CN101746836A - Method for preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater - Google Patents
Method for preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater Download PDFInfo
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- CN101746836A CN101746836A CN200910155779A CN200910155779A CN101746836A CN 101746836 A CN101746836 A CN 101746836A CN 200910155779 A CN200910155779 A CN 200910155779A CN 200910155779 A CN200910155779 A CN 200910155779A CN 101746836 A CN101746836 A CN 101746836A
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- iron oxide
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- coloured light
- oxide pigment
- black iron
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000002351 wastewater Substances 0.000 title claims abstract description 45
- 239000000049 pigment Substances 0.000 title claims abstract description 19
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052683 pyrite Inorganic materials 0.000 title claims abstract description 16
- 239000011028 pyrite Substances 0.000 title claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 87
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- 229910052742 iron Inorganic materials 0.000 claims abstract description 34
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 238000005070 sampling Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 10
- 239000012670 alkaline solution Substances 0.000 claims abstract description 6
- 239000001034 iron oxide pigment Substances 0.000 claims description 39
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000007689 inspection Methods 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 230000005587 bubbling Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 7
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 7
- 230000007246 mechanism Effects 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 5
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000605222 Acidithiobacillus ferrooxidans Species 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000005065 mining Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- -1 Fe 2+ Chemical class 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000004099 anaerobic respiration Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001651 autotrophic effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003818 cinder Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052952 pyrrhotite Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000019600 saltiness Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000010129 solution processing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Compounds Of Iron (AREA)
Abstract
The invention discloses a method for preparing an iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater. The method comprises the following steps: (1) adding alkaline solution into pyrite wastewater, adjusting a pH value to between 8 and 10, standing the mixture to obtain sediments and a supernatant liquid, and removing the supernatant liquid; and (2) putting the sediments obtained in the step (1) into a reactor, pumping in the air, making the sediments and the air react with each other by heating and stirring, controlling a temperature of between 80 and 100 DEG C, a stirring rate of between 100 and 200r/min, an air adding amount of between 0.01 and 0.05m3/h, tracking the reaction product in the reaction liquid and sampling to test chromatic light, when the chromatic light of the reaction product is consilient with that of a sample of iron oxide black pigment by comparing the reaction product with the sample of iron oxide black pigment, stopping the reaction, and processing the reaction liquid to obtain the iron oxide black pigment. The invention not only processes the acid pyrite wastewater to make the acid pyrite wastewater discharged after reaching standards, but also utilizes useful components in the pyrite wastewater to prepare the iron oxide black pigment, realizes the resourceful treatment of the waste, can be widely applied to the treatment of mineral wastewater with higher iron content, and has obvious social and environmental benefits.
Description
(1) technical field
The present invention relates to a kind of method of preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater.
(2) background technology
A kind of in the world abundant Mineral resources of sulfurous iron ore, mainly be by the sulphur in the earth mantle and the iron in the earth's crust and other impurity element such as Al, Mn, Cu etc. under suitable geochemical conditions, one-tenth ore deposit through thousands of years develops (hydrothermal solution, deposition, biology, rotten, compound isotype) and forms, so the main component of sulfurous iron ore is FeS
2(pyrite, white pyrite), FeS (pyrrhotite) also contain metallic elements such as Al, Zn, Cu, Pb simultaneously.In mining process or the pit discarded after owing to have oxygen and microorganism in the pit, surface precipitation and underground water can produce a large amount of Fe that contains in the pit under its effect
2+And SO
4 2-Acid waste water.
Sum up through scholars' in decades discussion and to confirm that the mechanism that sulfurous iron ore waste water forms is the oxidation of sulfurous iron ore, hydrogeological conditions, weather, temperature and the microbiological condition of sulfide self component, mining type and the locality in main and mine are relevant.
The primary process of its oxidation is as follows with reaction:
4Fe
2++O
2+4H
+＝4Fe
3++2H
2O (2)
By the primary process of reaction formula (1)～(3) oxidation, the Fe of generation
2+Can be at O
2Generate Fe down with the catalysis of ferrobacillus ferrooxidans (T.ferroxidans)
3+Reaction cycle is gone on, and the acidity of water increases.Ferrobacillus ferrooxidans is a kind of aerobic autotrophic bacteria that is grown in the sour water, and being grown in pH is in 1.13～4.15, and best PH is 2.15～3.18,10 ℃～37 ℃ of growth temperatures, 30 ℃～35 ℃ of optimum tempss.This bacterium is that nature exists in the waste water of pit, generally need not inoculate, and when pH value was higher, ferrobacillus ferrooxidans had just lost effect, and Fe
3+Generate the insoluble complex compound of precipitation and iron.
