CN109811132A - A method of comprehensive reutilization carbon, iron, aluminium, zinc, lead from blast furnace gas mud - Google Patents
A method of comprehensive reutilization carbon, iron, aluminium, zinc, lead from blast furnace gas mud Download PDFInfo
- Publication number
- CN109811132A CN109811132A CN201910126563.8A CN201910126563A CN109811132A CN 109811132 A CN109811132 A CN 109811132A CN 201910126563 A CN201910126563 A CN 201910126563A CN 109811132 A CN109811132 A CN 109811132A
- Authority
- CN
- China
- Prior art keywords
- carbon
- zinc
- aluminium
- lead
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The method of the invention discloses a kind of from blast furnace gas mud comprehensive reutilization carbon, iron, zinc, aluminium, lead, first dry, the broken, grinding by blast furnace gas mud, multistage flotation, pickling filter recycling carbon;Acidleach will be carried out through carbon tailing after the recovery, be aoxidized, be filtered to get filtrate and filter residue;Then gained filtrate pH value is adjusted, fractional precipitation goes out iron hydroxide, zinc hydroxide and aluminium hydroxide, and carries out roasting to obtain iron ore concentrate, zinc concentrate and aluminium concentrate respectively;Saturated acetic acid ammonium salt solution is added in filter residue after filtration, sodium carbonate liquor is added into filtrate for agitation and filtration, filters to obtain basic lead carbonate precipitating, and roast to obtain lead concentrate.Recovery process of the present invention is easy to operate, can carbon, iron, zinc, aluminium, lead in synthetical recovery gas mud, realize that the renewable resources of a variety of valuable elements recycle, and reduce the pollution to environment, there is important economy and environmental benefit, be suitble to promote and apply.
Description
Technical field
The invention belongs to metallurgical solid waste renewable resources to utilize field, be related to a variety of valuable elements in a kind of blast furnace gas mud
Comprehensive reutilization method, and in particular to a method of comprehensive reutilization carbon, iron, aluminium, zinc, lead from blast furnace gas mud.
Background technique
Blast furnace gas mud is carried out by high-temperature region, reaction is generated in steel smelting procedure microfine and blast furnace gas
Raw material dust, through the obtained product of wet dust removal washing precipitation concentration, main component is that carbon, iron, zinc and content are opposite
More aluminium, lead etc. is valuable or poisoning metal element.Currently, it is more than 5,000,000 tons that China about produces blast furnace gas mud every year, conduct is removed
Solid waste stockpiling is outer, is used generally as Sintering Blend.Since gas mud granularity is very thin, can reduce during the sintering process
The gas permeability of sinter bed influences to be sintered efficiency.The Volatile Elements such as metallic zinc, lead in gas mud recycle in blast furnace simultaneously
Enrichment causes upper blast furnace dross and gas piping to block, to influence the normal operation of blast furnace.
Carbon, iron contained in blast furnace gas mud, zinc, aluminium, lead etc. are all very important the raw material of industry, such as without reasonable
Recycling, be not only the significant wastage to resource, meanwhile, if not being pocessed directly stacking, landfill or only simple
Ground is used as roadbed material, and the heavy metal element in gas mud can also cause serious pollution to environment.Therefore, synthetical recovery blast furnace
The valuable metals elements such as carbon and iron, zinc, aluminium, lead in gas mud, the renewable resources for being both able to achieve metallurgical solid waste utilize, can also subtract
Few environmental pollution, realizes the greenization sustainable development of industry.
Mainly pass through physics and chemical method recycles carbon, iron, zinc to gas mud comprehensive reutilization from gas mud at present:
Chinese patent (publication number CN105063254B) " a method of separation blast furnace gas mud in iron zinc carbon " is by by gas mud magnetic
Magnetic separation of iron ore concentrate and zinc-rich tailing after changing roasting, aoxidizing obtain zinc-rich liquid and carbon by leaching, being separated by solid-liquid separation to zinc-rich material
Powder realizes the synthetical recovery of carbon in gas mud, iron, zinc;A kind of Chinese patent (publication number CN106119557B) " blast furnace gas
The method of zinc, iron, carbon synthetical recovery in mud " utilizes sulfuric acid dissolution gas mud, and filtered filtrate passes through oxidation, neutralization, filtering
Obtain scum;Except the filtrate electrodeposition after iron obtains electric zinc;The scum mixing magnetizing roast dissolving the filter residue of gas mud and filtering obtains iron
Concentrate;Tailing flotation recovery carbon therein again.However, both methods utilizes in gas mud certainly in the separation process of iron ore concentrate
Iron oxide is converted magnetic iron ore by some reducing agent carbon, consumes the carbon in gas mud, releases carbon monoxide and carbon dioxide
Gas, therefore the recycling of carbon in gas mud is reduced, the discharge of greenhouse gases is increased, there is certain destruction to environment;
Further, since there are the carbon dust of a large amount of fine sizes to micro-nano-scale in gas mud, when magnetic separation, is difficult to separate it with magnetic iron ore
It opens, causes the reduction of iron concentrate grade;Meanwhile also containing the relatively large number of valuable metal element aluminum of content and toxic in gas mud
Metallic element lead is both a kind of waste of resource, also will increase the pollution to environment if do not recycled.
