materials.Therefore, retain particle primary morphology in solid slag, neither influence to recycle, also reach
Energy-saving purpose.
Further more, chemical method realizes high selectivity separation.Mixed chemical pharmacy effect do not terminate in solid slag difference into
Divide the dissociation of crystalline particle space, also reside in some granular boundaries of Selective activation, strengthen heterogeneity settlement difference, for sedimentation point
From having established solid foundation.Mixed chemical medicament has different crystalline particle interfaces very strong selectivity, and interface selective is lived
Change, cause variable grain settling property similar in equal in magnitude, proportion that larger difference is presented, be conducive to by Multistage settling mode
Realize separation.Experiment shows that the present invention not only has various slags, metallurgical slag good separating effect, but also to Fluorite slag
Silver enrichment etc. also has good effect in middle calcirm-fluoride recycling, beryllium element enrichment and Zn smelting wastes.
In addition, mixed chemical medicament of the present invention has also taken into account the harmless treatment of free CaO, MgO in industrial solid waste residue,
Free CaO, MgO remaining quantities add up to no more than 1%, comply fully with the national standards such as clinker.
In short, the present invention overcomes drawbacks such as traditional handicraft high energy consumption, secondary pollution, inferior separating effects, and with extensive
Applicability, cannot be only used for steel slag and iron slag, the stainless steel slag of steel industry, be also applied for the nonferrous metallurgy solid such as Zn smelting wastes
Waste residue, it may also be used for tailings recycles after being fluorinated the fluorite flotation of work.
Brief description of the drawings
Fig. 1 is a kind of concrete technology flow process figure of industrial solid waste residue Selective Separation and recycling.
Embodiment
The present invention is described further with reference to the accompanying drawings and embodiments.
Fig. 1 is the process flow chart that the present invention proposes a kind of industrial solid waste residue Selective Separation and recoverying and utilizing method,
It specifically comprises the following steps：
1) mixed chemical medicament is prepared first：Following three classes material is mixed in proportion, i.e., by 10-70% acids,
5-10% interfacial agents and 20-80% auxiliary agents are uniformly mixed, and are configured to mixed chemical medicament, wherein the acid is
One or more of mixtures in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid and acetic acid；The interfacial agent is polyoxy second
Alkene ether, sodium stearyl sulfonate, oleic acid, cetyl ammonium bromide, octadecylamine, triethanolamine, imidazoline and cationic poly third
One or more of mixtures in acrylamide；The auxiliary agent is sodium hexametaphosphate, sodium metasilicate, sodium silicate, ethylene glycol and third
One or more of mixtures in triol.
2) mixed chemical medicament, solid slag and water are mixed into slurries, are put into fermentation vat and soak, generally in fermentation vat
When middle soaking time is 0.5-6 small；The solid content for making mixing rear slurry is 20-50wt%；Mixed chemical medicament is in slurries
Mass content is 1-10wt%；
3) after soaking rear slurry feeding grinding mill attrition grinding, into magnetic separator；The magnetic separator is using multistage wet magnetic separation
Machine；
4) after magnetic separator isolates magnetisable material, slurries flow into cone tank；
5) Multistage settling groove is entered by overflow at the top of cone tank containing short grained slurries, the slurries containing bulky grain are in taper
Trench bottom, which is enriched with and returns to grinding mill, to be continued to grind；The Multistage settling groove, the elongated sink not waited by width form, and are divided into three
To six sections, bottom of gullet is equipped with slurry discharge ports；5-50 seconds initial segment residence time, water velocity 1-3 meter per seconds；From second segment
Start, next section of residence time is 2-3 times of the preceding paragraph, and water velocity is the preceding paragraph half to 1/3rd.
6) overflow slurry settles in Multistage settling groove difference section and completes separation, and clear liquid is returned as circulation fluid and soaked after sedimentation
Pond recycles；
7) after sediment exports discharge respectively by Multistage settling trench bottom, filter, dry respectively, obtain a variety of different productions
Thing.