The mechanism that produces from above-mentioned sulfurous iron ore waste water as can be seen, the main characteristic of sulfurous iron ore waste water is a strongly-acid, the iron-holder height, generally between the hundreds of milligram is to several thousand milligrams, expose air after colourity big.Its pH value is between 1～4; Contain a large amount of Fe
2+, SO
4 2-Especially up to thousands of milligrams; Also contain a small amount of other metal ion such as Al
3+, Zn
2+, Cu
2+Deng; Fe behind the waste water exposure air
2+Be oxidized to Fe
3+, waste water can present rust.If, the pH value of water body is changed if sulfurous iron ore waste water does not add processing and directly enters water body, suppress bacterium and microbial growth, hinder the self-cleaning of water body, cause the mining area severe contamination of water body on every side; And some salt of the interaction of the mineral substance in acid waste water and water body meeting generation, the growth generation detrimentally affect to limnobios and plant causes hydrobiont death such as fish, algae, planktonic organism; Even more serious is that sulfurous iron ore waste water prolonged permeation further makes underground water source be polluted.Therefore, sulfurous iron ore waste water all is serious source of pollution to surface water and underground water undoubtedly, can cause serious destruction to ecotope.
Sulfurous iron ore waste water is the high acid waste water of typical inorganic heavy metal saltiness.Check in from existing literature, according to the characteristics of waste water self, treatment process is divided into two big classes substantially.
First kind is the active process method.The active process method is called direct facture again, promptly adopts to add the alkali neutralization, the pH value is improved, and heavy metal ion is precipitated.This method is in sulfurous iron ore waste water or is subjected to the water body of sulfurous iron ore contaminated wastewater directly to add alkaline matter to neutralize, as ammonia, Wingdale, lime etc., be a kind of application the earliest, than successful method.The reaction mechanism of this method is fairly simple, mainly is to utilize acid-base neutralisation to improve the pH value, makes Fe
2+, Fe
3+Precipitation is removed Al by precipitation absorption simultaneously
3+, Zn
2+, Cu
2+Etc. heavy metal ion.But there is the influence that is subject to external flow and acidity increase in this method, the not enough situation of basicity occurs, influences effluent quality; The metal bigger to solubleness is difficult to precipitation; Expense is higher; Produce a large amount of iron containing sludges, need regular maintenance to remove, and iron containing sludge is difficult for dehydration, generation secondary pollution or the like drawback.
Second method is passive facture.Its cardinal principle is to utilize the biological-chemical method, sets up wet land system.Mainly be to seek the biology that can reduce metal content in the Passive evolution.At present, using many is reversion bacterium (SRB-Sulfate Reducing Bacteria), and SRB is distributed widely in water body and the soil.Under the condition that carbon and sulfate source are arranged, carry out in the process of anaerobic respiration, utilize vitriol to carry out the alienation reduction of vitriol as final electron acceptor(EA), produce H
2S and HCO
3 -, precipitation, Adsorption of Heavy Metal Ions such as Fe
2+, Fe
3+, Al
3+, Zn
2+Deng, the sewage that so both neutralized has also been removed heavy metal ion.
Reaction mechanism:
Fe
2++HS
-＝FeS+H
+
Passive it has operation, safeguards fairly simple advantage with the comparison of active process method, and technology is comparatively ripe.But initial investment is many, and the processing cycle is longer, and is not suitable for the [underground effluent of big flow.
At present, the cheap by-product scrap iron skin and the vitriol oil are the main raw materials of producing iron pigment.Along with increasing substantially of iron pigment output, the iron sheet resource lacks gradually, therefore skyrocketing of price utilized the useless secondary resource of industry widely, as the ferrous sulfate of pyrite cinder, titanium white by product object height concentration, steel mill's dedusting ash etc. all in the technology of progressively seeking to prepare iron pigment.
(3) summary of the invention
The method that the purpose of this invention is to provide a kind of preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater.
The inventive method is not only made every effort to the processing up to standard of sulfurous iron ore waste water from Green Chemistry changing waste into resources theory; Be raw material with sulfurous iron ore waste water especially, utilize sulfurous iron ore waste water to prepare iron pigment, thereby really reach environment and economic harmonious development.
Because sulfurous iron ore waste water is a kind of strongly acid wastewater, wherein contains a large amount of Fe
2+, SO
4 2-Ion, the raw materials for production of analogy conventional iron series pigments can utilize sulfurous iron ore waste water to prepare black iron oxide pigment.