Summary of the invention
It is a primary object of the present invention to the low, iron concentrate grades for the blast furnace gas peat rate of recovery of the existing technology
It is not high, be difficult to recycle aluminium and lead, easily cause the problems such as environmental pollution, provide one kind from blast furnace gas mud comprehensive reutilization
The method of carbon, iron, zinc, aluminium and lead, the synchronous high efficiente callback for realizing blast furnace gas mud fixed-end forces process utilizes and low pollution is arranged
It puts, takes into account economy and environmental benefit.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A method of comprehensive reutilization carbon, iron, zinc, aluminium and lead from blast furnace gas mud, first with flotation-acid
- suction method recycling carbon is washed, recycles step-by-step precipitation method successively to recycle iron, zinc, aluminium, lead element, specifically comprises the following steps:
1) blast furnace gas mud is dried, milled, add water and stir into ore pulp, adjust the pH value of gained ore pulp, addition is caught
Agent, foaming agent are received, flotation collecting carbon slurry is carried out, filters, dry carbon mine I, pickling, then filter, obtains carbon mine II;
2) tailing obtained by step 1) flotation filtered, dried, acidleach, with hydrogen peroxide oxidation, filtering obtains filtrate respectively
I and filter residue I;
3) sodium hydroxide solution adjusting pH value is added into filtrate I obtained by step 2) and carries out heavy iron, controls temperature, promotes life
At ferric hydroxide precipitate, filtering obtains filtrate II and filter residue II;Gained filter residue II is carried out washing to obtain scum, roasts to obtain iron ore concentrate;
4) sodium hydroxide solution adjusting pH value is continuously added into filtrate II obtained by step 3) and carries out heavy zinc, and filtering must filter
Liquid III and filter residue III;Gained filter residue III is washed, cadmia is obtained, then roasts to obtain zinc concentrate;
5) dilute sulfuric acid is added into filtrate II I obtained by step 4) and adjusts the heavy aluminium of pH value, filters and simultaneously precipitating is repeatedly washed
It washs, obtains cadmia, then roast to obtain aluminium concentrate;
6) filter residue I obtained by step 2) filtered, dried, saturated acetic acid ammonium salt solution, stirring, filtering, in filtrate is added
Middle addition sodium carbonate liquor adjusts the heavy lead of pH value;It filters and precipitating is washed, obtain lead skim, then roast to obtain lead concentrate.
In above scheme, the granularity of gas ash described in step 1) is less than 0.1 μm.
In above scheme, for the collecting agent used in step 1) for diesel oil, foaming agent is 2# oil.
In above scheme, pulp density described in step 1) is 4~6%, and pH value is 10~13.
In above scheme, in floatation process described in step 1), collecting agent is 6~8wt% with respect to the dosage of gas mud;It rises
Dosage 3~4wt% of the infusion with respect to gas mud.
Preferably, the floatation process includes one roughing, triple cleaning;The pickling of carbon mine I uses dilute sulfuric acid, matter
Measuring concentration is 20~25%, and the mass ratio of dilute sulfuric acid and carbon mine I are (5~10): 1.
In above scheme, step of acid dipping described in step 2) uses dilute sulfuric acid, and mass concentration is 20~25%;Acid with watt
This mud mass ratio is (12~13): 1;The volume ratio of hydrogen peroxide and dilute sulfuric acid be 1:(1.2~1.3), hydrogen peroxide concentration be 25~
35%;;The temperature that acidleach uses is controlled at 60~70 DEG C.
Preferably, acidleach, hydrogen peroxide oxidation step are that after tailing obtained by flotation is filtered, dried, dilute sulphur is added
Acid, hydrogen peroxide react 0.5~1h at a temperature of stirring condition and 60~70 DEG C.
In above scheme, pH value described in step 3) is 2.3~4.0, and controlled at 65~70 DEG C, maturing temperature is
850~880 DEG C, calcining time is no less than 2h.
In above scheme, pH value described in step 4) is 8.0~10.5, and maturing temperature is 125~150 DEG C, calcining time
No less than 2h.
