CN105776339A - Method for preparing nano-sized zinc ferrite through comprehensive treatment of zinc containing steel pickling waste liquid - Google Patents
Method for preparing nano-sized zinc ferrite through comprehensive treatment of zinc containing steel pickling waste liquid Download PDFInfo
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- CN105776339A CN105776339A CN201610084068.1A CN201610084068A CN105776339A CN 105776339 A CN105776339 A CN 105776339A CN 201610084068 A CN201610084068 A CN 201610084068A CN 105776339 A CN105776339 A CN 105776339A
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- zinc
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a method for preparing nano-sized zinc ferrite through comprehensive treatment of zinc containing steel pickling waste liquid.The method comprises the following steps that 1, reductant ferric iron is added into the zinc containing steel pickling waste liquid, and the mixture is stirred to be uniform and stands for 8-14 h; 2, pH is regulated to 3-6, auxiliaries are added, stirring, standing and filtering are conducted at the temperature of 40-80 DEG C, and secondary treating fluid is obtained; 3, the total amount-of-substance concentration of Zn2+ and Fe in the secondary treating fluid is measured, and zinc chloride or zinc oxide and water are added while stirring; 4, a precipitator is added while stirring, sediment is generated, and stirring is continued; 5, filtering is conducted, and obtained filtrate is used for replacing the water in the step 3; filter cakes are washed, dried, ground and calcined to obtain nano-sized zinc ferrite.The zinc containing steel pickling waste liquid is subjected to recycled innocent treatment, cost is low, efficiency is high, product quality is high, environment friendliness is achieved, and a good technical scheme is provided for treatment of the zinc containing pickling waste liquid in the steel industry.
Description
Technical field
The present invention relates to inorganic nanometer functional field of material preparation, particularly relate to one and prepared nanometer by the iron and steel pickling waste liquid containing zinc
The method of zinc ferrite.
Background technology
At steel industry, owing to pickling is inevitable step, so every day all can produce substantial amounts of iron and steel pickling waste liquid.Steel
Ferrum pickle liquor generally refers to hydrochloric acid, the hydrochloric acid containing high concentration and ferrous ion in the waste liquid of steel hydrochloric acid pickling, acid
Wash waste liquor PH at about 0.2-3.0, be mainly composed of Fe2+, containing a small amount of Fe3+With some other impurity, have possibly together with
The PO of trace4 3-、Zn2+, it is commonly called as " pickle ".Therefore, if waste liquid is without processing directly discharge, will result in serious ring
Environment pollution, causes a series of environmental issue to occur.And for containing zinc iron and steel pickling waste liquid, owing to it contains more Zn2+,
Its content is considerably beyond the discharge standard of national regulation, and therefore this type pickle can not be according to general pickle
Processing mode solves.The iron and steel pickling waste liquid containing zinc is the mixture that composition is extremely complex, not only has containing a certain amount of zinc
And ferrum, possibly together with a large amount of hydrochloric acid and multiple non-quantitative metal ion, such as aluminum, silicon, manganese, copper, lead, magnesium, nickel, calcium, bismuth etc.
Ion, and the preparation of pure zinc ferrite is affected the biggest by these metal ions, it is necessary to process；Fail to understand thing possibly together with many simultaneously
Matter dust etc. must process.Due to its particularity, steel industry never has suitable way and solves the pickle liquor band on zinc
The most serious problem of environmental pollution come.Therefore, the most effectively processing containing zinc iron and steel pickling waste liquid is also that steel industry faces
A significant technology issues, this problem is not only related to the development of industry self, the most closely affects the environment of surrounding.
Zinc ferrite (ZnFe2O4) due to its construction features and the excellent characteristic such as heat-resisting, fast light, antirust, nontoxic, magnetic material,
There are purposes and application prospect widely in the fields such as catalysis dehydrogenation, flue gas desulfurization and anti-corrosion paint.Zinc ferrite is a kind of function admirable
Soft magnetic materials, be again the catalyst of the most representational alkenes oxidation of organic compounds dehydrogenation, there is the highest photocatalysis simultaneously
Activity and the semiconductor catalyst sensitive to visible ray, zinc ferrite nanoparticle is also the transparent inorganic pigment of a function admirable.Main
It is used for needing high-fire resistance, occasion nontoxic, inert, such as plastics, enamel, toy etc..The antirust face of coating level zinc ferrite
Material is applicable to all kinds of solvent-borne type antirust paint, corrosion resistant coating, paint for priming paint and top lacquer.Owing to having these special performances, people are more and more heavier
Application depending on zinc ferrite powder body.Therefore, exploitation has nanometer Zn Fe of good characteristic2O4Powder body has a wide range of applications, city
Field demand is the most increasing.Zinc ferrite is prepared for raw material with this kind of iron and steel pickling waste liquid, if be left intact,
It is impossible to prepare qualified zinc ferrite.