Embodiment 1
Weigh 50 kilograms of blast furnace slags, add 100 grams of sulfuric acid, 11 grams of cetyl ammonium bromide, sodium silicate (45 °, modulus
3.0) 100 grams, it is mixed 30 minutes, when standing 4 is small；Then rod mill is started, being passed through circulation fluid with 30 liters/min of speed (opens
Stage beginning is passed through clear water), mixed serum is continuously added to, overflowing liquid enters three-level magnetic separator, and the solid mixing magneticly elected, dehydration is dried
It is dry；Magnetic separation rear slurry enters taper overflow settler, and lower part sediment, which returns to rod mill, to be continued to grind, and upper strata overflow flows into accurate
Subsider, sedimentation channel are divided into three sections, and the residence time is respectively 10 seconds, 50 seconds and 19 minutes, total residence time 20 minutes, is sunk
Clear liquid returns to rod mill and recycles after drop.The solid slurry that three sections of water channels are deposited to bottom is drawn from bottom, is carried 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
Related national standard method carries out constituent analysis.Experimental result is as follows：
1st, experimental raw analysis result：Component content is wt%
2nd, product analysis result：Component content is WT%
Embodiment 2
50 kilograms of stainless steel smelting waste residues are weighed, add 1:1:1 nitric acid, hydrochloric acid, 100 grams of acetic acid mixture, 1:1:1 miaow
Oxazoline, oleic acid, 20 grams of triethanolamine mixed liquor, 1:1:1 sodium sulphate, sodium metasilicate, sodium silicate (45 °, modulus 3.0) mixture
100 grams, it is mixed 30 minutes, when standing 6 is small；Then rod mill is started, being passed through circulating clear liquid with 20 liters/min of speed (starts
Stage is passed through clear water), mixed serum is continuously added to, overflowing liquid enters three-level magnetic separator, and the solid mixing magneticly elected, dehydration is dried
It is dry；Magnetic separation rear slurry enters taper overflow settler, and lower part sediment, which returns to rod mill, to be continued to grind, and upper strata overflow flows into accurate
Subsider, sedimentation channel are divided into four sections, and the residence time is respectively 10 seconds, 20 seconds, 30 seconds and 19 minutes, and total residence time 20 is divided
Clock, clear liquid returns to rod mill and recycles after sedimentation.Five sections of water channels are deposited to the solid slurry of bottom and are drawn from bottom, respectively into
Row filtering and drying；After finally immersion material all adds, equipment stops after continuing to run with 30 minutes, samples weighing after drying,
Constituent analysis is carried out according to related national standard method.Experimental result is as follows：
1st, experimental raw analysis result：Component content is WT%
2nd, product analysis result：Component content is WT%
Test result indicates that metallic iron, chromium primarily enter magnetic separation product, iron and chromated oxide are mainly settled in first segment,
Nickel is settled in second segment, and manganese is settled at the 3rd section, and the 4th section is settled into silicates.
Embodiment 3
50 kilograms of metallic zinc melting waste slags are weighed, add 1:1:1 formic acid, acetic acid, 100 grams of benzoic acid mixed liquor, 1:1:1
Cetyl ammonium bromide, oleic acid, 20 grams of cationic polyacrylamide mixed liquor, 1:1:1 glycerine, sodium hexametaphosphate, flower bulb
100 grams of alkali (45 °, modulus 3.0) mixture, is mixed 30 minutes, when standing 3 is small；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-level magnetic separator, magnetic separation
The solid mixing gone out, dewatered drying；Magnetic separation rear slurry enters taper overflow settler, and lower part sediment, which returns to ball mill, to be continued to grind
Mill, upper strata overflow flow into accurate subsider, and sedimentation channel is divided into three sections, and the residence time is respectively 30 seconds, 60 seconds and 18.5 points
Clock, total residence time 20 minutes, clear liquid returns to ball mill and recycles after sedimentation.Five sections of water channels are deposited to the solid slurry of bottom
Drawn from bottom, filtered and dried respectively；After finally immersion material all adds, equipment is stopped after continuing to run with 30 minutes
Only, samples weighing after drying, constituent analysis is carried out according to related national standard method.Experimental result is as follows：
1st, experimental raw analysis result：Component content is WT%
2nd, product analysis result：Component content is WT%
Test result indicates that metallic iron primarily enters magnetic separation product, iron and chromated oxide are mainly settled in first segment, and silver exists
Second segment sedimentation enrichment, aluminium and silicate are mainly in the 3rd section of sedimentation.
