CN101837435A - Method for preparing casting covering slag by utilizing stainless steel cold-rolling pickling wastewater - Google Patents
Method for preparing casting covering slag by utilizing stainless steel cold-rolling pickling wastewater Download PDFInfo
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- CN101837435A CN101837435A CN200910047959A CN200910047959A CN101837435A CN 101837435 A CN101837435 A CN 101837435A CN 200910047959 A CN200910047959 A CN 200910047959A CN 200910047959 A CN200910047959 A CN 200910047959A CN 101837435 A CN101837435 A CN 101837435A
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Abstract
The invention discloses a method for preparing casting covering slag by utilizing stainless steel cold-rolling pickling wastewater, which comprises the following steps of: after the stainless steel cold-rolling pickling wastewater is chemically reduced, adding a first neutralizing agent into a front-section precipitation tank to complex and precipitate heavy metal ions in the wastewater, concentrating, dehydrating and drying precipitates and returning the precipitates to a metallurgical process for reuse; making supernatant fluid enter a rear-section precipitation tank, adding a second neutralizing agent and a coagulant, discharging the supernatant fluid after the supernatant fluid meets the standard, and concentrating, dehydrating, drying and crushing rear-section sludge primarily comprising a calcium salt component to obtain a dry sludge base material; uniformly mixing 20 to 60 weight percent of dry sludge base material and 40 to 80 weight percent of auxiliary materials, melting the mixture in a high-temperature furnace after performing agglomeration or palletizing on the mixture, and crushing, grinding and milling the treated mixture to obtain a pre-melted base material of the covering slag; and adding 2 to 15 weight percent of carbonaceous material and 0 to 5 weight percent of bonding agent into the pre-melted base material of the covering slag, and then palletizing, drying and sieving the mixture to obtain the finished product of the covering slag.
Description
Technical field
The invention belongs to the comprehensive utilization technique field of stainless steel cold-rolling pickling wastewater, particularly a kind of back segment mud that produces with electronation-fractional precipitation PROCESS FOR TREATMENT stainless steel cold-rolling pickling wastewater is raw material, prepares the method for casting covering slag.
Background technology
In the surface treatment process of stainless-steel cold-rolling coiled sheet, can discharge a large amount of pickling waste waters, wherein T.Fe, Cr
6+, T.Cr, Ni
2+, Zn
2+, Pb
2+, F
-, pollutant load height such as SS, harm be big, must discharge through just allowing behind the governance for reaching standard.
For technology maturation, operating cost and consideration easy to maintenance etc., improvement technology to stainless steel cold-rolling pickling wastewater is mainly electronation-precipitation method at present, be the multichannel pickling waste waters after regulating reservoir mixes, (reducing agent adopts NaHSO more to take the multi-grade chemical reduction
3, Na
2SO
3, FeSO
4Deng) and the mode of multistage neutralization (nertralizer is generally milk of lime) all contaminations is transferred in the cold rolling mud, waste water effluxes after up to standard.The shortcoming of this technology is: up to standard in order to ensure water outlet, often need to add excessive milk of lime, this can cause, and cold rolling sludge yield is big, complicated component, processing and disposal difficulty are big, integrated cost to its processing is quite high, and be easy to generate secondary pollution in the above-mentioned processing procedure, thereby this type of mixing sludge is identified as hazardous waste (being numbered HW17 in the China national hazardous waste catalogue).For example, the pickling waste waters amount is 100m
3The tame stainless steel enterprise of/h, the output of mixing sludge promptly surpasses 1.5 ten thousand t/a, and these mud can't utilize in the factory, and annual outer committee handles, the expense of disposal is up to five or six hundred ten thousand yuan.
