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WO1994018126A1 - Procede pour eliminer les ions de metaux lourds de l'eau - Google Patents

Procede pour eliminer les ions de metaux lourds de l'eau Download PDF

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Publication number
WO1994018126A1
WO1994018126A1 PCT/CA1994/000012 CA9400012W WO9418126A1 WO 1994018126 A1 WO1994018126 A1 WO 1994018126A1 CA 9400012 W CA9400012 W CA 9400012W WO 9418126 A1 WO9418126 A1 WO 9418126A1
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Prior art keywords
water
iron
stage
heavy metal
metal ions
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Ceased
Application number
PCT/CA1994/000012
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English (en)
Inventor
Nikolay Valerjevich Pertsov
Zoya Rudolfovna Ulberg
Vitality Anatolievich Prokopenko
Tamara Alexandrovna Polishchuk
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958075 Ontario Inc
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958075 Ontario Inc
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Publication date
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Priority to AU58307/94A priority Critical patent/AU5830794A/en
Publication of WO1994018126A1 publication Critical patent/WO1994018126A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/62—Heavy metal compounds

Definitions

  • the invention relates to a water treatment process, and more
  • Natural and industrial waters contain ions of different chemical elements, including metallic ions.
  • One or several chemical elements are usually predominant in such natural and industrial waters. Since the method or manner of separating each particular element from water is usually element- specific, it is difficult to develop a single process which enables the
  • Natural subsoil water or waters used in mining operations contain ions of different metals, with iron ions usually being predominant. It is known in the art that treatment of subsoil water containing up to 6mg/l of Fe 2+ ions may be accomplished by aeration, followed by filtering the oxygen-saturated water through a filter, such as a sand filter (L. Kulsky, P. Strokach "Processes for treating natural waters", 1981, p.217).
  • a filter such as a sand filter
  • this process is generally unsatisfactory, even for the single removal of iron ions, since the aeration alone does not provide the required degree of iron ion removal, especially when iron salts of strong mineral acids or iron salts of humic acids are present in the input water.
  • chlorine or potassium permanganate must be additionally introduced into the water prior to the filtration stage in order to adequately remove the iron ions. This procedure is undesirable from an environmental standpoint, since the resultant water is unsuitable for discharge into sewers or lakes.
  • calcium hydroxide may be introduced into the water in the known process for removing iron ions from subsoil water described in the above-mentioned manual of L. Kulsky. Calcium hydroxide added into the water first reacts with iron (II) sulphate as show below :
  • Iron (II) hydroxide Fe(OH) 2
  • Fe(OH) 3 Iron (II) hydroxide
  • calcium hydroxide is introduced in combination with chlorination or aeration technique.
  • potassium permanganate is further added to the water. This technique results in considerable pH increase (up to 9.5 - 10.5) and in precipitation of certain amount of other metal hydroxides which were formed in the water.
  • hydrochloric acid is added, which enables said water to be applied for production needs as well as to be discharged into natural water streams.
  • liquid effluents from galvanic treatment operations contain mixtures of various chemical elements, including heavy metal ions.
  • Heavy metal ions are removed from such liquid effluents by using the above chemical reagent techniques as is done with natural waters.
  • the above technique is performed on liquid effluent by introducing into the heavy metal ion-containing effluents an alkaline reagent, such as sodium hydroxide, sodium carbonate, or calcium hydroxide (Zapolsky A., Obraztsov V. "Complex treatment of the galvanic industry effluents" Kiev, 1989 p. 29-43).
  • alkaline reagents such as sodium hydroxide, sodium carbonate, or calcium hydroxide
  • an alkali metal hydroxide may be added to acidic water (of pH below 4.0) to raise the ph between 4.8 to 5.4 to thereby precipitate out an iron hydroxide-containing precipitate at this pH.
  • a second step is performed, whereby additional metal hydroxide is added to raise the pH even higher, to around 8.8 to 9.4, where other metal hydroxides, such as Zn(OH) 2 have very poor solubility, thereby causing them to precipitate out of the solution.
