CN106391018A - Method for preparing active waste slag catalyst by metallurgical waste slag and application of active waste slag catalyst - Google Patents
Method for preparing active waste slag catalyst by metallurgical waste slag and application of active waste slag catalyst Download PDFInfo
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- CN106391018A CN106391018A CN201611019642.1A CN201611019642A CN106391018A CN 106391018 A CN106391018 A CN 106391018A CN 201611019642 A CN201611019642 A CN 201611019642A CN 106391018 A CN106391018 A CN 106391018A
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- Prior art keywords
- waste residue
- catalyst
- metallurgical slag
- active
- waste slag
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
Abstract
The invention provides a method for preparing an active waste slag catalyst by metallurgical waste slag. The method comprises the following steps of (1) dissolving iron salt into water, so as to prepare an iron salt solution; (2) adding the clean metallurgical waste slag into a Fenton fluidized bed, adding the iron salt solution and hydrogen peroxide, adjusting the pH (potential of hydrogen) value, and performing crystallization reaction; (3) drying the crystallized material in step (2), so as to prepare the active waste slag catalyst. The activated waste slag catalyst contains a ferric oxide thin film. The preparation method has the advantage that by combining the characteristics of the Fenton fluidized bed and waste slag, a preparation method of Fenton fluidized bed catalyst based on the steel and iron smelting waste slag is proposed, so that the purposes of enhancing Fenton reaction and realizing resource utilization of waste slag are realized.
Description
Technical field
The present invention relates to field of waste water treatment, more particularly to a kind of utilization metallurgical slag preparation activity waste residue catalyst
Method and its application.
Background technology
With people, environmental conservation is paid close attention to the increase of temperature, industrial wastewater discharge standard is increasingly strict.Traditional life
Change process+flocculation sediment can not meet the requirement of existing discharge standard, and therefore, further treatment technique is gradually at waste water
Reason field is extensively applied.
Fenton's reaction can produce hydroxyl radical free radical, has great oxidability, is capable of the oxidized waste water of no selection
Middle most of Organic substance, is used to process many used water difficult to degradate.Ferrous ion in conventional homogeneous Fenton's reaction is in catalysis
During hydrogen peroxide, iron cement can be formed, lead to catalyst loss with the iron cement that water outlet is discharged, utilization rate is low, cost of material increases
Plus.Although the iron cement being formed has certain flocculation sediment effect, flocculu shape is more open, and dewatering is poor, is formed
Sludge volume is larger, and subsequent treatment is costly.For solving the disadvantages mentioned above of homogeneous Fenton's reaction, in recent years, study both at home and abroad
Person begins to focus on Fenton fluid bed.Fenton fluid bed passes through to introduce filler, the iron cement producing is crystallized on filler, is that Fenton is anti-
Heterogeneous catalytic reaction point position should be provided, improve catalyst use efficiency, reduce the yield of iron cement；And this reactor combines
Homogeneously with heterogeneous Fenton's reaction, significantly improve reaction efficiency and reduce processing cost.How to prepare efficient, cheap solid phase
Catalyst filling is the core of Fenton fluidization.
Metallurgical slag is a kind of inevitable by-product of typical smelting process.The smelting of China's steel industry generation in 2013
Up to 4.16 hundred million tons of waste residue, comprehensive utilization ratio is only 30%.Substantial amounts of waste residue does not obtain sufficient effectively utilizes, is not only
Waste to resource, even more causes great pressure to environment.The discharge of waste residue and to deal carefully be a stubborn problem.
Separately, waste residue contains 10～23% iron oxide composition, and loose porous, specific surface area is big, is a kind of potential good adsorbent material
Material, can be used in various wastewater treatments.
Content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of lived using metallurgical slag preparation
Property the method for waste residue catalyst and its application, do not obtain fully for solving a large amount of waste residues that in prior art, smelting process produces
Using the problems such as after, discharge, environmental pollution is serious, existing fenton catalyst production cost is higher.
For achieving the above object and other related purposes, the present invention provides and a kind of prepare active waste residue using metallurgical slag and urges
The method of agent, comprises the steps：
1) iron salt is soluble in water, prepared iron salt solutions；
2) clean metallurgical slag is added in Fenton fluid bed, add iron salt solutions and hydrogen peroxide, adjust pH, carry out
Crystallization reaction；
3) by step 2) the prepared drying materials of crystallization reaction, described activity waste residue catalyst is obtained.This active waste residue is urged
Agent contains oxide ferroelectric thin film.