In order to solve the problem that cold rolling mud is difficult to utilize, people had once proposed several different methods, but had all run into such or such problem.For example, the Chinese patent publication number is that sludge curing processing cost height, volume that CN1451495A and CN101066826 put down in writing are big, deposits with the passing of time Cr
6+, Ni
2+Leaching concentration in heavy metal can surpass limit value; The Chinese patent publication number is that mud that CN1935709 put down in writing is baked bricks and Cr can be taken place in the process
3+Secondary oxidation, the fluorine steam that volatilizes can make a very bad impression to habitat on every side, (for example, the Longjing tea output in somewhere, Hangzhou, because of near little brickkiln too much the underproduction half), country has prohibited this type of disposal approach of cold rolling mud; Even if the Chinese patent publication number is that the mud that CN1061948 put down in writing is very little as the cement ingredient volume, also causes problems such as ambient air contamination, rotary kiln kilneye crust, air door place fouling corrosion easily, even can have influence on the direct motion of original technology; The Chinese patent publication number is that mud that CN1272408, CN101058436, CN101066827, CN101070564 and CN1827802 are all put down in writing leaches step by step or heavy metal element equipment complexity is reclaimed in high-temperature roasting, technological process is long, cost is higher, and the disposal and the energy consumption problem of waste water and dregs can take place; The Chinese patent publication number is to obtain alloy block after mud that CN1733628 and CN101092662 put down in writing and flux, the fuel reduction roasting to return metallurgical operation of a high price, do not have economy, content of beary metal in the mud is limited after all, and the low melting point in the while mud is Na particularly
2O and K
2O is extremely harmful to blast furnace; In addition, the simple and easy landfill of mud can pollute underground water and surrounding soil, and the mud security landfill is with high costs, and general enterprise is difficult to long-term payment.
Be difficult to handle at mixing cold rolling mud, recently people are at the source of cold-rolling pickling wastewater, proposed some new thinkings: the Chinese patent publication number is the extracting method that CN101096276 discloses chromium, nickel salt in a kind of stainless steel acid cleaning waste water, contain chromium, nickel salt product though can extract part by the acid solution leaching, but whole wet process medicament expense is difficult to effective utilization with a large amount of filter residues high, discharging, and also there is secondary pollution problem in the heavy metal concentrate; The Chinese patent publication number has been for CN 1418831A discloses the method that two-stage method is handled organic metal acid waste water, its essence is neutralizing zone and flocculation section separated to carry out, and overcomes the deficiency of one section neutralization, and the mud of this technology is still mixing sludge, be difficult to reuse.
Therefore, cold rolling mixing sludge is as the difficult point of industry solid waste disposal, it utilizes approach to reclaim and three aspects expansion of recycling based on source decrement, wastewater treatment process optimization, mud classification, takes all factors into consideration economy, the feature of environmental protection and the reliability of technology.
Meanwhile, the inventor notices that covering slag is the essential auxiliary material that use in the molten steel foundry technology process, and it is to the quality important influence of strand or ingot casting, and steel per ton needs 0.5kg approximately.At present, the covering slag raw material all is to obtain through production by mineral matter (lime stone, fluorite, quartz, graphite etc.) and the chemical industry material (cement, carbon black, borax, lithium carbonate, soda ash etc.) that adopts stable components.For example; the present pre-melted type covering slag that generally uses; exactly several raw materials are mixed back high temperature melting, shrend, the levigate fritting base-material that becomes; again according to the performance requirement of various covering slags; in the fritting base-material, allocate suitable raw mineral materials into and adjust composition, performance; handle through granulation, drying, screening and make the covering slag finished product, price is up to 2000 yuan/ton.
By analysis, in the composition of the back segment mud that in utilizing chemical precipitation method segment processing stainless-steel cold-rolling waste water process, is produced, it contains Na, K, the elements such as Mg, Fe of a large amount of Ca, Al, Si, F and trace, and sludge components is comparatively stable, and fusing point is lower; Therefore, in the cold rolling wastewater processing procedure, if modified through composition, heavy metal sewage sludge is after leading portion precipitates fully substantially, and is follow-up with CaO, CaF
2, Al
2O
3Be main back segment mud, after materializations such as mummification, fragmentation are handled, can be used as one of the raw material of covering slag fully and high value added utilization in addition.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag, with solve the cold rolling Treatment of Sludge of acid-washing stainless steel that exists in the prior art with high costs, utilize in the big and process of difficulty and easily produce secondary pollution problem, reclaimed and utilize and cold rolling mud classifies: the contents of heavy metal elements height of leading portion mud, return metallurgical operation as raw material to utilize; Back segment mud F, constituent content height such as Ca, Al are then as being prepared into one of raw material of the required covering slag of molten steel casting production process.