  • additional metal hydroxide is added to raise the pH even higher, to around 8.8 to 9.4, where other metal hydroxides, such as Zn(OH) 2 have very poor solubility, thereby causing them to precipitate out of the solution.
  • the resulting solution even though stripped of Fe +2 and Zn +2 heavy metal ions, is of high pH and thus unsuitable for discharge into lakes or rivers, without further treatment.
  • the applicants have found that by subsequently bringing the resultant mixture into contact with galvanic pair-forming substances, such as iron and coke, iron and copper, or aluminum and copper, the concentration of heavy metal ions in the mixture was actually further reduced. This has been found to occur when the alkaline reagent is first added in a certain quantity in accordance with a specific formula to thereby bring the pH up to a range between 4.0 to 6.0, and the resulting mixture including all precipitates is subsequently brought into contact with those galvanic pair-forming compounds.
  • galvanic pair-forming substances such as iron and coke, iron and copper, or aluminum and copper
  • the concentration of heavy metal ions were further reduced as a result of contact with the galvanic pair-forming compounds, but the resulting mixture had a pH in the desired neutral range (7.0), and did not require the addition of further acids or bases to adjust the pH to the neutral range.
  • the galvanic pair-forming compounds operate to cause further precipitation out of heavy metal ions. While the mechanism by which the galvanic pair-forming compounds operate to cause further precipitation out of heavy metal ions is not clear, it is thought that the effect is likely achieved due to the formation of highly- dispersed particle sediment within the mixture at the first water treatment stage (when the alkaline reagent is introduced), which then each individually function as crystallization centres at the second stage treatment where the mixture is then mixed with the galvanic pair-forming compounds under galvanocoagulation conditions.
  • the presence of crystallization centers accelerates the iron, copper, or aluminum dissolving process due to the intensification of iron, copper, or aluminum ion diffusion, and further facilitates precipitation of these ions on crystallization centres.
  • the formed sediment has a highly developed surface which enables the ions of other chemical elements present in the water to be absorbed thereon, and thus removed from solution.
  • a two stage process for removing heavy metal ions from water, comprising adding a specific amount of alkaline reagent to the input water in an amount required to raise the water pH to between 4.0 to 6.0 and being determined according to the formula (0.03 to 4.2)grams/liter + (2.0 to 2.8) x [Fe 3+ ] grams/liter, wherein
  • Fe 3+ is the concentration of Fe 3+ ions initially resident in the input water to thereby form a mixture; supplying said mixture together with formed sediment therein into a vessel filled with galvanic pair-forming substances, said galvanic pair-forming substances being one or more combinations of substances selected from the group of pair-forming substances comprising iron and coke, iron and copper, aluminum and coke, or aluminum and copper; and ensuring said mixture together with formed sediment therein is in close and intimate contact with said galvanic pair-forming substances for between at least 5 to 60 minutes.
  • the two-stage process according to present invention provides the effective removal of a number of water-contaminating heavy metal ions such as copper, zinc, lead, nickel, cadmium, aluminum, mercury, manganese, etc., and is not just specific to one or two heavy metals, such as iron and zinc.
  • Said process also makes possible to remove the ions of non- metals, such as arsenate ions (AsO 4 -3 ) as well as sulfate (SO 4 -2 ) anions.
  • the galvanic pair-forming substances be mixtures of iron and coke, or iron and copper, and in a ratio therebetween equal to (3 to 4):1.
  • the galvanic pair-forming substances being used be mixtures of aluminum and coke, or aluminum and copper, and that the ratio of aluminum to coke or copper be (1 to 4):(4 to 1).
  • the alkaline reagent to be used for the above process may be of any type typically used in the art. Reagents particularly suited to this application are sodium hydroxide (Na(OH) 2 ), calcium hydroxide (Ca(OH) 2 ), lime or slaked lime (CaO), sodium bicarbonate (Na(CO 3 ) 2 ), and calcium bicarbonate (Ca(CO 3 ) 2 ), because of their low cost.