The technical solution used in the present invention is:
A kind of method of preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater said method comprising the steps of: it is 8～10 that (1) sulfurous iron ore waste water adds alkaline solution adjusting pH value, leaves standstill and obtains throw out ferrous hydroxide and supernatant liquor, abandoning supernatant; (2) the throw out ferrous hydroxide that obtains of step (1) adds reactor, bubbling air, and the heated and stirred reaction, controlled temperature is 80～100 ℃, and stirring velocity is 100～200r/min, and air feeding amount is 0.01～0.05m
3/ h reacted 3～5 hours, followed the tracks of reaction product sampling inspection coloured light in the reaction solution, compared to coloured light when consistent when reaction product and black iron oxide pigment sample, and stopped reaction obtains black iron oxide pigment after the reaction solution processing.
The inventive method step (1) is the preparation of ferrous hydroxide.Its chemical reaction mechanism as shown in the formula:
FeSO
4+2NaOH→Fe(OH)
2+Na
2SO
4
Or FeSO
4+ 2NH
3H
2O → Fe (OH)
2+ (NH
4)
2SO
4
The inventive method step (2) is the preparation of black iron oxide pigment.Its chemical reaction mechanism is as follows:
Fe(OH)
2+2Fe(OH)
3→Fe(OH)
2·2Fe(OH)
3→Fe
2O
3·FeO+4H
2O
In the slow oxidation process, dehydration reaction is carried out fast, the Fe of generation
2O
3FeO constantly gathers, and enlarges gradually, finally forms iron oxide black pigment.When reacting near end, the blackening of reaction solution color, reacting liquid pH value is 7～8.
Alkaline solution in the step of the present invention (1) is the NaOH aqueous solution or ammoniacal liquor, the preferred NaOH aqueous solution.The concentration of the described NaOH aqueous solution is generally 10wt%～30wt%, and the concentration of ammonia soln is generally 5mol/L～15mol/L.
In the step of the present invention (2), described sampling inspection coloured light method is: extract a small amount of reaction solution, and suction filtration, behind the washing filter cake, oven dry, check coloured light is with the coloured light contrast of black iron oxide pigment sample.
In the described step (2), the reaction solution treatment process is: the reaction solution cooling, suction filtration washes filter cake with water, is crushed to 350～400 orders after the oven dry, gets described black iron oxide pigment.The temperature of described oven dry is preferably 55～65 ℃.
Comparatively concrete, recommend the method for preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater of the present invention to carry out according to following steps: (1) sulfurous iron ore waste water adds the NaOH aqueous solution, regulating the pH value is 8～10, leaves standstill and obtains throw out ferrous hydroxide and supernatant liquor, abandoning supernatant; (2) the throw out ferrous hydroxide that obtains of step (1) adds reactor, bubbling air, and the heated and stirred reaction, controlled temperature is 80～100 ℃, and stirring velocity is 100～200r/min, and air feeding amount is 0.01～0.05m
3/ h follows the tracks of reaction product sampling inspection coloured light in the reaction solution, compares to coloured light when consistent with the black iron oxide pigment sample, stopped reaction, reaction solution cooling, suction filtration, wash filter cake with water, be crushed to 350～400 orders after the oven dry under 55～65 ℃ of temperature, obtain described black iron oxide pigment; Described sampling inspection coloured light method is: extract a small amount of reaction solution, and suction filtration, behind the washing filter cake, oven dry, check coloured light compares with the coloured light of black iron oxide pigment sample.
Beneficial effect of the present invention is: this method has not only been handled sour sulfur iron ore waste water, makes its qualified discharge; Simultaneously also utilize the useful component in the sulfurous iron ore waste water to prepare black iron oxide pigment, realized the recycling treatment of refuse.
The inventive method can be widely used in the processing of the higher pit waste water of iron-holder, has tangible society and environmental benefit.
(4) description of drawings
The process flow sheet of Fig. 1 preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater.
(5) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Embodiment 1:
The sulfurous iron ore waste water of A, 500ml (ore deposit waste water is closed in the ox horn gulf under the hugeization chemical industry company limited of Zhejiang) adds the NaOH aqueous solution (10wt%), and regulating the pH value is 8.Leave standstill and obtain throw out ferrous hydroxide and supernatant liquor, discard supernatant liquor up to standard.
B, the throw out ferrous hydroxide is poured in the reactor, heat temperature raising to 80 ℃ stirs and reacts gradually, feeds a spot of air simultaneously, carries out slow oxidation, and this process air capacity is controlled at 0.01m
3/ h, stirring velocity is 100r/min, and the reaction solution color is by the original blackish green blackish green that is transformed into, and centre sampling inspection coloured light is carried out in last blackening incessantly.Sampling inspection coloured light method is: extract a small amount of reaction solution, and suction filtration, behind the washing filter cake, oven dry, check coloured light is with the coloured light contrast of black iron oxide pigment sample.When filter cake and black iron oxide pigment sample are compared to coloured light when consistent stopped reaction.