Technical conceive of the present invention is as follows: stainless steel cold-rolling pickling wastewater is after electronation is handled, and the inventor changes the traditional mode that adds the mixed precipitation of superfluous lime breast, and takes segment processing technology.As shown in Figure 1, promptly in the leading portion sedimentation basin, add first nertralizer, so that Cr in the waste water
3+, Ni
2+, Fe
3+, Zn
2+, Pb
2+, Cu
2+, Fe
2+Etc. heavy metal ion generation complex-precipitation, precipitation is returned metallurgical operation and is reclaimed, utilizes as raw material after concentrated, dehydration, mummification; Supernatant enters in the back segment sedimentation basin, adds second nertralizer and coagulant again, so that supernatant effluxes the Ca in the waste water after up to standard
2+, F
-, SO
4 2-In the back segment mud that obtains after the generation complex-precipitation based on the calcium salt composition, this back segment mud obtains mud butt material again after concentrated, dehydration, mummification, pulverizing.Then, after this mud butt material and auxiliary material mixed,, can obtain the fritting base-material through broken, levigate and powder process successively again through melt process; Subsequently, allocate carbonaceous material and binding agent into after, handle through granulation, drying, screening again, the slag finished product promptly is protected.
Particularly, above-mentioned implementation step is respectively:
(1) stainless steel cold-rolling pickling wastewater is in electronation is handled, with the Cr more than 99%
6+Be reduced to Cr
3+, enter segment processing technology.At leading portion sedimentation basin inner control pH value is 9.0～10.0, and adds first nertralizer (for the liquid alkali of dissolubility, can be selected from a kind of or its combination in NaOH, KOH, the ammoniacal liquor), so that Cr in the waste water
3+, Ni
2+, Fe
3+, Fe
2+, Zn
2+, Pb
2+, Cu
2+Etc. heavy metal ion generation complex-precipitation, precipitation is returned metallurgical operation and is reclaimed, utilizes as raw material after concentrated, dehydration, mummification.
The main chemical reaction that takes place is as follows in the leading portion sedimentation basin:
Cr
3++3OH
-→Cr(OH)
3↓
Ni
2++2OH
-→Ni(OH)
2↓
Fe
3++3OH-→Fe(OH)
3↓
Fe
2++2OH-→Fe(OH)
2↓
Pb
2++2OH
-→Pb(OH)
2↓
Zn
2++2OH
-→Zn(OH)
2↓
Mn
2++2OH-→Mn(OH)
2↓
Cu
2++2OH
-→Cu(OH)
2↓
Mg
2++2OH-→Mg(OH)
2↓
Al
3++3OH-→Al(OH)
3↓
(2) through the leading portion post precipitation, supernatant enters pH value and is controlled at 8～9.5 back segment sedimentation basin, adds second nertralizer and coagulant, and this second nertralizer is Ca (OH)
2, coagulant is aluminum sulfate, alum, sodium aluminate, reaches a kind of or its combination in the aluminium salt such as aluminium polychloride (PAC), polyaluminium sulfate; The supernatant standard discharge, the Ca in the waste water
2+, F
-, SO
4 2-Obtain back segment mud based on the calcium salt composition Deng complex-precipitation takes place, back segment mud obtains mud butt material after concentrated, dehydration, mummification, pulverizing.
