CN107673410A - The method that nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid - Google Patents
The method that nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid Download PDFInfo
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- CN107673410A CN107673410A CN201710974079.1A CN201710974079A CN107673410A CN 107673410 A CN107673410 A CN 107673410A CN 201710974079 A CN201710974079 A CN 201710974079A CN 107673410 A CN107673410 A CN 107673410A
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- waste liquid
- ferriferrous oxide
- nano ferriferrous
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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
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- 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
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention provides one kind to prepare nano ferriferrous oxide（Fe3O4）Method, be using iron content waste liquid as raw material, under magnetic agitation in iron content waste liquid add dispersant stir, add cushioning liquid（pH 9~11）Stir；By mixed solution under ventilation condition autoxidation；By magnetic force by the debris buildup of product after the completion of oxidation, separate, washing, produce nano ferriferrous oxide sample.Nano ferriferrous oxide particle diameter prepared by the present invention is smaller, and for particle diameter in below 100nm, particle diameter distribution is uniform, and dispersiveness is preferably, available for coating, telecommunication apparatus, rubber, ceramics, papermaking, ink, art painting etc.；The present invention is also reclaimed while nano ferriferrous oxide is prepared to the ferro element in Industry Waste iron liquid, not only has actual economic value, it is often more important that have environment protection significance.
Description
Technical field
The present invention relates to a kind of preparation method of nano ferriferrous oxide, more particularly to prepared and received using industrial ferrous contained waste liquid
The method of rice ferroso-ferric oxide, belongs to technical field of inorganic material.
Background technology
Ferroso-ferric oxide（Fe3O4）It is a kind of important inverse spinel ferrite, is the soft magnetic material being most widely used
One of.Ferroso-ferric oxide is rich in natural magnetite, widely distributed.Due to its abundant resource, cheap price, and room temperature
Magnetic is preferable, has extensive purposes in fields such as magnetic material, pigment.With the informationization of society and answering for nanometer technology
With, research of the people to ferroso-ferric oxide also complete one gone to from macroscopic view it is microcosmic, the size of particle from micron, sub-micron to
The course of nano-scale transition, the nanometer technology of this granular oneself for the development in many fields create condition.With it is common
Ferroso-ferric oxide is compared, nano ferriferrous oxide powder（Particle diameter is in the range of 5 ~ 100nm）, quasi-zero dimension category should be belonged to（Size
Between atom, molecule and macroscopic solid）, there are many special performances, nano ferriferrous oxide is commonly used for recording materials, face
Material, magnetic fluid material, catalyst, magnetic macromolecular microsphere and electronic material etc., its in biological technical field and medical domain also
There is good application prospect.
The ferroso-ferric oxide of different sizes has different performances.Such as four oxidations three of 100 ~ 300nm scope particle diameters
Iron ultramicro magnetic particulate, because its chemical stability is good, raw material is easy to get, cheap, is to prepare magnetic ink and duplicating powder
Important materials, it has also become important one kind in inorganic pigment, be widely used in the fields such as coating, ink.Particle diameter 10nm or so
The suitable interfacial agent of the adsorption of ferroso-ferric oxide, is dispersed in polarity and nonpolar carrier fluid, can make
Into magnetic liquid new material, it has the mobility of liquid, and superfine powder is magnetic recording material, magnetic flow in the electronics industry
The important component of body, gas humidity-sensitive material, it is a focus of current field of nanometer material technology and field of functional materials.Magnetic simultaneously
Iron ore in addition to as microwave absorbing material, it still synthesize ammonia, F.T synthesis, water gas shift reaction, butylene and ethylbenzene dehydrogenation and
The excellent catalyst of oxidative dehydrogenation.
With it is high-tech develop rapidly and to synthesis new material there is an urgent need to the exploitation of nano ferriferrous oxide, grind
Study carefully and be highly valued, research worker oneself by distinct methods prepared different-shape, different-grain diameter be distributed nanometer four
Fe 3 O, but due to the particle very little of nano ferriferrous oxide, itself has magnetic again, so easily reunite, simultaneously because
Active higher, the less stable of nano ferriferrous oxide, its Fe2+It is oxidized easily, therefore stability is also asking of being considered as
Topic.