C, reaction solution cooling with circulating vacuum pump suction filtration, wash filter cake with water, use oven for drying, and temperature is controlled at 55 ℃.
D, dried filter cake is crushed to 350～400 orders, makes black iron oxide pigment 1.8896g with pulverizer.
Embodiment 2:
Reaction conditions is with embodiment 1, and different is, adds the NaOH aqueous solution (30wt%) in the steps A, and regulating pH value is 10, other operate and condition with embodiment 1, make black iron oxide pigment 2.0304g.
Embodiment 3:
Reaction conditions is with embodiment 1, and different is, heat temperature raising to 100 ℃ among the step B, and other operations and condition make black iron oxide pigment 2.0965g with embodiment 1.
Embodiment 4:
Reaction conditions is with embodiment 1, and different is that air capacity is controlled at 0.05m among the step B
3/ h, other operations and condition make black iron oxide pigment 2.1203g with embodiment 1.
Embodiment 5:
Reaction conditions is with embodiment 1, and different is, stirring velocity is 200r/min among the step B, and other operations and condition make black iron oxide pigment 2.0803g with embodiment 1.
Embodiment 6:
Reaction conditions is with embodiment 1, and different is, bake out temperature is controlled at 65 ℃ among the step C, and other operations and condition make black iron oxide pigment 2.0639g with embodiment 1.
Embodiment 7:
Reaction conditions is with embodiment 2, and different is, heat temperature raising to 100 ℃ among the step B, and other operations and condition make black iron oxide pigment 2.1354g with embodiment 2.
Embodiment 8:
Reaction conditions is with embodiment 2, and different is that air capacity is controlled at 0.05m among the step B
3/ h, other operations and condition make black iron oxide pigment 2.0924g with embodiment 2.
Embodiment 9:
Reaction conditions is with embodiment 2, and different is, stirring velocity is 200r/min among the step B, and other operations and condition make black iron oxide pigment 2.0013g with embodiment 2.
Embodiment 10:
Reaction conditions is with embodiment 2, and different is, bake out temperature is controlled at 65 ℃ among the step C, and other operations and condition make black iron oxide pigment 1.9997g with embodiment 2.
Embodiment 11:
Reaction conditions is with embodiment 3, and different is that air capacity is controlled at 0.05m among the step B
3/ h, other operations and condition make black iron oxide pigment 2.031g with embodiment 3.
Embodiment 12:
Reaction conditions is with embodiment 3, and different is, stirring velocity is 200r/min among the step B, and other operations and condition make black iron oxide pigment 1.9867g with embodiment 3.
Embodiment 13:
Reaction conditions is with embodiment 3, and different is, bake out temperature is controlled at 65 ℃ among the step C, and other operations and condition make black iron oxide pigment 1.9334g with embodiment 3.
Embodiment 14:
Reaction conditions is with embodiment 4, and different is, bake out temperature is controlled at 65 ℃ among the step C, and other operations and condition make black iron oxide pigment 1.9025g with embodiment 4.
Embodiment 15:
Reaction conditions is with embodiment 1, and different is, adds ammonia soln in the steps A, and other operations and condition make black iron oxide pigment 1.8756g with embodiment 1.
Embodiment 16:
Reaction conditions is with embodiment 2, and different is, adds ammonia soln (5mol/L) in the steps A, and other operations and condition make black iron oxide pigment 2.0146g with embodiment 2.
Embodiment 17:
Reaction conditions is with embodiment 3, and different is, adds ammonia soln (15mol/L) in the steps A, and other operations and condition make black iron oxide pigment 2.0844g with embodiment 3.
Embodiment 18:
Reaction conditions is with embodiment 4, and different is, adds ammonia soln (5mol/L) in the steps A, and other operations and condition make black iron oxide pigment 2.1167g with embodiment 4.
(HG-T2250-1991) check and prepare product according to " People's Republic of China's chemical industry standard---black iron oxide pigment ", every index all can reach the requirement of salable product in the black iron oxide pigment industry standard.
Concrete assay such as the following table of embodiment 1-4, all the other results are basic identical, do not explain.