The main chemical reaction that takes place is as follows in the back segment sedimentation basin:
Ca
2++2F
-→CaF
2↓
xCa
2++yAl
3++zF
-→[CaxAly]Fz↓
Ca
2++SO
4 -→CaSO
4↓
Ca
2++CO
3 2-→CaCO
3↓
(3) by the mud butt material of 20～60wt%, all the other are that the charge ratio of auxiliary material (auxiliary material be wollastonite, clinker, quartz sand, power plant's flue dust, blast furnace granulated slag, electroslag, borax, fluorite, sodium carbonate, lithium carbonate etc. one or more) mixes; through agglomeration or make ball; melt process in high temperature furnace; the furnace temperature condition is 1100～1400 ℃; be cooled to normal temperature after coming out of the stove; through broken, levigate and powder process, slag fritting base-material is protected again.Wherein, the composition of above-mentioned mud butt material is: Ca0:40～50%; Al
2O
3: 15～25%; SiO
2: 4～10%; CaF
2: 15～30%; T.Fe:0～2%; H
2O :≤1%.
(4) in the fritting base-material, allocate carbonaceous material and binding agent into, this carbonaceous material is a kind of or its combination in coke blacking, graphite, carbon black, the acidifying graphite, binding agent is a kind of or its combination among starch, pitch, the CMC-Na; Through granulation, drying, screening and packing, the slag finished product promptly is protected.
The object of the present invention is achieved like this: a kind of method of utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag is characterized in that comprising the steps:
(1) stainless steel cold-rolling pickling wastewater is after electronation is handled, in the leading portion sedimentation basin, add first nertralizer, so that the heavy metal ion generation complex-precipitation in the waste water, precipitation is returned metallurgical operation and is reclaimed, utilizes as raw material after concentrated, dehydration, mummification; Wherein, described first nertralizer is a liquid-state soluble alkali, and the pH value scope of described leading portion sedimentation basin is 9.0～10.0;
(2) through the leading portion post precipitation, supernatant enters the back segment sedimentation basin, adds second nertralizer and coagulant then, the supernatant standard discharge, and obtaining back segment mud based on the calcium salt composition, this back segment mud is through concentrating, obtaining mud butt material after the dehydration, mummification, pulverizing; Wherein, described second nertralizer is Ca (OH)
2, described coagulant is an aluminium salt, the pH value scope of described back segment sedimentation basin is 8～9.5;
(the 3 mud butt material by 20～60wt%, all the other mix for the charge ratio of auxiliary material, after agglomeration or making ball, carry out melt process in high temperature furnace, again through broken, levigate and powder process and the slag fritting base-material that is protected;
(4) in described covering slag fritting base-material, add the carbonaceous material of 2～15wt% and the binding agent of 0～5wt%, handle through granulation, drying, screening again, the slag finished product promptly is protected.
Preferably, described liquid-state soluble alkali is at least a in NaOH, KOH or the ammoniacal liquor.
Preferably, Ca (OH) in the described step (2)
2Injected volume be more than 1.2 times of theoretical amount.
Preferably, described aluminium salt is at least a in aluminum sulfate, aluminum potassium sulfate, sodium aluminate, aluminium polychloride or the polyaluminium sulfate, and the dosage of this coagulant is for handling the water yield 0.1～1.0wt%.
Preferably, described auxiliary material is at least a in wollastonite, clinker, quartz sand, power plant's flue dust, blast furnace granulated slag, electroslag, borax, fluorite, sodium carbonate or the lithium carbonate.
Preferably, the chemical composition of described mud butt material is by weight percentage:
CaO：40～50％；
Al
2O
3：15～25％；
SiO
2：4～10％；
CaF
2：15～30％；
T.Fe：0～2％；
H
2O：≤1％。
Preferably, described high temperature furnace is shaft furnace or electric furnace.
Preferably, the furnace temperature condition of described melt process is 1100～1400 ℃, is cooled to normal temperature after coming out of the stove.
Preferably, described carbonaceous material is at least a in coke blacking, graphite, carbon black or the acidifying graphite.
Preferably, described binding agent is at least a among starch, pitch or the CMC-Na.
The present invention makes it compared with prior art owing to adopted above technical scheme, has the following advantages and good effect:
(1) changed present stainless-steel cold-rolling mixing sludge processing cost high, utilize in the big and process of difficulty and easily produce the present situation of secondary pollution, and, realized a kind of development and utilization measure of high added value with its main batching as continuous casting covering slag.