Summary of the invention
Present invention aim to address that current domestic steel industry processes a difficult problem for the technology that the iron and steel pickling waste liquid on zinc is faced, carry
For a kind of method being prepared nanometer zinc ferrite by the pickling waste acid liquor resource utilization integrated treatment containing zinc.
Technical scheme is summarized as follows:
A kind of method being prepared nanometer zinc ferrite by the iron and steel pickling waste liquid integrated treatment containing zinc, comprises the steps:
(1) to containing adding reducing agent reduction ferric iron in zinc iron and steel pickling waste liquid, the addition quality of reducing agent is containing zinc pickling iron and steel
The 0.2%～1% of waste liquid quality, stirs, and places 8-14h；
(2) regulating step (1) obtains the pH to 3～6 of liquid, adds auxiliary agent and makes final concentration of the 40～80mg/L of auxiliary agent,
Stir 0.5-3h when 40～80 DEG C, stand 1-2h, filter, obtain after-treatment liquid；
(3) Zn in after-treatment liquid is surveyed2+And FeAlwaysSubstance withdrawl syndrome, be 25-80 DEG C in temperature, under stirring, add chlorine
Change zinc or zinc oxide and water, make n (Fe in mixed liquorAlways)/n(Zn2+)=1.8-2.2, makes Fe simultaneouslyAlwaysConcentration is 0.5mol/L
-3mol/L；
(4) carry out by one of following two ways:
Mode one: under stirring, adds precipitant NaOH or KOH in the mixed liquor that step (3) obtains, makes in mixed liquor
n(OH-)/n(Zn2+)=3.6；There is precipitation to generate, continue stirring 10-60min；
Mode two: under stirring, adds precipitant oxalic acid or oxalates in the mixed liquor that step (3) obtains, makes in mixed liquor
n(C2O4 2-)/n(Zn2+)=0.8-1.2, has precipitation to generate, and continues stirring 10-60min；
(5) filtering, the filtrate obtained is for alternative steps (3) described water；Cake Wash, dry, grind, calcine,
To nanometer zinc ferrite.
The addition quality of reducing agent preferably contains the 0.3%～0.5% of zinc iron and steel pickling waste liquid quality.
The preferred iron powder of reducing agent or scrap iron skin.
Step (2) is preferably: obtain the pH to 5～6 of liquid with sodium hydroxide regulating step (1), adds auxiliary agent and makes auxiliary agent
Final concentration of 50～65mg/L, when 50～65 DEG C stir 1-2h, stand 1-2h, filter, obtain after-treatment liquid.
Auxiliary agent preferred cationic polyacrylamide or poly-iron chloride.
Preferably: n (FeAlways)/n(Zn2+)=2, make Fe simultaneouslyAlwaysConcentration is 3.0mol/L.
The preferred Disodium oxalate. of oxalates or potassium oxalate.
Preferably: n (C2O4 2-)/n(Zn2+)=1.2.
Calcining heat is 400-800 DEG C, calcines 1-3h.
Advantages of the present invention: carry out recycling treatment to containing zinc pickle liquor by the method for the present invention, thoroughly solves pickle liquor pair
The pollution of environment；By to preparation process produces the recycling of waste liquid, the problem solving secondary pollution；Use side of the present invention
Method obtains the nanometer zinc ferrite of high-quality, it is achieved that turn waste into wealth；The method investment of the present invention is low, low cost, efficiency high, product
Product quality is high, environmental protection, processes the pickle liquor on zinc for steel industry and provides a kind of well technical scheme.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the zinc ferrite that embodiment 1 obtains.
Fig. 2 is the XRD figure spectrum of the zinc ferrite that embodiment 2 obtains.