In above scheme, pH value described in step 5) is 5.2~7.8, and maturing temperature is 450~470 DEG C, and calcining time is
No less than 2h.
In above scheme, the mass ratio of saturated acetic acid ammonium salt solution described in step 6) and filter residue I are (3~4): 1;The carbon
The concentration of acid sodium solution is 1.0~1.5mol/L.
In above scheme, pH value described in step 6) is 7.2~8.7, and maturing temperature is 420~450 DEG C, and calcining time is
No less than 2h.
The principle of the present invention are as follows:
The present invention uses floatation process, high efficiente callback carbon mine, and combines pickling-suction filtration technique, further removes carbon
Mixed metal oxide impurities in mine can effectively reduce the medicines such as hydrogen peroxide in acidleach oxidation process to improve carbon concentrate grade
Product dosage reduces process costs, and advantageously ensures that the rate of recovery and grade of subsequent iron;Then by tailing obtained by flotation in water-bath
Under conditions of temperature is 60~70 DEG C, valuable metal is dissolved into metal cation using acidleach, and utilize hydrogen peroxide by gas
Ferrous ion in mud is converted to ferric ion, zinc sulphide is oxidized to soluble zinc sulfate, it is insoluble to be oxidized to vulcanized lead
Lead sulfate, filtering the metal cation in addition to lead is separated with insoluble impurity;It will be in insoluble impurity using saturated acetic acid ammonium
Lead sulfate be dissolved into lead acetate;Precipitating pH range is generated not further according to iron, zinc, the hydroxide of aluminium and basic lead carbonate
Together, extract that iron, zinc, aluminium, lead etc. is valuable or harmful metal elements respectively by fractional precipitation;Wherein, it is precipitated due to aluminium and zinc
PH is closer to, and the precipitating pH range of aluminium is relatively narrow, therefore reversed adjusting method is taken to realize the separation of aluminium and zinc, effectively avoids passing
Uniting, pH adjusting method serious forgiveness is low, product recoveries and the problems such as purity lower (easily adulterating zinc etc. in aluminium);It is final to realize gas
Carbon, iron, zinc, aluminium, the efficient of lead, comprehensive reutilization and harmless treatment in mud.
Compared with prior art, the invention has the benefit that
1) compared with existing blast furnace gas mud processing method, this method carries out the recycling of carbon first, avoids acidleach oxidation
The problems such as carbon is consumed by hydrogen peroxide in the process, can effectively promote the rate of recovery and grade of carbon in blast furnace gas mud, iron, and reduce
Processing cost is saved in the consumption of hydrogen peroxide.
2) it further realizes the recycling of zinc, aluminium and lead and preferably avoids tradition especially in the recycling to aluminum and zinc
The problems such as serious forgiveness of pH adjusting method is low, can operating space it is bigger, it is more efficient, it is more convenient, the life of enterprise is effectively reduced
The business efficiency for producing cost, increasing enterprise is better achieved valuable, harmful element recycling in metallurgical solid waste and recycles.
3) it can effectively avoid and utilize pollution of the heavy metals in process element to environment in stockpiling or low value because of blast furnace gas mud,
With important economy and environmental benefit.
Detailed description of the invention
Fig. 1 is the process flow of the comprehensive reutilization method of a variety of valuable elements in blast furnace gas mud described in embodiment 1
Figure.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
The comprehensive reutilization method of a variety of valuable elements, process flow chart are shown in Fig. 1 in a kind of blast furnace gas mud, specifically
Include the following steps:
1) blast furnace gas mud is put into drying box, the dry 36h at 120 DEG C grinds 2h with planetary ball mill, it is small to obtain granularity
In 0.1 μm of gas ash;
2) add water to make pulp density 6wt% gas ash obtained by step 1), stir evenly, be added and catch into gained slurry
(collecting agent is 7wt% with respect to the dosage of gas mud for receipts agent diesel oil and foaming agent 2# oil;Foaming agent is with respect to the dosage of gas mud