  • the natural and industrial waters of various production processes typically contain ions of following concentrations (milligrams/liter) : Fe 3+ (35.0 - 410), Fe 2+ (1.1-975.0), Zn 2+ (4.5 - 200.0), Cu 2+ (22-60), Pl 2+ (0.12-18.0), Ni 2+ (0.005-16.0), Cd 2+ (0.04-0.60), Mn 2+ (3.5-11.0), Hg(total) (0-0.002), As(total) (0.006-2.0), Cr(total) (1.9-42.2), Al 3+ (0-16.0), V(total) (0.3-4.5), and
  • the invention is directed to treating water of the above type, and is particularly directed to treating input waters of the above type having a pH in the range of 2.0 to 3.3.
  • the process for treating said waters is performed in two stages.
  • the input water is collected in some kind of accumulator, such as a concrete container with its capacity being dependent on the flow volume of the water to be treated.
  • some kind of accumulator such as a concrete container with its capacity being dependent on the flow volume of the water to be treated.
  • the daily volume of treated water to be collected in the accumulator amounts to 1200 liters.
  • the water is further supplied to a vessel having the capacity of about 50 liters and being equipped with stirring means and pH meter, wherein the alkaline reagent, such as calcium hydroxide, is introduced and mixing is performed for 10-15 minutes.
  • the alkaline reagent such as calcium hydroxide
  • the amount of alkaline reagent determined according to the above formula is sufficient to raise the pH of water to be treated from 4.0 to 6.0 and to precipitate as substantial quantity of the Fe 3+ ions.
  • the sediment formed at the first treatment stage consists of metal hydroxides, as well as calcium sulphate where calcium hydroxide or lime is used as the alkaline reagent.
  • the sediment may also contain certain amount of As- ions.
  • An alkaline reagent such as sodium hydroxide or sodium carbonate could also be used, in which case the sediment formed at the first treatment stage consists of metal hydroxides, and sodium sulphate.
  • the so treated water together with formed sediment is further supplied under gravity or by means of a pump to the second stage treatment into a rotating cylindrical vessel made of stainless steel with its capacity being 1.0 cubic metre and the rotation rate constituting 2-3 rpm.
  • the capacity of said vessel may be variable depending on the volume of water to be treated.
  • Said vessel is charged with a mixture of iron scrap and coke, with the ratio therebetween respectively being (3 to 4):1.
  • the amount of water in said vessel usually constitutes 1 ⁇ 4 - 1 ⁇ 2 part of its volume.
  • the treatment of water in said vessel is accomplished for 5.0 - 60.0 minutes.
  • the cylindrical vessel can also be filled with iron and copper mixture at a ratio therebetween (3 to 4):1 as well as with a mixture of aluminum and copper being taken at a ratio of aluminum to coke or copper equal to (1 to 4):(4 to 1). Due to the above treatment the pH of water is further increased, and reaches the neutral values of 6.5-7.0. While treating water in this vessel an additional amount of sediment (precipitate) is formed, promoting the effective removal from water of above said ions.
  • the water together with formed sediment is discharged into the precipitator in order to separate the dispersed particles therefrom.
  • the purified water flows under gravity from the upper part of precipitator.
  • Commercially available filters can also be used for separating the dispersed particles.
  • the water treated according to present invention may be used to satisfy production needs of a chemical plant, or alternatively be discharged into the water streams.
  • the formed sediment is easy to dry and dispose of.
  • Calcium hydroxide in an amount of 1.0 g/l was added to the input water at the first treatment stage which enabled the pH value to be increased to 4.0.
  • the water containing the first stage formed sediment was then, during the second stage, charged into a vessel rotating at a rate of 2 rpm and filled with iron and coke mixture at a ratio therebetween of 3:1 respectively, wherein said water was treated for 60 minutes. Due to above treatment water pH value increased to 6.6.
  • the amount of iron hydroxide [Fe(OH) 3 ] sediment formed at the second stage totalled 6.0 g/l.
  • compositions of input water, first and second stage treatment waters are given in Table 1.
  • Input water containing certain heavy metal ions (see Table 1) of pH 2.5 was used.