The iron content acid solution occurred at present in metallurgy industry, for example, steel plant's hydrochloric acid or sulfuric acid wash the waste liquid of steel, or
When improving chromite ferrochrome ratio using acid leaching process, substantial amounts of iron content waste liquid is generated, iron ion, chlorine are mainly contained in its composition
Ion or sulfate ion etc..If iron content waste liquid is directly discharged in nature, the exploitation value of its application is not only lost
Value, and cause environmental pollution.The more iron content process for treating waste liquor of commercial Application mainly has neutralisation and sulphate of iron method.In
It is simple and easy to do with method, but the iron ion in water fails to utilize.Sulphate of iron rule can produce ferrous sulfate, polymeric iron and pigment
Deng product.
The content of the invention
It is an object of the invention to provide a kind of method that nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid, with effective
Realize the recycling to the iron ion in waste liquid.
The method that the present invention prepares nano ferriferrous oxide, it is under magnetic stirring, dispersant to be added in iron content waste liquid
Stir, add cushioning liquid（pH 9~11）Stir；Then by mixed solution under ventilation condition autoxidation 1 ~
4 h；By magnetic force by the debris buildup of product after the completion of oxidation, separate, washing, produce nano ferriferrous oxide sample.
The iron concentration of the iron content waste liquid is 0.2 ~ 0.3 mol/L.In iron content waste liquid, the concentration of iron ion is such as less than
This value, iron concentration can be improved by adding a small amount of iron filings；If above this value, this concentration range can be reached by dilution.
Influence of the iron liquid concentration to nano ferriferrous oxide sample：Iron liquid concentration is smaller, and the particle diameter of product is smaller, evenly, but point
It is poor to dissipate property.Iron liquid concentration is bigger, and the particle diameter of product is larger, and dispersiveness is preferably.When the concentration of iron ion in iron content waste liquid is
During 0.2 ~ 0.3 mol/L, the particle diameter of product is all in 100 below nm, and particle diameter distribution is uniform, favorable dispersibility.
Dispersant is the starch solution that mass concentration is 0.5 ~ 1%.Influence of the dispersant to nano ferriferrous oxide sample：
During without starch dispersant, ferro element and oxygen element institute accounting and are most connect in all numerical value closer to theoretical value in product
Nearly theoretical value, nitrogen is also minimum, the content highest of ferroso-ferric oxide, impurity in product with chlorine element proportion
At least, product is most pure.But agglomeration can occur for no dispersant, product；And after adding starch dispersant, product
Quality substantially increases, it may be possible to which, because starch dispersant has tack, it is while nano ferriferrous oxide pattern is changed
Particle surface has been attached to, or because when nano ferriferrous oxide particle attracts each other, a part of starch dispersant has been pressed from both sides
Between particle.The addition volume of dispersant solution is 1 with iron content waste liquid volume:1~1:When 2, the particle diameter of product is small,
Particle diameter is in below 100nm；Evenly, dispersiveness is more preferable for particle diameter.
The preparation of the cushioning liquid：Chloride leach is made into 0.1 ~ 0.5mol/L solution in deionized water, added
Enter the ammonium chloride solution of same concentration, it is 1 to make the volume ratio of ammonium chloride and ammoniacal liquor:0.5~1:32, it is molten that the buffering that pH is 9 ~ 11 can be obtained
Liquid.The addition of buffer solution and the volume ratio 1 of iron content waste liquid:4~1:5.Shadow of the cushioning liquid to nano ferriferrous oxide sample
Ring：During without buffer solution, ferro element and oxygen element proportion are closer to theoretical value in product, the proportion of nitrogen and chlorine element
It is significantly smaller, illustrate that product is purer during no buffer solution.But phenomenon of flocculating easily occurs for product, particle diameter is big.And add buffer solution
Afterwards, product particle diameter is smaller, and evenly, dispersiveness is preferable, and particle size is in below 100nm for particle diameter.
Influences of the pH to nano ferriferrous oxide sample：With pH increase, iron, oxygen in the ferroso-ferric oxide sample of generation
The ratio between element is closer to theoretical value, and nitrogen and chlorine element proportion are significantly smaller, and product is purer, and impurity is less；Particle diameter distribution
Evenly, dispersiveness is more preferable.As pH to 9 ~ 11, particle size is in below 100nm.