The pH value of quick lime adjusting gained slurry 4wt%) is then added to 11, carries out one roughing triple cleaning and collects carbon slurry and tail
Mine;24 hours dry at 120 DEG C after the carbon slurry of collection is filtered, the mass concentration that 5 times of carbon mineral amounts are then added is
The dilute sulfuric acid of 20wt% carries out pickling, obtains carbon mine after suction filtration;
3) tailing obtained by step 1) flotation is filtered, it is 24 hours dry at 120 DEG C, it is then charged into beaker, is added
The mass concentration of 12 times of gas mud quality is the dilute sulfuric acid of 20wt%, and being then added with sulfuric acid volume ratio is 1:1.2's
The hydrogen peroxide of 30wt%, beaker is put into thermostat water bath, controls 60 DEG C of bath temperature, electric mixer revolving speed 150r/
Min, while acidleach, oxidation, reaction time 1h are carried out, filtering obtains filtrate I and filter residue I respectively;
4) dropwise addition sodium hydroxide solution adjusting pH value is (no controlled at 70 DEG C to 4.0 in the filtrate I obtained by step 3)
Then have ferric hydroxide colloid generation, it is difficult to be separated off, be affected to result quality is extracted), promote generation iron hydroxide heavy
It forms sediment;Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed, obtains filter residue II (scum) and filtrate II;Scum is put into
Muffle furnace roasts 2 hours at 850 DEG C, obtains iron ore concentrate;
5) sodium hydroxide is added dropwise into filtrate II obtained by step 4) and adjusts pH value to 10.0, promotes generation zinc hydroxide heavy
It forms sediment;Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed, obtains filtrate II I and filter residue III (cadmia);Cadmia is put
Enter Muffle furnace, is roasted 2 hours at 150 DEG C, obtain zinc concentrate;
6) dilute sulfuric acid is added into filtrate II I obtained by step 5) and adjusts pH value to 7.0, promotes to generate aluminum hydroxide precipitation;
Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed using decantation, collects gained filter residue (aluminium slag) and filter
Liquid IV;Cadmia is put into Muffle furnace, is roasted 2 hours at 450 DEG C, obtains aluminium concentrate;
7) filter residue I obtained by step 3) filtered, dried, saturated acetic acid ammonium salt solution, ammonium acetate solution and filter residue I is added
Mass ratio be 4:1, be stirred, filter, then into filtrate be added concentration be 1mol/L sodium carbonate liquor, adjust pH value to
8.2, promote to generate basic lead carbonate precipitating;10 minutes are stood, filter and precipitating is repeatedly washed using decantation, obtains lead
Slag and filtrate V;Lead skim is put into Muffle furnace, is roasted 2 hours at 420 DEG C, obtains lead concentrate;
8) merge filtrate V obtained by filtrate IV obtained by step 6) and step 7), the dilute sulfuric acid of mass concentration 20~25% be added dropwise,
Adjust pH value makes to be in neutrality to 7.0, or directly return step 3) it is used as leaching agent.
In the present embodiment, the blast furnace gas mud of use is provided by Hubei steel plant;ICP constituent analysis shows the blast furnace
Contained element includes carbon, iron, zinc, aluminium, silicon, sulphur, calcium, potassium, sodium, lead etc. in gas mud;XRD material phase analysis shows the high tile
Zinc and lead mainly exist in the form of zinc sulphide and vulcanized lead in this mud;Mainly recyclable valuable constituent is shown in Table 1.
Valuable constituent information mainly recyclable in 1 Hubei steel plant blast furnace gas mud of table
Ingredient | C | TFe | ZnO | Al2O3 | PbO |
Content (wt%) | 51.025 | 15.902 | 7.99 | 4.171 | 1.544 |
After tested, using recovery process described in the present embodiment, the rate of recovery of carbon is 89.5% in blast furnace gas mud;Iron recycling
Rate is 76.8%;Zinc recovery is 89.4%;Aluminium recovery is 76.1%;Lead recovery is 72.1%;By further ingredient
Analysis is as a result, the carbon purity recycled is 89.2%;Iron purity is 88.7%;Zinc purity is 92.4%;Aluminium purity is 84.4%;
Lead purity be 77.4%, it can be achieved that carbon, iron, zinc, aluminium and lead high efficiente callback, and purity is preferable.