Further, step 1) in, described iron salt is sulfate containing iron ion, one of nitrate, hydrochlorate or
Several combinations.Iron ion includes ferric ion, ferrous ion etc..
Further, step 1) in, the mass concentration of described iron salt solutions is 1wt%-50wt%.I.e. molten in iron salt solutions
The percentage ratio that the quality of matter accounts for solution quality is 1%-50%.
Further, step 2) in, described metallurgical slag includes smelting ferrum waste residue, non-ferrous metal slag.
Further, described smelting ferrum waste residue includes blast furnace slag, vessel slag, slag, described non-ferrous metal cinder ladle include copper ashes,
Lead skim, cadmia, nickel slag.
Further, step 2) in, in described iron salt solutions, iron ion and the mol ratio of hydrogen peroxide in hydrogen peroxide are
(0.2-4)：1.Described hydrogen peroxide can be commercially available hydrogen peroxide.
Further, step 2) in, in iron salt solutions, iron ion and the mass ratio of metallurgical slag are (0.1-1)：1.
Further, step 2) in, during crystallization reaction, the pH value of feed liquid controls in 2-5.During pH regulator, dilute sulfur can be adopted
Acid, sodium hydrate aqueous solution etc..
Preferably, step 2) in, during crystallization reaction, the pH value of feed liquid controls in 4-5.
Further, step 2) in, crystallization reaction is to waste residue Surface Creation brown oxide ferroelectric thin film.Response time is usual
For 2-5h.
Further, step 2) in, the particle diameter of described metallurgical slag is 0.5mm-4mm.
Further, step 2) in, described metallurgical slag first passes through cleaning, and cleaning comprises the steps：By metallurgical slag
Add in acid solution, stirring at normal temperature 6h～18h, filters, washs to neutrality, be dried, obtain the metallurgical slag of cleaning.
Further, step 3) in, drying temperature is 20 DEG C -120 DEG C.
Second aspect present invention provides the active waste residue catalyst that a kind of said method is obtained.
Third aspect present invention provides the application in Fenton fluid bed wastewater treatment for the waste residue catalyst of above-mentioned activity.
As described above, a kind of method of the active waste residue catalyst of utilization metallurgical slag preparation of the present invention and its application, tool
There is following beneficial effect：The present invention combines Fenton fluid bed and waste residue characteristic, propose a kind of based on smelting iron and steel waste residue
The preparation method of Fenton fluid catalyst, the purpose reaching strengthening Fenton's reaction and realizing waste residue resource utilization.Prepared
Active waste residue catalyst contains iron oxides overlay film, can be used for Fenton fluid bed wastewater treatment.Adding in Fenton fluid bed should
After catalyst, can effectively remove the pollutant in waste water, reaction efficiency significantly improves than conventional homogeneous Fenton's reaction；Can be greatly
Save the addition of pharmacy response, reduce iron cement yield nearly 70%, reduce the cost about 50% of wastewater treatment；This active waste residue is urged
Agent can reuse, and there is not secondary pollution.
Brief description
Fig. 1 is shown as the active waste residue catalyst preparation process flow chart of the embodiment of the present invention.
Specific embodiment
Below by way of specific instantiation, embodiments of the present invention are described, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also be by addition different concrete realities
The mode of applying is carried out or applies, and the every details in this specification can also be based on different viewpoints and application, without departing from
Carry out various modifications and changes under the spirit of the present invention.
The preparation technology flow process of present invention activity waste residue catalyst is as shown in Figure 1.
Embodiment 1
The active waste residue method for preparing catalyst of the present embodiment is as follows：
Choose the slag of Chongqing steel mill, screened, take particle diameter to be that 0.5mm～0.8mm obtains slag standby；After screening
Slag is put in the sulfuric acid solution of 2wt%, stirring at normal temperature 12h, filters, and washs to neutrality, is dried, obtains the slag of cleaning；Will
Ferrous sulfate is soluble in water, prepares copperas solution, and its mass concentration is 10wt%, adds commercially available hydrogen peroxide (quality
Concentration 30%), crystallize in fluid bed with clean slag, during crystallization reaction, the pH of reactant liquor is controlled to 3, crystallization is anti-
Should be to waste residue Surface Creation brown oxide ferroelectric thin film, 20 DEG C of drying, obtain the active waste residue catalysis containing iron oxides overlay film
Agent.