The washing is first to be cleaned twice with 5% ammoniacal liquor, then is cleaned twice with ultra-pure water, is then cleaned three times with ethanol,
Fully to wash the impurity in product off.
In summary, the present invention is prepared in the technique of nano ferriferrous oxide is prepared, and it is in the range of 9 ~ 11 to add pH
Buffer solution, in the case of adding starch dispersant, product particle diameter is small, and particle diameter distribution is uniform, good dispersion；It is not added with starch dispersion
Agent, no cushioning liquid, product is although pure, and impurity does not almost have, the reunion but product easily flocculates, bad dispersibility.
The present invention has advantages below compared with the prior art：
1st, the present invention is raw material using industrial iron content waste liquid, by coprecipitation, has prepared nano ferriferrous oxide, four
The particle diameter of Fe 3 O sample is smaller, in below 100nm；And particle diameter distribution is uniform, dispersiveness is preferably；
2nd, the processing step for preparing nano ferriferrous oxide of the invention is simple, and there have that cost is low, pollution-free, technique is simple etc. to be excellent
Point；
3rd, the present invention is also reclaimed, no while nano ferriferrous oxide is prepared to the ferro element in Industry Waste iron liquid
Only there is actual economic value, it is often more important that there is the environment protection significance of reality.
Brief description of the drawings
Fig. 1 is scanning electron microscope (SEM) photograph and the elementary analysis of ferroso-ferric oxide（0.3mol/L iron liquid, no starch, 5mL bufferings
Liquid, pH 9）.N：01.91%, O：18.54%, Cl：00.66%, Fe：78.89%.
Fig. 2 is scanning electron microscope (SEM) photograph and the elementary analysis of ferroso-ferric oxide（0.3mol/L iron liquid, 25mL starch, 5mL bufferings
Liquid, pH 9）.N：04.02%, O：34.22%, Cl：01.27%, Fe：60.49%.
Fig. 3 is scanning electron microscope (SEM) photograph and the elementary analysis of ferroso-ferric oxide（0.3mol/L iron liquid, 25mL starch, 5mL bufferings
Liquid, pH 11）.N：04.68%, O：36.15%, Cl：01.52%, Fe：57.65%.
Embodiment
Below by preparation of the specific embodiment to a kind of nano ferriferrous oxide material of the present invention and for industrial scrap iron
The recycling of liquid is described in detail.
Embodiment 1
（1）The preparation of cushioning liquid：Accurate weighing 0.5350g ammonium chlorides, 100mL volumetric flasks are settled to deionized water dissolving
In, as 0.1mol/L ammonium chloride solution.Prepare the ammonia spirit with concentration：7.7mL concentrated ammonia liquors are pipetted, add water to be settled to
In 1000mL.The volume ratio of ammonium chloride and ammoniacal liquor is 2:During 1 mixing, the cushioning liquid that pH is 9 can be obtained, it is stand-by；
（2）The preparation of starch solution：5.00g starch is weighed, with deionized water dissolving, 500 mL is settled to, produces 1% starch
Solution, it is stand-by；
（3）The synthesis of nano ferriferrous oxide：Add containing the mL of iron content waste liquid 25 that concentration of iron is 0.3mol/L, open in beaker
Open magnetic stirring apparatus to be stirred, add starch solution 25mL, add the cushioning liquid 5mL that pH is 9, close magnetic stirring apparatus；
After beaker is placed in into the h of ventilation autoxidation 1, beaker is placed on magnet, thing sedimentation aggregation to be generated will with rubber head dropper
Supernatant suctions out, then clean twice with 5% ammoniacal liquor, ultra-pure water cleaning twice, alcohol washes three times, in cleaning process if because
Product is magnetic and can not fully cleaned, and can be stirred with glass bar.Sample is placed in after ventilation spontaneously dries and sealed
Preserve.
The scanning electron microscope (SEM) photograph of the ferroso-ferric oxide of generation such as Fig. 2：Particle size is in below 100nm, and uniform particle sizes, point
It is preferable to dissipate property.Elementary analysis：N：04.02%, O：34.22%, Cl：01.27%, Fe：60.49%.