Embodiment 2
The comprehensive reutilization method of a variety of valuable elements, specifically comprises the following steps: in a kind of blast furnace gas mud
1) blast furnace gas mud is put into drying box, the dry 36h at 120 DEG C grinds 2h with planetary ball mill, it is small to obtain granularity
In 0.1 μm of gas ash;
2) add water to make pulp density 6% gas ash obtained by step 1), stir evenly, collecting is added into gained slurry
Agent diesel oil and foaming agent 2# oil, collecting agent are mass fraction 7% with respect to the dosage of gas mud;Dosage of the foaming agent with respect to gas mud
For mass fraction 4%.Then the pH value of quick lime adjusting gained slurry is added to 12, carries out one roughing triple cleaning and collects carbon
Slurry and tailing;It is 24 hours dry at 120 DEG C after the carbon slurry of collection is filtered, the quality of 5 times of carbon mineral amounts is then added
The dilute sulfuric acid that concentration is 20wt% carries out pickling, obtains to obtain carbon mine after suction filtration;
3) tailing obtained by step 1) flotation is filtered, it is 24 hours dry at 120 DEG C, it is then charged into beaker, is added
The concentration of 12 times of gas ash quality is the 30wt% that the dilute sulfuric acid of 25wt%, then addition and sulfuric acid volume ratio are 1:1.3
Beaker is put into thermostat water bath by hydrogen peroxide, 65 DEG C of bath temperature, electric mixer revolving speed 150r/min of control, while into
Row acidleach, oxidation, reaction time 1h, filtering obtain filtrate I and filter residue I respectively;
4) sodium hydroxide is added dropwise in the filtrate I obtained by step 2) and adjusts pH value to 3.6, controlled at 70 DEG C, promotes life
At ferric hydroxide precipitate;Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed, obtains filter residue II (scum) and filtrate
II;Scum is put into Muffle furnace, is roasted 1 hour at 880 DEG C, obtains iron ore concentrate;
5) sodium hydroxide is added dropwise into filtrate II obtained by step 4) and adjusts pH value to 10.2, promotes generation zinc hydroxide heavy
It forms sediment;Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed, obtains filtrate II I and filter residue III (cadmia);Cadmia is put
Enter Muffle furnace, is roasted 2 hours at 150 DEG C, obtain zinc concentrate;
6) dilute sulfuric acid is added into filtrate II I obtained by step 5) and adjusts pH value to 6.7, promotes to generate aluminum hydroxide precipitation;
Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed using decantation, collects gained filter residue (aluminium slag) and filter
Liquid IV;Cadmia is put into Muffle furnace, is roasted 2 hours at 470 DEG C, obtains aluminium concentrate;
7) filter residue I obtained by step 3) filtered, dried, pour into saturated acetic acid ammonium salt solution, ammonium acetate solution and filter residue I
Mass ratio be 4:1, be stirred, filter, then into filtrate be added concentration be 1mol/L sodium carbonate liquor, adjust pH value to
8.0, promote to generate basic lead carbonate precipitating;10 minutes are stood, filter and precipitating is repeatedly washed using decantation, obtains lead
Slag and filtrate V;Lead skim is put into Muffle furnace, is roasted 1 hour at 450 DEG C, obtains lead concentrate.
8) merge filtrate V obtained by filtrate IV obtained by step 6) and step 7), the dilute sulfuric acid of mass concentration 20~25% be added dropwise,
Adjust pH value makes to be in neutrality to 7.0, or directly return step 3) it is used as leaching agent.
In the present embodiment, the blast furnace gas mud of use is provided by Hubei steel plant;ICP constituent analysis shows the blast furnace
Contained element includes carbon, iron, zinc, aluminium, silicon, sulphur, calcium, potassium, sodium, lead etc. in gas mud;XRD material phase analysis shows the high tile
Zinc and lead mainly exist in the form of zinc sulphide and vulcanized lead in this mud;Mainly recyclable valuable constituent is shown in Table 2.
Valuable constituent information mainly recyclable in 2 Hubei steel plant blast furnace gas mud of table
Ingredient | C | TFe | ZnO | Al2O3 | PbO |
Content (wt%) | 43.663 | 16.741 | 5.844 | 5.674 | 1.417 |
After tested, using recovery process described in the present embodiment, the rate of recovery of carbon is 86.3% in blast furnace gas mud;Iron recycling
Rate is 80.2%;Zinc recovery is 88.1%;Aluminium recovery is 79.2%;Lead recovery is 70.4%;By further ingredient
Analysis is as a result, the carbon grade recycled is 88.7%;Iron purity is 86.5%;Zinc purity is 90.6%;Aluminium purity is 81.6%;
Lead purity be 80.1%, it can be achieved that carbon, iron, zinc, aluminium and lead high efficiente callback, and grade is preferable.