Fig. 3 is the TEM picture of the zinc ferrite that embodiment 1 obtains.
Fig. 4 is the TEM picture of the zinc ferrite that embodiment 2 obtains.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated, and the following examples are to make those skilled in the art
Member better understood when the present invention, but does not impose any restrictions the present invention.
Embodiment 1
A kind of method being prepared nanometer zinc ferrite by the iron and steel pickling waste liquid integrated treatment containing zinc, comprises the steps:
(1) adding iron powder reducing ferric iron in containing zinc iron and steel pickling waste liquid (60ml, 78g), the addition quality of iron powder is containing zinc steel
The 0.5% of ferrum pickle liquor quality, stirs, and places 14h；
(2) obtain the pH to 6 of liquid with sodium hydroxide regulating step (1), add PAMC and make polypropylene
The final concentration of 65mg/L of amide, stirs 1h, stands 1h, filter, obtain after-treatment liquid when 65 DEG C；
(3) Zn in after-treatment liquid is surveyed2+And FeAlwaysSubstance withdrawl syndrome, n (Zn2+)=0.43mol/L；n(FeAlways)=3.324mol/L
(wherein n (Fe2+)=3.299mol/L, n (Fe3+)=0.025mol/L) under temperature is 25 DEG C, stirs, to 45.13ml
After-treatment liquid adds solder(ing)acid (6.63g solid ZnCl2It is dissolved in 100ml water, is sufficiently stirred for) and 154.87ml
Water obtains mixed liquor, makes n (Fe in mixed liquorAlways)/n(Zn2+)=2.2, make Fe simultaneouslyAlwaysConcentration is 0.5mol/L；
(4) under agitation, in the mixed liquor that step (3) obtains, 10.96g Na is added2C2O4, make in mixed liquor
n(C2O4 2-)/n(Zn2+)=1.2, have precipitation to generate, and continue stirring 60min；
(5) filtering, the filtrate obtained is for alternative steps (3) described water；Filter cake washes with water 3 times, 60 DEG C of drying, grinds,
400 DEG C of calcining 3h, obtain nanometer zinc ferrite 15.23g.
Embodiment 2
A kind of method being prepared nanometer zinc ferrite by the iron and steel pickling waste liquid integrated treatment containing zinc, comprises the steps:
(1) adding iron powder reducing ferric iron in containing zinc iron and steel pickling waste liquid (300ml, 390g), the addition quality of iron powder is containing zinc
The 0.2% of iron and steel pickling waste liquid quality, stirs, and places 14h；
(2) obtain the pH to 3 of liquid with sodium hydroxide regulating step (1), add PAMC and make polypropylene
The final concentration of 40mg/L of amide, stirs 3h, stands 1h, filter, obtain after-treatment liquid when 40 DEG C；
(3) Zn in after-treatment liquid is surveyed2+And FeAlwaysSubstance withdrawl syndrome, n (Zn2+)=0.43mol/L；n(FeAlways)=3.324mol/L
(wherein n (Fe2+)=3.299mol/L, n (Fe3+)=0.025mol/L) temperature be 80 DEG C, under stirring, to 270ml bis-times
Treatment fluid adds solder(ing)acid (45.41g solid ZnCl2It is dissolved in 20ml water, is sufficiently stirred for) and 10ml embodiment
The filtrate that 1 step (5) obtains dilutes to obtain mixed liquor, makes n (Fe in mixed liquorAlways)/n(Zn2+)=2.0, make Fe simultaneouslyAlwaysConcentration is
3mol/L；
(4) under agitation, in the mixed liquor that step (3) obtains, 45.72g K is added2C2O4, make in mixed liquor
n(C2O4 2-)/n(Zn2+)=0.8, has precipitation to generate, and continues stirring 10min；
(5) filtering, the filtrate obtained is for alternative steps (3) described water；Filter cake washes with water 3 times, 80 DEG C of drying, grinds,
800 DEG C of calcining 1h, obtain nanometer zinc ferrite 104.80g.
The K of the present embodiment is substituted with oxalic acid (32.4g)2C2O4, other same the present embodiment, obtain nanometer zinc ferrite 103.2g.