Embodiment 2
（1）The preparation of ammonium chloride, ammoniacal liquor and starch solution：With embodiment 1.The volume ratio of ammonium chloride and ammoniacal liquor is 1:32 mixing
When, the cushioning liquid that pH is 11 can be obtained, it is stand-by；
（2）The synthesis of nano ferriferrous oxide：Add containing the 25 mL iron content waste liquids that concentration of iron is 0.3mol/L, open in beaker
Open magnetic stirring apparatus to be stirred, add the mL of starch solution 25, add the mL of cushioning liquid 5 that pH is 11, close magnetic agitation
Device；After beaker is placed in into ventilation autoxidation 1h, beaker is placed on magnet, thing sedimentation aggregation to be generated, with rubber head dropper
Supernatant is suctioned out, then cleaned twice with 5% ammoniacal liquor, ultra-pure water cleans twice, and alcohol washes are three times；Sample is placed in ventilation
Place is sealed after spontaneously drying.
The scanning electron microscope (SEM) photograph of the ferroso-ferric oxide of generation such as Fig. 3：Particle size is in below 100nm, and uniform particle sizes, point
It is preferable to dissipate property.Elementary analysis：N：04.68%, O：36.15%, Cl：01.52%, Fe：57.65%.
Claims (8)
- It is under magnetic stirring, to add in iron content waste liquid 1. preparing the method for nano ferriferrous oxide using industrial ferrous contained waste liquid Enter dispersant to stir, add pH and stirred for 9 ~ 11 cushioning liquid；Then by mixed solution under ventilation condition from So oxidation；By magnetic force by the debris buildup of product after the completion of oxidation, separate, washing, produce nano ferriferrous oxide sample Product.
- 2. the method for nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid as claimed in claim 1, it is characterised in that：It is described Iron concentration is 0.2 ~ 0.3 mol/L in iron content waste liquid.
- 3. the method for nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid as claimed in claim 1, it is characterised in that：It is scattered Agent is the starch solution that mass concentration is 0.5 ~ 1%.
- 4. the method for nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid as claimed in claim 3, it is characterised in that：It is scattered The addition of agent and the volume ratio 1 of iron content waste liquid:1~1:2.
- 5. the method for nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid as claimed in claim 1, it is characterised in that：Buffering The preparation of solution：Chloride leach is formed to 0.1 ~ 0.5mol/L solution in deionized water, the ammoniacal liquor of same concentration is added, makes The volume ratio of ammonium chloride and ammoniacal liquor is 1:0.5~1:32, it is made into the cushioning liquid that pH is 9 ~ 11.
- 6. the method for nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid as claimed in claim 1, it is characterised in that：Buffering The addition of liquid and the volume ratio 1 of iron content waste liquid:4~1:5.
- 7. the method for nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid as claimed in claim 1, it is characterised in that：It is described The time of autoxidation is 1 ~ 4 h.
- 8. the method for nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid as claimed in claim 1, it is characterised in that：It is described Washing is first to be cleaned twice with 5% ammoniacal liquor, then is cleaned twice with ultra-pure water, is then cleaned three times with ethanol.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109850951A (en) * | 2019-04-01 | 2019-06-07 | 中钢集团南京新材料研究院有限公司 | A method of iron oxide black is prepared using titanium white by product object |
| CN110194490A (en) * | 2019-06-14 | 2019-09-03 | 长春工程学院 | A kind of method and apparatus preparing magnetic nano ferroferric oxide |
| CN111672466A (en) * | 2020-06-07 | 2020-09-18 | 桂林理工大学 | Preparation method and application of magnetic iron oxide/mulberry tree stalk biochar composite material |
| CN114259985A (en) * | 2021-12-21 | 2022-04-01 | 中州水务控股有限公司 | Method for preparing biochar by using kitchen waste as biomass |
| CN115947379A (en) * | 2022-12-30 | 2023-04-11 | 江苏理工学院 | Paramagnetic micron material and preparation method thereof |
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| CN111672466A (en) * | 2020-06-07 | 2020-09-18 | 桂林理工大学 | Preparation method and application of magnetic iron oxide/mulberry tree stalk biochar composite material |
| CN114259985A (en) * | 2021-12-21 | 2022-04-01 | 中州水务控股有限公司 | Method for preparing biochar by using kitchen waste as biomass |
| CN115947379A (en) * | 2022-12-30 | 2023-04-11 | 江苏理工学院 | Paramagnetic micron material and preparation method thereof |
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