(2) the inventive method propose to the cold rolling wastewater segment processing, the mud segmentation can be reclaimed, the sludge yield of new technology is 70～80% of a traditional handicraft, this technology not only can be used for stainless steel cold-rolling pickling wastewater, can also extend in other the wastewater treatment that possesses conditions of similarity such as electroplating wastewater, breadboard industrial waste water, colored metallurgical industrial, aluminium industrial wastewater.
(3) the inventive method utilizes the back segment mud that produces in the chemical method segment processing cold rolling wastewater process to prepare the process route of continuous casting covering slag; in implementation process, do not need to increase special equipment; on original covering slag production line, can carry out, therefore help cost control.
(4) prepared covering slag chemical composition of the inventive method and phase constituent are evenly, heat insulation effect and spreadability be good; fusing evenly, the dross inclusion adsorption ability is strong, water absorption rate is low and the term of validity is long; adaptability to steel grade and casting parameters variation is strong, and production cost can significantly reduce.
(5) the aluminium content of the prepared covering slag of the inventive method is high slightly, is particularly useful for the covering slag as high aluminum steel.
Description of drawings
The invention will be further described below in conjunction with the drawings and specific embodiments.
Fig. 1 prepares the process chart of the method for casting covering slag for the present invention utilizes stainless steel cold-rolling pickling wastewater.
The specific embodiment
As shown in Figure 1, this is that the present invention utilizes stainless steel cold-rolling pickling wastewater to prepare the process chart of the method for casting covering slag.The inventive method is applied to a tame stainless steel enterprise cold-rolling pickling wastewater treating stations, and the daily wastewater treatment capacity of this treating stations is 100m
3/ h, process route originally are traditional Ca (OH)
2The excessive method that adds of one step produces the mixing sludge 50t/d that is difficult to utilize, and behind the process route that adopts two sections precipitations of the present invention, its mud total output is 42t/d, and correspondence has reduced 8t/d.
According to technology of the present invention, in the multi-grade chemical reduction of stainless steel cold-rolling pickling wastewater is handled, with the Cr more than 99%
6+Be reduced to Cr
3+Enter segment processing technology afterwards.In the leading portion sedimentation basin, pH value is controlled between 9.0～10.0, the Cr in the waste water
3+, Ni
2+, Fe
3+, Fe
2+, Zn
2+, Pb
2+, Cu
2+With NaOH complex-precipitation takes place etc. heavy metal ion in the leading portion sedimentation basin, heavy metal hydroxide mud returns metallurgical operation to reclaim, utilize as raw material after concentrated, dehydration, mummification; Then, supernatant enters in the back segment sedimentation basin, and adding calcium injected volume is that (theoretical amount herein is for making OH more than 1.2 times for theoretical amount
-In and whole heavy metal cation Me in the waste water
N+, required stoichiometric number) Ca (OH)
2As second nertralizer and dosage for the aluminium salt of handling the water yield 0.1～1.0wt% (in aluminum sulfate, aluminum potassium sulfate, sodium aluminate, aluminium polychloride or the polyaluminium sulfate at least a) as coagulant, pH value is 8～9.5 in the control pond, and back segment mud obtains mud butt material after concentrated, dehydration, mummification, pulverizing (its chemical composition is by weight percentage: CaO:40～50%; Al
2O
3: 15～25%; SiO
2: 4～10%; CaF
2: 15～30%; T.Fe:0～2%; H
2O :≤1%).
Subsequently, one or more of above-mentioned mud butt material and wollastonite, clinker, quartz sand, power plant's flue dust, blast furnace granulated slag, electroslag, borax, fluorite, sodium carbonate or lithium carbonate are prepared burden after (concrete proportion scale is as shown in table 1) evenly mix, carry out agglomeration again or make the ball processing, promptly in shaft furnace (lining-less, furnace wall water-cooling pattern), carry out melt process (concrete fusion furnace temperature is as shown in table 1) subsequently, be cooled to normal temperature after coming out of the stove.Then, melting charge is through broken, levigate and powder process, and slag fritting base-material promptly is protected.