Embodiment 3
A kind of method being prepared nanometer zinc ferrite by the iron and steel pickling waste liquid integrated treatment containing zinc, comprises the steps:
(1) adding iron powder reducing ferric iron in containing zinc iron and steel pickling waste liquid (200ml, 260g), the addition quality of iron powder is containing zinc
The 1% of iron and steel pickling waste liquid quality, stirs, and places 8h；
(2) obtain the pH to 6 of liquid with sodium hydroxide regulating step (1), add PAMC and make polypropylene
The final concentration of 80mg/L of amide, stirs 0.5h, stands 1h, filter, obtain after-treatment liquid when 80 DEG C；
(3) Zn in after-treatment liquid is surveyed2+And FeAlwaysSubstance withdrawl syndrome, n (Zn2+)=0.43mol/L；n(FeAlways)=3.324
Mol/L (wherein n (Fe2+)=3.299mol/L, n (Fe3+)=0.025mol/L), under temperature is 50 DEG C, stirs, to 180.5ml
After-treatment liquid adds solder(ing)acid (34.77g solid ZnCl2It is dissolved in 100ml water, is sufficiently stirred for) and 19.5ml
The filtrate that in embodiment 2, step (5) obtains dilutes to obtain mixed liquor, makes n (Fe in mixed liquorAlways)/n(Zn2+)=1.8, make simultaneously
FeAlwaysConcentration is 2mol/L；
(4) under agitation, in the mixed liquor that step (3) obtains, add 47.99g NaOH, make in mixed liquor
n(OH-)/n(Zn2+)=3.6, have precipitation to generate, and continue stirring 60min；
(5) filtering, the filtrate obtained is for alternative steps (3) described water；Filter cake washes with water 3 times, 70 DEG C of drying, grind,
Calcine 3h at 400 DEG C, obtain nanometer zinc ferrite 72.35g.
The iron powder of the present embodiment is substituted with scrap iron skin, other same the present embodiment, nanometer zinc ferrite can be obtained.
Embodiment 4
A kind of method being prepared nanometer zinc ferrite by the iron and steel pickling waste liquid integrated treatment containing zinc, comprises the steps:
(1) adding iron powder reducing ferric iron in containing zinc iron and steel pickling waste liquid (60ml, 78g), the addition quality of iron powder is containing zinc
The 0.3% of iron and steel pickling waste liquid quality, stirs, and places 12h；
(2) obtain the pH to 5 of liquid with sodium hydroxide regulating step (1), add poly-iron chloride and make end of poly-iron chloride dense
Degree is 50mg/L, stirs 2h when 50 DEG C, stands 2h, filters, obtain after-treatment liquid；
(3) Zn in after-treatment liquid is surveyed2+And FeAlwaysSubstance withdrawl syndrome, n (Zn2+)=0.43mol/L；n(FeAlways)=3.324
Mol/L (wherein n (Fe2+)=3.299mol/L, n (Fe3+)=0.025mol/L) under temperature is 60 DEG C, stirs, to 45.13ml
After-treatment liquid adds zinc oxide aqueous solution (3.95g solid Zn0 is dissolved in 100ml water, is sufficiently stirred for) and 154.87ml
The filtrate that in embodiment 3, step (5) obtains dilutes to obtain mixed liquor, makes n (Fe in mixed liquorAlways)/n(Zn2+)=2.2, make simultaneously
FeAlwaysConcentration is 0.5mol/L；
(4) under agitation, in the mixed liquor that step (3) obtains, add 13.74g KOH, make in mixed liquor
n(OH-)/n(Zn2+)=3.6, have precipitation to generate, and continue stirring 10min；
(5) filtering, the filtrate obtained is for alternative steps (3) described water；Filter cake washes with water 3 times, and 60 DEG C of drying are ground
Mill, at 800 DEG C, calcines 1h, obtains nanometer zinc ferrite 15.31g.
The iron and steel pickling waste liquid containing zinc that each embodiment is used is to enable those skilled in the art to be more fully understood that this
Bright, but the present invention is not imposed any restrictions.