Comparative example 1
A method of a variety of valuable elements of synthetical recovery from blast furnace gas mud, the blast furnace gas used with embodiment 1
Mud is sample, is specifically comprised the following steps:
1) blast furnace gas mud is put into drying box, the dry 36h at 120 DEG C grinds 2h with planetary ball mill, obtains granularity
Gas ash less than 0.1um;
2) gas ash for obtaining step 1), which adds water and stirs, makes pulp density 6%, and diesel oil is added as collecting agent, is added
As foaming agent, (collecting agent is 7wt% with respect to the dosage of gas mud to 2# oil;Foaming agent is 4wt% with respect to the dosage of gas mud),
Quick lime is added, adjusting pH is 10, by one roughing primary cleaning, collects carbon slurry and tailing;After the carbon slurry of collection is filtered
It is 24 hours dry at 120 DEG C, obtain carbon mine;
3) the remaining tailing of step 1) is filtered, it is 24 hours dry at 120 DEG C, it is then charged into beaker, is added 5 times watts
The dilute sulfuric acid that the concentration of this grey volume is 20% is added the hydrogen peroxide with the 30wt% that sulfuric acid volume ratio is 1:30, beaker is put
Entering in thermostat water bath, controls 60 DEG C of bath temperature, electric mixer revolving speed 150r/min, acidleach, oxidation 30min are filtered, point
It Bao Cun not filtrate and filter residue;
4) ammonium hydroxide is added dropwise in the filtrate made from step 3), adjusts pH value to 4.0, makes to generate hydrogen-oxygen controlled at 70 DEG C
Change iron to precipitate, remove beaker, stand 10 minutes, filter and precipitating is repeatedly washed, obtains scum and except liquid after iron;Scum is put into
Muffle furnace roasts 2 hours at 850 DEG C, obtains iron ore concentrate;
5) continue that ammonium hydroxide is added dropwise in the filtrate after step 4) iron removal by filtration, adjust pH value to 4.8, make to generate aluminium hydroxide
Precipitating;Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed, obtains aluminium slag and except liquid after aluminium;Aluminium slag is put into Muffle
Furnace roasts 2 hours at 450 DEG C, obtains aluminium concentrate;
6) sodium hydroxide is added in the filtrate that step 5) crosses after filtering out aluminium, adjusts pH value to 8.0, makes to generate zinc hydroxide
Precipitating;Beaker is removed, stands 10 minutes, filter and precipitating is repeatedly washed using decantation, obtains cadmia and except liquid after zinc.
Cadmia is put into Muffle furnace, is roasted 2 hours at 125 DEG C, obtains zinc concentrate;
7) filter residue for obtaining step 3) is filtered, is dried, and pours into saturated acetic acid ammonium salt solution, ammonium acetate solution and filter residue
The mass ratio of I is 4:1, and stirring is filtered, the sodium carbonate liquor that addition concentration is 1mol/L in filtrate, adjusting pH value to 8.3,
Generate basic lead carbonate precipitating;10 minutes are stood, filter and precipitating is repeatedly washed using decantation, obtains lead skim and except lead
Liquid afterwards;Lead skim is put into Muffle furnace, is roasted 2 hours at 420 DEG C, obtains lead concentrate;
8) filtrate and step 7) that merging step 6) is crossed after filtering out zinc, which are crossed, filters out the filtrate after lead, and the dilute of 15-20% is added dropwise
Sulfuric acid, adjust pH value makes to be in neutrality to 6.5-7.0, or directly return step 3) it is used as leaching agent.
After tested, using recovery process described in the present embodiment, the rate of recovery of carbon is 82.5% in blast furnace gas mud;Iron recycling
Rate is 68.3%;Zinc recovery is 86.1%;Aluminium recovery is 81.2%;Lead recovery is 70.%;By further ingredient point
Analysis as a result, the carbon grade recycled is 81.3%, in carbon containing 10.2% iron;Iron purity is 81.2%;Zinc purity is
85.6%, in zinc containing 3.3% iron;Aluminium purity is 70.7%, contains 4.7% iron and 5.1% zinc in aluminium;Lead purity is
73.1%.Compared with Example 1, carbon, iron, the rate of recovery of aluminium and purity have obvious decline, the rate of recovery and concentration of zinc
Deng also there is certain downward trend.
Each raw material cited by the present invention can realize that the bound value of the present invention and each raw material, interval value can
Realize the present invention;Embodiment numerous to list herein.The bound value of technological parameter of the invention, interval value can realize this
Invention, embodiment numerous to list herein.
Claims (10)
1. a kind of method of comprehensive reutilization carbon, iron, zinc, aluminium, lead from blast furnace gas mud, which is characterized in that first with
Flotation-pickling-suction method recycles carbon, and step-by-step precipitation method is recycled successively to recycle iron, zinc, aluminium, lead element.
2. the method according to claim 1, wherein the flotation-pickling-suction method include the following steps: by
Blast furnace gas mud carries out flotation and obtains carbon mine I and tailing, and carbon mine I is then carried out pickling, filters to obtain carbon mine II.
3. according to the method described in claim 2, it is characterized in that, the flotation step includes: to do blast furnace gas mud
It is dry, mill, add water and stir and ore pulp be made, adjust gained ore pulp pH value, be added collecting agent, foaming agent, carry out direct flotation obtain carbon
Slurry and tailing collect gained carbon slurry, are filtered, dry to obtain carbon mine I.
4. according to the method described in claim 3, foaming agent is 2# oil it is characterized in that, the collecting agent used is diesel oil;Ore pulp
Concentration is 4~6wt%, and pH value is 10~13.