Then; the above-mentioned fritting base-material that obtains is allocated into the binding agent (concrete proportion scale is as shown in table 1) of 2～15% carbonaceous materials and 0～5%; and the powder that weighing prepares put into granulating system in batches, the slag that promptly is protected after drying, the screening is packaged into finished product with this covering slag at last.
The concrete condition of the embodiment of the invention sees also table 1, and embodiment A wherein, B, C, D and E can be used as thin plate blanket continuous casting protective slag, silicon steel covering slag, continuous casting heavy slab peritectic steel covering slag, round steel crystallizer one of prescription of covering slag and conventional continuous casting covering slag respectively.
The chemical composition of table 1 embodiment of the invention and technological parameter
Those of ordinary skill in the art will be appreciated that, above embodiment is used for illustrating the present invention, and be not to be used as limitation of the invention, as long as in connotation scope of the present invention, all will drop in claims scope of the present invention variation, the modification of the above embodiment.
Claims (10)
1. a method of utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag is characterized in that comprising the steps:
(1) stainless steel cold-rolling pickling wastewater is after electronation is handled, in the leading portion sedimentation basin, add first nertralizer, so that the heavy metal ion generation complex-precipitation in the waste water, precipitation is returned metallurgical operation and is reclaimed, utilizes as raw material after concentrated, dehydration, mummification; Wherein, described first nertralizer is a liquid-state soluble alkali, and the pH value scope of described leading portion sedimentation basin is 9.0～10.0;
(2) through the leading portion post precipitation, supernatant enters the back segment sedimentation basin, adds second nertralizer and coagulant then, the supernatant standard discharge, and obtaining back segment mud based on the calcium salt composition, this back segment mud is through concentrating, obtaining mud butt material after the dehydration, mummification, pulverizing; Wherein, described second nertralizer is Ca (OH)
2, described coagulant is an aluminium salt, the pH value scope of described back segment sedimentation basin is 8～9.5;
(3) by the mud butt material of 20～60wt%, all the other mix for the charge ratio of auxiliary material, after agglomeration or making ball, carry out melt process in high temperature furnace, again through broken, levigate and powder process and the slag fritting base-material that is protected;
(4) in described covering slag fritting base-material, add the carbonaceous material of 2～15wt% and the binding agent of 0～5wt%, handle through granulation, drying, screening again, the slag finished product promptly is protected.
2. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: described liquid-state soluble alkali is at least a in NaOH, KOH or the ammoniacal liquor.
3. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: Ca (OH) in the described step (2)
2Injected volume be more than 1.2 times of theoretical amount.
4. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1; it is characterized in that: described aluminium salt is at least a in aluminum sulfate, aluminum potassium sulfate, sodium aluminate, aluminium polychloride or the polyaluminium sulfate, and the dosage of this coagulant is for handling the water yield 0.1～1.0wt%.
5. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: described auxiliary material is at least a in wollastonite, clinker, quartz sand, power plant's flue dust, blast furnace granulated slag, electroslag, borax, fluorite, sodium carbonate or the lithium carbonate.
6. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: the chemical composition of described mud butt material is by weight percentage:
CaO：40～50％；
Al
2O
3：15～25％；
SiO
2：4～10％；
CaF
2：15～30％；
T.Fe：0～2％；
H
2O：≤1％。
7. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: described high temperature furnace is shaft furnace or electric furnace.
8. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: the furnace temperature condition of described melt process is 1100～1400 ℃, is cooled to normal temperature after coming out of the stove.
9. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: described carbonaceous material is at least a in coke blacking, graphite, carbon black or the acidifying graphite.
10. the method for utilizing stainless steel cold-rolling pickling wastewater to prepare casting covering slag as claimed in claim 1 is characterized in that: described binding agent is at least a among starch, pitch or the CMC-Na.
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