Claims (9)
1. the method being prepared nanometer zinc ferrite by the iron and steel pickling waste liquid integrated treatment containing zinc, is characterized in that comprising the steps:
(1) to containing adding reducing agent reduction ferric iron in zinc iron and steel pickling waste liquid, the addition quality of reducing agent is containing zinc pickling iron and steel
The 0.2%～1% of waste liquid quality, stirs, and places 8-14h；
(2) regulating step (1) obtains the pH to 3～6 of liquid, adds auxiliary agent and makes final concentration of the 40～80mg/L of auxiliary agent,
Stir 0.5-3h when 40～80 DEG C, stand 1-2h, filter, obtain after-treatment liquid；
(3) Zn in after-treatment liquid is surveyed2+And FeAlwaysSubstance withdrawl syndrome, be 25-80 DEG C in temperature, under stirring, add chlorine
Change zinc or zinc oxide and water, make n (Fe in mixed liquorAlways)/n(Zn2+)=1.8-2.2, makes Fe simultaneouslyAlwaysConcentration is 0.5mol/L
-3mol/L；
(4) carry out by one of following two ways:
Mode one: under stirring, adds precipitant NaOH or KOH in the mixed liquor that step (3) obtains, makes in mixed liquor
n(OH-)/n(Zn2+)=3.6；There is precipitation to generate, continue stirring 10-60min；
Mode two: under stirring, adds precipitant oxalic acid or oxalates in the mixed liquor that step (3) obtains, makes in mixed liquor
n(C2O4 2-)/n(Zn2+)=0.8-1.2, has precipitation to generate, and continues stirring 10-60min；
(5) filtering, the filtrate obtained is for alternative steps (3) described water；Cake Wash, dry, grind, calcine,
To nanometer zinc ferrite.
Method the most according to claim 1, is characterized in that the addition quality of described reducing agent is for containing zinc iron and steel pickling waste liquid matter
The 0.3%～0.5% of amount.
Method the most according to claim 1 and 2, is characterized in that described reducing agent is iron powder or scrap iron skin.
Method the most according to claim 1, is characterized in that described step (2) is: with sodium hydroxide regulating step (1)
Obtain the pH to 5～6 of liquid, add auxiliary agent and make final concentration of the 50～65mg/L of auxiliary agent, stir 1-2h when 50～65 DEG C, quiet
Put 1-2h, filter, obtain after-treatment liquid.
5., according to the method described in claim 1 or 4, it is characterized in that described auxiliary agent is PAMC or poly-iron chloride.
Method the most according to claim 1, is characterized in that n (FeAlways)/n(Zn2+)=2, make Fe simultaneouslyAlwaysConcentration is 3.0mol/L.
Method the most according to claim 1, is characterized in that described oxalates is Disodium oxalate. or potassium oxalate.
8., according to the method described in claim 1 or 7, it is characterized in that described n (C2O4 2-)/n(Zn2+)=1.2.
Method the most according to claim 1, is characterized in that described calcining heat is 400-800 DEG C, calcines 1-3h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107140691A (en) * | 2017-06-30 | 2017-09-08 | 江苏省冶金设计院有限公司 | A kind of utilization zinc leaching residue prepares the method and device of zinc ferrite |
| CN109399725A (en) * | 2017-08-15 | 2019-03-01 | 中国石油化工股份有限公司 | A kind of preparation method and applications of the nano-structure array of dregs containing zinc |
| CN109437316A (en) * | 2018-12-06 | 2019-03-08 | 钦州学院 | A kind of preparation method of nanometer level superfine iron zinc composite oxide material |
| CN115893504A (en) * | 2022-01-10 | 2023-04-04 | 中南大学 | Microwave-assisted preparation method of magnetic zinc ferrite |
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| CN104787803A (en) * | 2015-04-04 | 2015-07-22 | 天津大学 | Method for preparing nano-sized zinc ferrite from zinc-contained steel pickling waste liquid |
| CN105271432A (en) * | 2015-10-19 | 2016-01-27 | 天津大学 | Method for preparing nano ferroferric oxide particle with steel picking waste liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107140691A (en) * | 2017-06-30 | 2017-09-08 | 江苏省冶金设计院有限公司 | A kind of utilization zinc leaching residue prepares the method and device of zinc ferrite |
| CN109399725A (en) * | 2017-08-15 | 2019-03-01 | 中国石油化工股份有限公司 | A kind of preparation method and applications of the nano-structure array of dregs containing zinc |
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| CN115893504A (en) * | 2022-01-10 | 2023-04-04 | 中南大学 | Microwave-assisted preparation method of magnetic zinc ferrite |
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Application publication date: 20160720 |