5. according to the method described in claim 3, it is characterized in that, collecting agent is with respect to blast furnace gas in the direct floatation process
The dosage of mud is 6~8wt%;Dosage 3~4wt% of the foaming agent with respect to blast furnace gas mud.
6. according to the method described in claim 3, it is characterized in that, the direct floatation process includes roughing and concentration step;Carbon
The acid pickling step of concentrate I uses dilute sulfuric acid, and mass concentration is 20~25%, the mass ratio of dilute sulfuric acid and carbon mine I be (5~
10):1。
7. according to the method described in claim 2, it is characterized in that, the step-by-step precipitation method includes the following steps:
1) tailing filtered, dried, acidleach, with hydrogen peroxide oxidation, filter to get filtrate I and filter residue I;
2) sodium hydroxide solution adjusting pH value is added into filtrate I obtained by step 1) and carries out heavy iron, it is heavy that control temperature promotes to generate
It forms sediment, filtering obtains filtrate II and filter residue II;Gained filter residue II is washed, scum is obtained, then roasts to obtain iron ore concentrate;
3) sodium hydroxide solution adjusting pH value is continuously added into filtrate II obtained by step 2) and carries out heavy zinc, and filtering obtains filtrate II I
With filter residue III;Gained filter residue III is washed, cadmia is obtained, then roasts to obtain zinc concentrate;
4) dilute sulfuric acid is added into filtrate II I obtained by step 3) and adjusts the heavy aluminium of pH value, filtering and repeatedly washing precipitating obtain aluminium slag,
Aluminium concentrate is roasted to obtain again;
5) filter residue I obtained by step 1) filtered, dried, saturated acetic acid ammonium salt solution is added, stirring, filtering add in filtrate
Enter sodium carbonate liquor and adjusts the heavy lead of pH value;Precipitating is filtered and washed, lead skim is obtained, then roasts to obtain lead concentrate.
8. the method according to the description of claim 7 is characterized in that step of acid dipping described in step 1) uses dilute sulfuric acid, matter
Measuring concentration is 20~25%, and the mass ratio of dilute sulfuric acid and blast furnace gas mud is (12~13): 1;The volume of hydrogen peroxide and dilute sulfuric acid
Than for 1:(1.2~1.3);The temperature that acidleach uses is 60~70 DEG C.
9. the method according to the description of claim 7 is characterized in that controlled at 65~70 DEG C in step 2), the pH value
It is 2.3~4.0;PH value described in step 3) is 8.0~10.5;PH value described in step 4) is 5.2~7.8.
10. the method according to the description of claim 7 is characterized in that the quality of ammonium acetate solution described in step 5) and filter residue I
Than for (3~4): 1;The pH value is 7.2~8.7.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910126563.8A CN109811132B (en) | 2019-02-20 | 2019-02-20 | Method for comprehensively recycling carbon, iron, aluminum, zinc and lead from blast furnace gas mud |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910126563.8A CN109811132B (en) | 2019-02-20 | 2019-02-20 | Method for comprehensively recycling carbon, iron, aluminum, zinc and lead from blast furnace gas mud |
Publications (2)
Publication Number | Publication Date |
---|---|
CN109811132A true CN109811132A (en) | 2019-05-28 |
CN109811132B CN109811132B (en) | 2020-10-30 |
Family
ID=66607009
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910126563.8A Active CN109811132B (en) | 2019-02-20 | 2019-02-20 | Method for comprehensively recycling carbon, iron, aluminum, zinc and lead from blast furnace gas mud |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109811132B (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110257640A (en) * | 2019-07-25 | 2019-09-20 | 广东省资源综合利用研究所 | A kind of method that wiring board burns cigarette ash comprehensive reutilization |
CN111135957A (en) * | 2020-01-13 | 2020-05-12 | 中国科学院地球化学研究所 | Method for recovering carbon from barium slag through flotation |
CN112958275A (en) * | 2021-02-03 | 2021-06-15 | 许泽胜 | Method for flotation of coal from coal-containing casting dust |
CN113308607A (en) * | 2021-04-22 | 2021-08-27 | 昆明理工大学 | Method for enhancing zinc oxide smoke dust leaching by ultrasonic waves and hydrogen peroxide |
CN114314638A (en) * | 2021-12-29 | 2022-04-12 | 阜新成泰环保科技有限公司 | Process for producing glaze-grade zinc oxide by using blast furnace gas ash |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5235703A (en) * | 1975-09-17 | 1977-03-18 | Nippon Steel Corp | Method of treating carbon powder containing metals |