In the present embodiment, the iron ion in copperas solution used is 2 with the mol ratio of hydrogen peroxide in hydrogen peroxide:1；
Iron ion used and clean steel slag mass ratio are 1:1.
The active waste residue catalyst particle size containing iron oxides overlay film preparing is 0.6mm～0.9mm.
Process certain coke-oven plant's bio-chemical effluent, optimum response using prepared active slag catalyst in Fenton fluid bed
Under the conditions of (hydrogen peroxide dosage is 150mg/L, and the hydrogen peroxide in the hydrogen peroxide adding and ferrous sulfate mol ratio are 4:1),
Waste water COD is down to 60mg/L from 150mg/L, and clearance is 40%, reaches《Coking chemistry emission of industrial pollutants standard》
(GB16171-2012).Under conditions of reaching identical reflection effect, when being not added with active slag catalyst, hydrogen peroxide and ferrous iron
Dosage be respectively 450mg/L and 500mg/L.Therefore, after using active slag catalyst, it is possible to decrease medicament (hydrogen peroxide and
Iron salt solutions) usage amount about 60%, and, the crystallization due to active slag catalyst, the iron cement amount producing after reaction
Ratio is not added with during slag catalyst reducing about 70%.
Embodiment 2
The active waste residue method for preparing catalyst of the present embodiment is as follows：
Choose the slag of Chongqing steel mill, screened, the slag taking particle diameter to be 0.5mm～0.8mm is standby；After screening
Slag is put in the sulfuric acid solution of 2wt%, stirring at normal temperature 12h, filters, and washs to neutrality, is dried, obtains the slag of cleaning；Will
Ferrous sulfate is soluble in water, prepares copperas solution, and its mass concentration is 10wt%, adds commercially available hydrogen peroxide (quality
Concentration 30%), crystallize in fluid bed with clean slag, during crystallization reaction, the pH of reactant liquor is controlled to 4, crystallization is anti-
Should be to waste residue Surface Creation brown oxide ferroelectric thin film, 80 DEG C of drying, obtain the active waste residue catalysis containing iron oxides overlay film
Agent.
In the present embodiment, the iron ion in copperas solution used is 2 with the mol ratio of hydrogen peroxide in hydrogen peroxide:1；
Iron ion used and clean steel slag mass ratio are 1:1.
The active waste residue catalyst particle size containing iron oxides overlay film preparing is 0.6mm～0.9mm.
Process certain coke-oven plant's bio-chemical effluent, optimum response using prepared active slag catalyst in Fenton fluid bed
Under the conditions of (hydrogen peroxide dosage is 400mg/L, and the hydrogen peroxide in the hydrogen peroxide adding and ferrous sulfate mol ratio are 2:1),
Waste water COD is down to 60mg/L from 200mg/L, and clearance is 70%, reaches《Coking chemistry emission of industrial pollutants standard》
(GB16171-2012).When being not added with active slag catalyst, hydrogen peroxide and ferrous dosage be respectively 1500mg/L and
1500mg/L, COD are down to 93mg/L from 200mg/L, fail to reach corresponding discharge standard.Therefore, it is catalyzed using active slag
After agent, it is remarkably improved the efficiency of Fenton's reaction, realize discharged wastewater met the national standard.
Embodiment 3
The active waste residue method for preparing catalyst of the present embodiment is as follows：
Choose the slag of Chongqing steel mill, screened, the slag taking particle diameter to be 0.5mm～0.8mm is standby；After screening
Slag is put in the sulfuric acid solution of 2wt%, stirring at normal temperature 12h, filters, and washs to neutrality, is dried, obtains the slag of cleaning；Will
Ferrous sulfate is soluble in water, prepares copperas solution, and its mass concentration is 10wt%, adds commercially available hydrogen peroxide (quality
Concentration 30%), crystallize in fluid bed with clean slag, during crystallization reaction, the pH of reactant liquor is controlled to 5, crystallization is anti-
Should be to waste residue Surface Creation brown oxide ferroelectric thin film, 120 DEG C of drying, obtain the active waste residue catalysis containing iron oxides overlay film
Agent.
In the present embodiment, the iron ion in copperas solution used is 4 with the mol ratio of hydrogen peroxide in hydrogen peroxide:1；
Iron ion used and clean steel slag mass ratio are 1:1.
The active waste residue catalyst particle size containing iron oxides overlay film preparing is 0.6mm～0.9mm.