Claims (7)
1. the method for a preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater is characterized in that said method comprising the steps of: (1) sulfurous iron ore waste water adds alkaline solution, and regulating the pH value is 8～10, leaves standstill and obtains throw out and supernatant liquor, abandoning supernatant; (2) throw out that obtains of step (1) adds reactor, bubbling air, and the heated and stirred reaction, controlled temperature is 80～100 ℃, and stirring velocity is 100～200r/min, and air feeding amount is 0.01～0.05m
3/ h follows the tracks of the reaction product sampling inspection coloured light in the reaction solution, when reaction product and black iron oxide pigment sample are compared to coloured light when consistent stopped reaction, the treated black iron oxide pigment that obtains of reaction solution.
2. the method for claim 1 is characterized in that the alkaline solution in the described step (1) is the NaOH aqueous solution or ammonia soln.
3. the method for claim 1 is characterized in that in the described step (2), and described sampling inspection coloured light method is: extract a small amount of reaction solution, and suction filtration, behind the washing filter cake, oven dry, check coloured light compares with the coloured light of black iron oxide pigment sample.
4. the method for claim 1 is characterized in that the reaction solution treatment process is in the described step (2): the reaction solution cooling, suction filtration washes filter cake with water, is crushed to 350～400 orders after the oven dry, obtains described black iron oxide pigment.
5. method as claimed in claim 4, the temperature that it is characterized in that described oven dry is 55～65 ℃.
6. method as claimed in claim 2 is characterized in that the alkaline solution in the described step (1) is the NaOH aqueous solution.
7. as the described method of one of claim 1～6, it is characterized in that described method may further comprise the steps: (1) sulfurous iron ore waste water adds the NaOH aqueous solution or ammonia soln, and regulating the pH value is 8～10, leaves standstill and obtains throw out and supernatant liquor, abandoning supernatant; (2) throw out that obtains of step (1) adds reactor, bubbling air, and the heated and stirred reaction, controlled temperature is 80～100 ℃, and stirring velocity is 100～200r/min, and air feeding amount is 0.01～0.05m
3/ h, follow the tracks of the reaction product sampling inspection coloured light in the reaction solution, when reaction product and black iron oxide pigment sample are compared to coloured light when consistent, stopped reaction, the reaction solution cooling, suction filtration washes filter cake with water, be crushed to 350～400 orders after the oven dry under 55～65 ℃ of temperature, obtain described black iron oxide pigment; Described sampling inspection coloured light method is: extract a small amount of reaction solution, and suction filtration, behind the washing filter cake, oven dry, check coloured light compares with the coloured light of black iron oxide pigment sample.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102616997A (en) * | 2012-04-06 | 2012-08-01 | 中国中化股份有限公司 | Method for treating wastewater generated in production process of iron oxide pigment |
| CN103011304A (en) * | 2012-11-27 | 2013-04-03 | 常州大学 | Novel treatment method for pyrite wastewater |
| CN103585738A (en) * | 2013-11-06 | 2014-02-19 | 和丽萍 | Method for neutralizing sulphur smelting waste by quick lime |
| CN103754958A (en) * | 2014-01-15 | 2014-04-30 | 安徽八一化工股份有限公司 | Process for preparing black iron oxide by utilizing wastewater generated in production of chlorinated benzene |
| CN103964599A (en) * | 2013-01-29 | 2014-08-06 | 绍兴深水环保设备有限公司 | Recycling method for iron oxide dye wastewater treatment sludge |
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| CN1322067C (en) * | 2005-06-08 | 2007-06-20 | 刘世琦 | Method for producing iron oxide black |
| CN101559986A (en) * | 2009-05-14 | 2009-10-21 | 上海一品颜料有限公司 | Method for producing iron oxide black |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102616997A (en) * | 2012-04-06 | 2012-08-01 | 中国中化股份有限公司 | Method for treating wastewater generated in production process of iron oxide pigment |
| CN102616997B (en) * | 2012-04-06 | 2013-10-09 | 中国中化股份有限公司 | Method for treating wastewater generated in production process of iron oxide pigment |
| CN103011304A (en) * | 2012-11-27 | 2013-04-03 | 常州大学 | Novel treatment method for pyrite wastewater |
| CN103964599A (en) * | 2013-01-29 | 2014-08-06 | 绍兴深水环保设备有限公司 | Recycling method for iron oxide dye wastewater treatment sludge |
| CN103585738A (en) * | 2013-11-06 | 2014-02-19 | 和丽萍 | Method for neutralizing sulphur smelting waste by quick lime |
| CN103754958A (en) * | 2014-01-15 | 2014-04-30 | 安徽八一化工股份有限公司 | Process for preparing black iron oxide by utilizing wastewater generated in production of chlorinated benzene |
| CN109665566A (en) * | 2019-01-23 | 2019-04-23 | 深圳市长隆科技有限公司 | A kind of preparation method and sewage water treatment method of magnetic nano ferroferric oxide |
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