Embodiment 4
50 kilograms of fluorite flotation tailings are weighed, add 1:1:1 hydrochloric acid, nitric acid, 100 grams of sulfuric acid mixture liquid, 1:1:The ten of 1
Six alkyl bromination ammoniums, octadecylamine, 20 grams of imidazoline mixed liquor, 1:1:1 ammonium fluoride, sodium hexametaphosphate, sodium silicate (45 °, modulus
3.0) 100 grams of mixture, are mixed 30 minutes, when standing 1 is small；Then start ball mill, circulation is passed through 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-level magnetic separator, and the solid magneticly elected mixes
Close, dewatered drying；Magnetic separation rear slurry enters taper overflow settler, and lower part sediment, which returns to ball mill, to be continued to grind, and upper strata is overflow
Stream flows into accurate subsider, and sedimentation channel is divided into three sections, and the residence time is respectively 60 seconds, 15 minutes and 4 minutes, when always stopping
Between 20 minutes, after sedimentation clear liquid return ball mill recycle.The solid slurry that three sections of water channels are deposited to bottom is drawn from bottom,
Filtered and dried respectively；After finally immersion material all adds, equipment stops after continuing to run with 30 minutes, sample after drying
Weigh, constituent analysis is carried out according to related national standard method.Experimental result is as follows：
1st, experimental raw analysis result：Component content is WT%
2nd, product analysis result：Component content is WT%
Test result indicates that metallic iron primarily enters magnetic separation product, calcirm-fluoride is mainly settled in first segment, and silicate is the
Two sections of sedimentations, beryllium then form enrichment at the 3rd section.
Claims (4)
1. a kind of industrial solid waste residue Selective Separation and recoverying and utilizing method, it is characterised in that this method comprises the following steps：
1) mixed chemical medicament is prepared, which formed by following three classes material mixing：
Acid：10-70%
Interfacial agent：5-10%
Auxiliary agent：20-80%；
2) mixed chemical medicament, solid slag and water are mixed into slurries, are put into fermentation vat and soak, make consolidating for mixing rear slurry
Content is 20-50wt%；Mass content of the mixed chemical medicament in slurries is 1-10wt%；
3) after soaking rear slurry feeding grinding mill attrition grinding, into magnetic separator；
4) after magnetic separator isolates magnetisable material, slurries flow into cone tank；
5) Multistage settling groove is entered by overflow at the top of cone tank containing short grained slurries, the slurries containing bulky grain are at cone tank bottom
Portion, which is enriched with and returns to grinding mill, to continue to grind；
6) overflow slurry settles in Multistage settling groove difference section and completes separation, and clear liquid returns to fermentation vat as circulation fluid and follows after sedimentation
Ring uses；
7) after sediment exports discharge respectively by Multistage settling trench bottom, filter, dry respectively, obtain a variety of different products；
The acid is one or more of mixtures in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid and acetic acid；It is described
Interfacial agent for polyoxyethylene ether, sodium stearyl sulfonate, oleic acid, cetyl ammonium bromide, octadecylamine, triethanolamine,
One or more of mixtures in imidazoline and cationic-type polyacrylamide；The auxiliary agent is sodium hexametaphosphate, metasilicic acid
One or more of mixtures in sodium, sodium silicate, ethylene glycol and glycerine.
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：Step
It is rapid 2) in the fermentation vat soaking time for 0.5-6 it is small when.
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 magnetic separator stated is using multistage wet magnetic separator.
4. a kind of industrial solid waste residue Selective Separation and recoverying and utilizing method, its feature as described in claim 1,2 or 3 exist
In：The Multistage settling groove is made of the elongated sink that width does not wait, and is divided into three to six sections, bottom of gullet is discharged equipped with slurries
Mouthful；The initial segment residence time is 5-50 seconds, and water velocity is 1-3 meter per seconds；Since second segment, next section of residence time is upper
2-3 times of one section, water velocity for the preceding paragraph half to 1/3rd.
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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 |
| CN113441287B (en) * | 2021-07-09 | 2022-12-09 | 淮北市协力重型机器有限责任公司 | Method for preparing concentrate |
| CN113929334B (en) * | 2021-11-24 | 2022-05-27 | 山东大学 | Process for modifying steel slag by coupling acidification and carbonization |
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| US20140262968A1 (en) * | 2013-03-15 | 2014-09-18 | Fritz Enterprises, Inc. | System and method for recovery of valuable constituents from steel-making slag fines |
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| CN101342512A (en) * | 2007-07-12 | 2009-01-14 | 南京板桥钢渣有限责任公司 | Steel scoria processing method |
| TW201036718A (en) * | 2009-04-02 | 2010-10-16 | Atomic Energy Council | Method for recovering gold, silver, copper and iron from valuable metal-containing plasma-caused slag |
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