Process certain coke-oven plant's bio-chemical effluent, optimum response using prepared active slag catalyst in Fenton fluid bed
Under the conditions of (hydrogen peroxide dosage is 200mg/L, and the hydrogen peroxide in the hydrogen peroxide adding and ferrous sulfate mol ratio are 2:1),
Waste water COD is down to 50mg/L from 100mg/L, and clearance is 50%, reaches《Coking chemistry emission of industrial pollutants standard》
(GB16171-2012).Under conditions of reaching identical reflection effect, when being not added with active slag catalyst, hydrogen peroxide and ferrous iron
Dosage be respectively 300mg/L and 340mg/L.Therefore, after using active slag catalyst, it is possible to decrease medicament (hydrogen peroxide and
Iron salt solutions) usage amount about 33%, and, the crystallization due to active slag catalyst, the iron cement amount producing after reaction
Ratio is not added with during slag catalyst reducing about 40%.
In sum, effectively utilizes metallurgical slag of the present invention, the active waste residue catalyst preparing is in Fenton fluid bed
Play good catalytic action when purifying waste water, during wastewater treatment, significantly reduce the addition of hydrogen peroxide and iron ion.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (10)
1. a kind of method using the active waste residue catalyst of metallurgical slag preparation is it is characterised in that comprise the steps：
1) iron salt is soluble in water, prepared iron salt solutions；
2) clean metallurgical slag is added in Fenton fluid bed, add iron salt solutions and hydrogen peroxide, adjust pH, crystallized
Reaction；
3) by step 2) the prepared drying materials of crystallization reaction, described activity waste residue catalyst is obtained.
2. the active waste residue catalyst of utilization metallurgical slag according to claim 1 preparation method it is characterised in that：Step
1) in, described iron salt is sulfate containing iron ion, the combination of one or more of nitrate, hydrochlorate.
3. the active waste residue catalyst of utilization metallurgical slag according to claim 1 preparation method it is characterised in that：Step
1), in, the mass concentration of described iron salt solutions is 1wt%-50wt%.
4. the active waste residue catalyst of utilization metallurgical slag according to claim 1 preparation method it is characterised in that：Step
2), in, described metallurgical slag includes smelting ferrum waste residue, non-ferrous metal slag.
5. the active waste residue catalyst of utilization metallurgical slag according to claim 1 preparation method it is characterised in that：Step
2), in, in described iron salt solutions, iron ion and the mol ratio of hydrogen peroxide in hydrogen peroxide are (0.2-4):1.
6. the active waste residue catalyst of utilization metallurgical slag according to claim 1 preparation method it is characterised in that：Step
2), in, in iron salt solutions, iron ion and the mass ratio of metallurgical slag are (0.1-1)：1.
7. the active waste residue catalyst of utilization metallurgical slag according to claim 1 preparation method it is characterised in that：Step
2), in, during crystallization reaction, the pH value of feed liquid controls in 2-5.
8. the active waste residue catalyst of utilization metallurgical slag according to claim 1 preparation method it is characterised in that：Step
2), in, crystallization reaction is to waste residue Surface Creation brown oxide ferroelectric thin film；The particle diameter of described metallurgical slag is 0.5mm-4mm；Institute
State metallurgical slag and first pass through cleaning, cleaning comprises the steps：Metallurgical slag is added in acid solution, stirring at normal temperature 6h～
18h, filters, and washs to neutrality, is dried, obtains the metallurgical slag of cleaning；Step 3) in, drying temperature is 20 DEG C -120 DEG C.
9. the active waste residue catalyst that the method according to any one of claim 1-8 is obtained.
10. active application in Fenton fluid bed wastewater treatment for the waste residue catalyst according to claim 9.
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| CN201611019642.1A CN106391018A (en) | 2016-11-09 | 2016-11-09 | Method for preparing active waste slag catalyst by metallurgical waste slag and application of active waste slag catalyst |
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| CN201611019642.1A CN106391018A (en) | 2016-11-09 | 2016-11-09 | Method for preparing active waste slag catalyst by metallurgical waste slag and application of active waste slag catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201085A (en) * | 2018-10-29 | 2019-01-15 | 江苏哈宜环保研究院有限公司 | A kind of preparation method and applications of fluidized bed fenton catalyst |
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| CN102580743A (en) * | 2011-12-30 | 2012-07-18 | 浙江大学 | Method for preparing oxidation catalyst from gold ore tailing slag, and prepared oxidation catalyst and application thereof |
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