CN1908207A (en) * | 2006-08-18 | 2007-02-07 | 昆明理工大学 | Method of comprehensive utilizing iron making blast furnace dust resources |
CN106119557A (en) * | 2016-06-30 | 2016-11-16 | 昆明理工大学 | Zinc, ferrum, the method for carbon synthetical recovery in a kind of blast furnace gas mud |
-
2019
- 2019-02-20 CN CN201910126563.8A patent/CN109811132B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5235703A (en) * | 1975-09-17 | 1977-03-18 | Nippon Steel Corp | Method of treating carbon powder containing metals |
CN1908207A (en) * | 2006-08-18 | 2007-02-07 | 昆明理工大学 | Method of comprehensive utilizing iron making blast furnace dust resources |
CN106119557A (en) * | 2016-06-30 | 2016-11-16 | 昆明理工大学 | Zinc, ferrum, the method for carbon synthetical recovery in a kind of blast furnace gas mud |
Non-Patent Citations (1)
Title |
---|
林勇: "炼铁除尘灰与炼钢污泥的综合利用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110257640A (en) * | 2019-07-25 | 2019-09-20 | 广东省资源综合利用研究所 | A kind of method that wiring board burns cigarette ash comprehensive reutilization |
CN111135957A (en) * | 2020-01-13 | 2020-05-12 | 中国科学院地球化学研究所 | Method for recovering carbon from barium slag through flotation |
CN112958275A (en) * | 2021-02-03 | 2021-06-15 | 许泽胜 | Method for flotation of coal from coal-containing casting dust |
CN113308607A (en) * | 2021-04-22 | 2021-08-27 | 昆明理工大学 | Method for enhancing zinc oxide smoke dust leaching by ultrasonic waves and hydrogen peroxide |
CN114314638A (en) * | 2021-12-29 | 2022-04-12 | 阜新成泰环保科技有限公司 | Process for producing glaze-grade zinc oxide by using blast furnace gas ash |
CN114314638B (en) * | 2021-12-29 | 2024-03-01 | 阜新成泰环保科技有限公司 | Process for producing glaze-grade zinc oxide by using blast furnace gas ash |
Also Published As
Publication number | Publication date |
---|---|
CN109811132B (en) | 2020-10-30 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109811132A (en) | A method of comprehensive reutilization carbon, iron, aluminium, zinc, lead from blast furnace gas mud | |
CN101845562B (en) | Improved device and method for producing electrolytic manganese metal by two-ore method | |
CN103540765B (en) | Zinc smelting technology | |
CN106868307B (en) | A kind of comprehensive utilization process of pyrite cinder arsenic removal enrichment gold and silver | |
US11293076B2 (en) | Method for preparing iron ore concentrates by recycling copper slag tailings | |
CN103740945B (en) | A kind of method of enriching and recovering cadmium from plumbous smelting system | |
CN101871046A (en) | Method for recycling heavy metal pollution wastes | |
WO2020019919A1 (en) | Method for homogeneous precipitation separation of iron and aluminum from laterite nickel ore acid leaching solution | |
CN111647754A (en) | Comprehensive utilization method of zinc-containing dust and sludge in steel plant | |
CN109706312A (en) | A method of vanadic anhydride and chemical electrode manganese dioxide are prepared simultaneously using vanadium chromium slag and low-grade pyrolusite | |
CN112760487A (en) | Method for recovering manganese and lead from electrolytic manganese anode slag | |
CN103184334A (en) | Selection-smelting combined technology for treating mixed ore containing molybdenum, oxygen, sulfur and copper | |
CN105110300B (en) | The method that a kind of compound manganese ore of Containing Sulfur manganese extracts manganese and sulphur | |
CN103205772B (en) | Method for producing electrolytic manganese dioxide | |
CN108866337B (en) | A method of processing metal sludge | |
CN105671324A (en) | Method for preparing ammonium rhenate from rhenium-enriched slags | |
CN106119557A (en) | Zinc, ferrum, the method for carbon synthetical recovery in a kind of blast furnace gas mud | |
CN108624910A (en) | A kind of zinc Whote-wet method smelting process method of energy-saving and emission-reduction | |
CN105734293A (en) | High-grade lead matte resource comprehensive recovery technology | |
CN102634819A (en) | Method for preparing electrolytic manganese/electrolytic manganese dioxide through leaching manganese oxide by sulfur dioxide | |
CN107557590A (en) | Zinc dross recoverying and utilizing method | |
CN104402062A (en) | Method for preparing ferric chloride from pyrite cinder | |
CN102296323A (en) | Manufacturing system for producing electrolytic manganese metal by two-ore method | |
CN104120253A (en) | Leaching method of complex zinc calcined ores | |
CN105399132A (en) | Technology for preparing tribasic copper chloride and tetrabasic zinc chloride by utilization of brass slag and zinc-containing flue ash |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |