CN103818966A - Large-specific surface area superfine powdery iron oxide red spray roasting method - Google Patents
Large-specific surface area superfine powdery iron oxide red spray roasting method Download PDFInfo
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- CN103818966A CN103818966A CN201210466377.7A CN201210466377A CN103818966A CN 103818966 A CN103818966 A CN 103818966A CN 201210466377 A CN201210466377 A CN 201210466377A CN 103818966 A CN103818966 A CN 103818966A
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Abstract
The invention discloses a large-specific surface area superfine powdery iron oxide red spray roasting method. Superfine iron oxide red with a specific surface area of more than 5.0m<2>/g can be directly produced from waste acid fluid produced by a pickling unit sequentially by wastewater collection, PH value regulation, purification, precipitation, concentration, dilution, surfactant addition, stirring and roasting, the purity of the iron oxide red can reach more than 99.5 percent, and chemical performance indexes of the iron oxide red meet requirements on those of first-grade products.
Description
Technical field
The present invention relates to steel plate acid-washing waste water reclamation treatment technology, more particularly, relate to a kind of red iron oxide spray roasting method of ultrafine powder, high-specific surface area.
Background technology
Steel plate acid-washing is the indispensable operation of cold rolling production.Steel plate produces a large amount of spent acid solutions after chlorohydric acid pickling, and its main component is iron protochloride and hydrochloric acid, and a small amount of iron(ic) chloride.According to current domestic pickling unit layout, its spent pickle liquor all needs to recycle, and the recovery method adopting is substantially all spray roasting.The operational path of this method is, by spent acid solution desiliconization removal of impurities, carries out high-temperature roasting, generates regeneration hydrochloric acid, turns back to pickling zone and continues to use.Meanwhile, the iron in spent acid solution becomes red iron oxide, and this red iron oxide is the main raw material of ferrite magnetic material.The production technique of existing red iron oxide, is all using iron protochloride as raw material, through 700 ℃ of left and right roastings, produces pulverous red iron oxide.
As a kind of main raw material of magneticsubstance, after red iron oxide is mixed with other Multimetal oxide, adopt ceramic process to form a kind of nonmetal magnetic material through special chemical reaction, there is unique soft magnetism and higher specific conductivity, be the desirable magneticsubstance in frequency applications field, be widely used at present the fields such as televisor, receiving set, video camera, computer, watch-dog, surveying instrument, automatization control and communication equipment.From the trend of current domestic magnetic industry development and the development of red iron oxide production technique, industrial scale constantly expands, and output is doubled and redoubled, and the demand of higher-grade, high-quality brown iron oxide is also increased rapidly.
The red iron oxide that existing employing spray roasting explained hereafter goes out, its performance index comprise two aspects: the one, chemical property, mainly comprises the content of ferric oxide, and the content of the impurity such as silicon, aluminium, manganese.Because acid regeneration all needs to carry out desiliconization removal of impurities as last, therefore, the red iron oxide purity that this kind of explained hereafter goes out is higher, and foreign matter content can be controlled at a lower level; Be physicals on the other hand, magneticsubstance comprises specific surface area, primary crystallization particle diameter, loose density to the requirement of brown iron oxide physical index.This wherein, the most key with specific surface area (BET) index again, the sintering process of magneticsubstance is solid phase diffusion reaction, brown iron oxide BET is larger, and between particle, reaction area is larger, and brown iron oxide activity is better, it is easier to react, can reduce the sintering temperature of magneticsubstance and shorten sintering time, improving the output of magneticsubstance, reducing energy consumption.According to the requirement of soft magnetic materials manufacturer, high-end Ferrite Material is more than 4.0m2/g to the requirement of BET, indivedual materials are led material as height, even require more than BET reaches 5.0m2/g, and the red BET level of Domestic Ferric Oxide is generally below 3.0m2/g, indivedual producers can reach 3.5m2/g left and right, but the requirement that does not also reach high-end Ferrite Material.
In order to meet the market requirement of high-specific surface area red iron oxide, the domestic post-processed that generally adopts red iron oxide, modal is the washing process of red iron oxide, its roughly step for batching, washing, stir, dry, ball milling, for example, Chinese patent 201120158859.7 discloses a kind of device that improves specific surface area of iron oxide, successively by dosing vessel, 1# agitated pool, 2# agitated pool, pearl mill, washing steel basin, settling bath, diaphragm filter press, drying machine and pulverizer serial connection form, can particle diameter is thick, the red iron oxide that BET is low, through batching, washing, stir, ball milling, the series of process such as dry, be processed into the red iron oxide of high BET.According to contriver's introduction, more than its BET can reach 5.0m2/g, meet the demand of high-end Ferrite Material.
Again for example, Chinese patent 200910049609.7 discloses a kind of purification method of dry-type iron oxide powder solid, by brown iron oxide is carried out to de-salted water washing; Brown iron oxide dirty solution after washing is carried out to press filtration, make its solid-liquid separation; Gained mud cake is carried out to predrying, broken, kiln dried, finally grind with vibromill.
Above-mentioned two patent documentations, specific implementation process difference, its operational path is all roughly the treatment process that adopts washing, ball milling, though can meet the production requirement of high BET red iron oxide, the problem existing is also clearly:
1, adopt washing, ball-milling technology, need to increase specific equipment and place newly, relate to related investment higher.
2, adopt above-mentioned technique, larger to energy consumption, as the de-salted water using in water washing process, the combustion gas using in drying process etc. are larger to energy consumption, cost impact.
3, in water washing process, can produce the sewage that contains in a large number iron oxide dust, deal with the secondary pollution that is easy to cause environment improperly
4, in mechanical milling process, because red iron oxide dust is meticulous, there is certain environmental protection risk, also unfavorable to relevant operating personnel's Occupational health.
5, in water washing process, have quite a few red iron oxide with sewage discharge, the lumber recovery of whole technique is not high.
Summary of the invention
For the above-mentioned shortcoming existing in prior art, the object of this invention is to provide a kind of red iron oxide spray roasting method of ultrafine powder, high-specific surface area, the red iron oxide obtaining after roasting has high-specific surface area.
For achieving the above object, the present invention adopts following technical scheme:
The red iron oxide spray roasting method of this ultrafine powder, high-specific surface area, comprises the following steps:
A. collect the spent pickle liquor of chlorohydric acid pickling unit, and add waste iron filing or iron scale, make generation FeCl as much as possible in waste liquid
2and FeCl3, to consume the HCL in waste liquid;
B. add ammoniacal liquor, regulate waste liquid pH value to 3.5～5.0, then pass into air, generate the Fe(OH with flocculating effect)
3, in order to remove the heavies in spent acid;
C. add polyacrylamide coagulant aids, the impurity further flocculating in spent acid, to improve sedimentation speed;
D. leave standstill waste liquid, after precipitation is complete, filter;
E. the waste liquid after filtering is heated, make the moisture in waste liquid evaporate and concentrate, the waste liquid iron-holder after control is concentrated is between 200g/L～250g/L;
F. add the technical hydrochloric acid that concentration is 37wt%, in reducing waste liquid pH value, the iron level in waste liquid is diluted to below 150g/L;
G. add nonionic surfactant, to improve the diffusibleness of iron ion, further disperse the iron ion in waste liquid;
H. more than waste liquid being carried out to mechanical stirring 30min, and send into spray roasting stove by spray gun, control maturing temperature at 600 ℃～800 ℃, the time, at 1.5～2.5 hours, obtains the red iron oxide of ultrafine powder, high-specific surface area.
In step C, 1～2wt% that the addition of described polyacrylamide coagulant aids is waste liquid amount.
In step e, described Heating temperature to 70 ℃～100 ℃.
In step G, described nonionic surfactant is a kind of or composite in alkylphenol polyoxyethylene, sodium alkyl benzene sulfonate, fatty alcohol-polyoxyethylene ether.
In step G, 0.5～2.0wt% that the addition of described nonionic surfactant is waste liquid amount.
In technique scheme, the red iron oxide spray roasting method of ultrafine powder of the present invention, high-specific surface area, successively by wastewater collection, regulate pH value, removal of impurities, precipitation, concentrated, dilution, add tensio-active agent, stirring and roasting, the spent acid solution that pickling unit can be produced, it is red that direct production goes out the superfine iron oxide of specific surface area more than 5.0m2/g, and red iron oxide purity is more than 99.5%, and every chemical property index arrives the requirement of first grade.
Embodiment
In existing spray roasting technique, spent pickle liquor is directly sent to stoving oven, sprays into fine droplet by nozzle atomization, and first small droplets is heated to boiling and vaporization temperature, FeCl when by stoving oven
2particle is calcined into free hydrogenchloride and ferric oxide while decline in stove, that is:
4FeCl
2+4H
2O+O
2=2Fe
2O
3+8HCl
Here said ferric oxide, i.e. red iron oxide.Under micro, red iron oxide particle is spheroid tiny, hollow, its spherical shell porous surface.
Concentrated acid mist is ejected into red iron oxide particle from nozzle and forms, and is broadly divided into following steps:
Acid mist enters after stove, contacts with high-temperature gas, and moisture evaporation, causes free acid and iron protochloride in acid mist concentrated, and liquid particle viscosity and surface tension increase, and make liquid particle glomeration.
Water and hydrogenchloride evaporation, the iron protochloride in particle and hydrochloric acid is the tiny FeCl of concentrated generation further
2crystallization.
Drop surface water and hydrogenchloride evaporation, particle surface forms FeCl
2duricrust, water and hydrogenchloride continue evaporation, housing thickening by housing.
Particle deadweight reduces, and lowering speed is hurried to slow down, and in high-temperature zone, the residence time increases, and causes FeCl
2melting, and react generation ferric oxide (Fe with oxygen
2o
3), covering particle outermost layer, grain diameter is substantially fixed.
FeCl in particle
2all crystallizations, Fe
2o
3in particle, form cavity, in cavity, be full of water vapour and hydrogen chloride gas.
Temperature constantly raises, and cavity internal gas pressure constantly increases until break through shell, Fe
2o
3on particle with pore.The FeCl of remnants in particle
2total overall reaction becomes Fe immediately
2o
3.
From the forming process of red iron oxide particle, the clustering phenomena of red iron oxide particle is the spontaneous phenomenon of one that surface free energy reduces, at the granuloplastic initial stage, specific surface area, the surface of particle can sharply increase, cause system and powder in utmost point unsteady state, between particle, have spontaneous gathering to reduce the trend of system free energy.Another reverse side, in high-temperature reaction process, particle surface atom has very large activity, surface atom energy is much larger than inner nuclear energy, thereby makes particle surface atomic diffusion to adjacent particle surface, and the atomic linkage corresponding with it, form stable chemical bond, thereby form permanent hard aggregation.
Therefore, in a sense, solve the nascent intergranular agglomeration traits of red iron oxide, just can reduce the particle diameter of final particle, reach the object of increasing specific surface area.And avoid or reduce the reunion of nascent red iron oxide particle, the surface that need to reduce from the beginning particle can, if can find a kind of nucleation rate of method affect red iron oxide particle, improve the iron ion dispersion effect in spent pickle liquor, just can realize this purpose.
According to above-mentioned principle, a kind of ultrafine powder of the present invention and high-specific surface area red iron oxide spray roasting method, specifically comprise the following steps:
A. collect spent pickle liquor: the spent pickle liquor of chlorohydric acid pickling unit is collected, added waste iron filing or iron scale, make generation FeCl as much as possible in spent pickle liquor
2and FeCl
3, its objective is the HCL in as far as possible many consumption spent acid, reduce the usage quantity of follow-up ammoniacal liquor.
B. regulate waste liquid pH value: in the waste liquid of gained in steps A, add ammoniacal liquor, regulate pH value to 3.5～5.0, then pass into air, its objective is and generate the Fe(OH with flocculating effect)
3, in order to remove the heavies in spent acid.
C. waste liquid removal of impurities: add polyacrylamide coagulant aids in the waste liquid obtaining in step B, 1%～2wt% that addition is waste liquid amount, its objective is the impurity in further flocculation spent acid, improves sedimentation speed.
D. precipitation: the waste liquid obtaining in step C is left standstill to two hours, after precipitation is complete, filter.
E. concentrated: the waste liquid obtaining in step D is heated to 70 ℃～100 ℃, make moisture evaporation concentrating spent liquor in waste liquid, control the iron-holder of concentrated rear waste liquid between 200g/L～250g/L, its objective is the moisture in evaporation waste liquid, reduce the energy consumption of roasting link, and in minimizing roasting, moisture evaporates " capillary " phenomenon causing.
F. dilution: add the technical hydrochloric acid that concentration is 37wt% in the waste liquid obtaining in step D, in reducing waste liquid pH value, iron level in waste liquid is diluted to below 150g/L, its objective is the pH value that reduces waste liquid, and reduce the content of iron ion in unit volume
G. add promoting agent: in the waste liquid obtaining in step F, add nonionogenic tenside, addition is 0.5～2.0wt% of waste liquid amount, this nonionogenic tenside can adopt a kind of or composite in alkylphenol polyoxyethylene, sodium alkyl benzene sulfonate, fatty alcohol-polyoxyethylene ether, its objective is the diffusibleness that improves iron ion, further disperse the iron ion in waste liquid, reduce the agglomeration in roasting process.
H. stir and roasting: the waste liquid obtaining in step G is passed through more than mechanical stirring 30min, its objective is and improve the diffusion effect of promoting agent and add homogeneity, and then send into spray roasting stove by spray gun, maturing temperature is controlled at 600 ℃～800 ℃, roasting time is controlled at 1.5～2.5 hours, finally obtains the red iron oxide of ultrafine powder, high-specific surface area.
Embodiment 1
1) by 1m
3spent pickle liquor is collected, and adds 20kg waste iron filing;
2) add ammoniacal liquor, regulating waste liquid pH value is 4.5;
3) add polyacrylamide coagulant aids, addition is 10kg;
4) leave standstill 2 hours, after precipitation is complete, filter;
5) be heated to 90 ℃, transpiring moisture concentrating spent liquor, control iron-holder at 220g/L;
6) add the technical hydrochloric acid that concentration is 37wt%, when reducing waste liquid pH value, make iron level be diluted to 130g/L;
7) add 5kg sodium alkyl benzene sulfonate;
8) mechanical stirring 30min, sends into spray roasting stove by spray gun, and maturing temperature is controlled at 700 ℃, and roasting time is controlled at 2 hours, and institute's red iron oxide specific surface area that obtains is at 5.2m
2/ g.
Embodiment 2
1) by 10m
3spent pickle liquor is collected, and adds 100kg waste iron filing;
2) add ammoniacal liquor, regulating waste liquid pH value is 4.2;
3) add polyacrylamide coagulant aids, addition is 120kg;
4) leave standstill 2 hours, after precipitation is complete, filter;
5) be heated to 95 ℃, transpiring moisture concentrating spent liquor, control iron-holder at 210g/L;
6) add the technical hydrochloric acid that concentration is 37wt%, when reducing waste liquid pH value, make iron level be diluted to 115g/L;
7) add 60kg sodium alkyl benzene sulfonate;
8) mechanical stirring 30min, sends into spray roasting stove by spray gun, and maturing temperature is controlled at 720 ℃, and roasting time is controlled at 2 hours, and institute's red iron oxide specific surface area that obtains is at 5.1m
2/ g.
Embodiment 3
1) by 5m
3spent pickle liquor is collected, and adds 70kg waste iron filing;
2) add ammoniacal liquor, regulating waste liquid pH value is 3.8;
3) add polyacrylamide coagulant aids, addition is 60kg;
4) leave standstill 2 hours, after precipitation is complete, filter;
5) be heated to 85 ℃, transpiring moisture concentrating spent liquor, control iron-holder at 240g/L;
6) add the technical hydrochloric acid that concentration is 37wt%, when reducing waste liquid pH value, make iron level be diluted to 125g/L;
7) add 35kg sodium alkyl benzene sulfonate;
8) mechanical stirring 30min, sends into spray roasting stove by spray gun, and maturing temperature is controlled at 680 ℃, and roasting time is controlled at 2 hours, and institute's red iron oxide specific surface area that obtains is at 5.5m
2/ g.
In sum, adopt spray roasting method of the present invention, the waste liquid that can be produced by pickling unit, direct production goes out specific surface area at 5.0m
2superfine iron oxide more than/g is red, and red iron oxide purity is more than 99.5%, and every chemical property index arrives the requirement of first grade.
And, be that the iron protochloride through desiliconization processing, iron(ic) chloride clear liquid are concentrated, transpiring moisture, transfer to dilute its iron concentration with technical hydrochloric acid, can make iron concentration in unit volume drop reduce, red iron oxide initial particle attenuates, and has reduced the generation of particle agglomeration.Meanwhile, because moisture in waste liquid reduces, reduce moisture in roasting process and evaporated " capillary " phenomenon causing, avoided the stronger bonding force of formation between colloidal particle.
On the other hand, adopt tensio-active agent to improve the dispersion effect of iron ion, especially be adsorbed on the active site of nucleating surface by promoting agent, form local discrete wrap film, change the contact angle of solid-liquid, reduce the surface tension of solid-liquid interface in waste liquid, thereby prevented the gathering of solid particulate in liquid medium.
Therefore, spray roasting method of the present invention is produced unit applicable to the red iron oxide of all employing spray roasting techniques, adopt the present invention can significantly improve the physicals of red iron oxide, acquisition stable chemical performance, the high grade red iron oxide that reactive behavior is good, make rapid progress at magnetic industry development, today that technology is constantly updated, adopts the present invention can significantly promote the raw-material added value of red iron oxide, has boundless market application foreground.
Those of ordinary skill in the art will be appreciated that, above embodiment is only for the present invention is described, and be not used as limitation of the invention, as long as within the scope of connotation of the present invention, variation, modification to the above embodiment all will drop within the scope of claims of the present invention.
Claims (5)
1. a red iron oxide spray roasting method for ultrafine powder, high-specific surface area, is characterized in that,
Comprise the following steps:
A. collect the spent pickle liquor of chlorohydric acid pickling unit, and add waste iron filing or iron scale, make generation FeCl as much as possible in waste liquid
2and FeCl3, to consume the HCL in waste liquid;
B. add ammoniacal liquor, regulate waste liquid pH value to 3.5～5.0, then pass into air, generate the Fe(OH with flocculating effect)
3, in order to remove the heavies in spent acid;
C. add polyacrylamide coagulant aids, the impurity further flocculating in spent acid, to improve sedimentation speed;
D. leave standstill waste liquid, after precipitation is complete, filter;
E. the waste liquid after filtering is heated, make the moisture in waste liquid evaporate and concentrate, the waste liquid iron-holder after control is concentrated is between 200g/L～250g/L;
F. add the technical hydrochloric acid that concentration is 37wt%, in reducing waste liquid pH value, the iron level in waste liquid is diluted to below 150g/L;
G. add nonionic surfactant, to improve the diffusibleness of iron ion, further disperse the iron ion in waste liquid;
H. more than waste liquid being carried out to mechanical stirring 30min, and send into spray roasting stove by spray gun, control maturing temperature at 600 ℃～800 ℃, the time, at 1.5～2.5 hours, obtains the red iron oxide of ultrafine powder, high-specific surface area.
2. the red iron oxide spray roasting method of ultrafine powder as claimed in claim 1, high-specific surface area, is characterized in that:
In step C, 1～2wt% that the addition of described polyacrylamide coagulant aids is waste liquid amount.
3. the red iron oxide spray roasting method of ultrafine powder as claimed in claim 1, high-specific surface area, is characterized in that:
In step e, described Heating temperature to 70 ℃～100 ℃.
4. the red iron oxide spray roasting method of ultrafine powder as claimed in claim 1, high-specific surface area, is characterized in that:
In step G, described nonionic surfactant is a kind of or composite in alkylphenol polyoxyethylene, sodium alkyl benzene sulfonate, fatty alcohol-polyoxyethylene ether.
5. the red iron oxide spray roasting method of the ultrafine powder as described in claim 1 or 4, high-specific surface area, is characterized in that:
In step G, 0.5～2.0wt% that the addition of described nonionic surfactant is waste liquid amount.
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| CN104671290A (en) * | 2015-03-20 | 2015-06-03 | 王浩 | Method for preparing iron oxide red by pickling sludge |
| CN105036721A (en) * | 2015-06-24 | 2015-11-11 | 南京梅山冶金发展有限公司 | Method for preparing permanent-magnet ferrite pre-sintered material |
| CN105753068A (en) * | 2016-02-04 | 2016-07-13 | 河北爱德斯蒂尔环保科技有限公司 | Method for preparing iron oxide red through steel acid pickling waste liquor |
| CN110371929A (en) * | 2019-07-23 | 2019-10-25 | 马鞍山钢铁股份有限公司 | A kind of acid regeneration preprocess method and system |
| CN110980814A (en) * | 2019-12-31 | 2020-04-10 | 上海宝钢磁业有限公司 | Method for preparing ferric oxide by regenerating waste acid of steel rolling mill unit |
| CN111573739A (en) * | 2020-06-09 | 2020-08-25 | 首钢集团有限公司 | Method for producing iron oxide red from high manganese steel waste acid liquid |
| CN115355515A (en) * | 2022-09-02 | 2022-11-18 | 生态环境部南京环境科学研究所 | Spray roasting process for waste acid liquor treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110371929A (en) * | 2019-07-23 | 2019-10-25 | 马鞍山钢铁股份有限公司 | A kind of acid regeneration preprocess method and system |
| CN110980814A (en) * | 2019-12-31 | 2020-04-10 | 上海宝钢磁业有限公司 | Method for preparing ferric oxide by regenerating waste acid of steel rolling mill unit |
| CN111573739A (en) * | 2020-06-09 | 2020-08-25 | 首钢集团有限公司 | Method for producing iron oxide red from high manganese steel waste acid liquid |
| CN115355515A (en) * | 2022-09-02 | 2022-11-18 | 生态环境部南京环境科学研究所 | Spray roasting process for waste acid liquor treatment |
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