  • Calcium hydroxide in an amount of 1.29 g/l was added to the water at the first treatment stage which enabled the pH value to be raised to 5.0.
  • the water containing the first stage formed sediment at the second stage was fed into a vessel having the rotation rate of 2 rpm and being charged with iron and coke mixture at a ratio thereof equal to 3:1 respectively, herein said water was treated for 60 minutes. Due to above treatment the pH of water was increased to 6.8.
  • the amount of iron hydroxide sediment formed after the second stage treatment was 6.2 g/l.
  • Input water containing certain heavy metal ions (see Table 1) of pH 2.5 was used.
  • Calcium hydroxide in an amount of 1.7 g/l was added to the water at the first treatment stage which enabled the pH value to be increased to 6.0.
  • the water containing the first stage sediment at the second stage was charged into a vessel rotating at a rate of 2 rpm and being filled with iron and coke mixture at a ratio therebetween being 4:1 respectively, wherein said water was treated for 60 minutes.
  • the above treatment resulted in the pH value increase to 7.0.
  • the amount of iron hydroxide sediment formed after the second stage treatment totalled 6.5 g/l.
  • Input water containing certain heavy metal ions (see Table 1) with pH 2.0 was used.
  • Calcium hydroxide in an amount of 0.687 g/l was added to the water at the first treatment stage which enabled the pH value to be raised to 4.0
  • the water containing the first stage sediment at the second stage was supplied into a vessel having the rotation rate of 2 rpm and being charged with an iron and coke mixture at a ratio thereof being 3:1 respectively, wherein said water was treated for 60 minutes. Due to the above treatment the pH value increased to 6.5. The amount of iron hydroxide sediment formed after the second stage treatment constituted 6.0 g/l.
  • composition of the resulting first and second stage treated waters is further given in Table 1.
  • Input water containing certain heavy metal ions (see Table 1) of pH 3.0 was used.
  • Calcium hydroxide in an amount of 0.3 g/l was introduced into the water at the first treatment stage with the pH value to be increased to 4.0.
  • the water containing the first stage formed sediment at the second stage was fed into a vessel having the rotation rate of 2 rpm and being filled with iron and coke mixture at a ratio thereof being 3:1 respectively, wherein said water was treated for 30 minutes.
  • the above treatment resulted in pH increase up to 6.0.
  • the amount of iron hydroxide sediment after the second stage treatment totalled 5.2 g/l.
  • Input water containing various heavy metal ions (see Table 1) of pH 3.0 was used.
  • Calcium hydroxide in an amount of 0.22 g/l was added to the water at the first treatment stage which enabled the pH value to be raised to 4.0.
  • the water containing the first stage formed sediment at the second stage was charged into a vessel rotating at a rate of 2 rpm and being filled with iron and copper mixture at a ratio thereof equal to 4:1 respectively, wherein said water was treated for 15 minutes. Due to above treatment the pH value increased to 6.5.
  • the amount of iron hydroxide sediment formed after the second stage treatment was 5.1 g/l.
  • Input water containing certain heaving metal ions (see Table 1) of pH 3.3 was used.
  • Calcium hydroxide in an amount of 0.1 g/l was added to the water at the first treatment stage which enabled the pH value to be raised to
  • the water containing the first stage formed sediment at the second stage was fed into a vessel rotating at a rate of 2 rpm and being filled with iron and copper mixture at a ratio therebetween of 3:1 respectively, wherein said water was treated for 5 minutes.
  • the above treatment resulted in pH increase up to 6.5.
  • the amount of iron hydroxide sediment formed after the second stage treatment totalled 5.0.
  • composition of the input water, first and second stage treated waters is represented in Table 1.
  • Calcium hydroxide in an amount of 0.2 g/l was added to the water at the first treatment stage with pH being increased upto 6.0.
  • the amount of iron hydroxide sediment (Fe(OH) 3 ) formed at the second stage was 3.2 g/l.
  • Input water containing various heaving metal ions with pH 2.6 was used.
  • Calcium hydroxide in an amount of 0.86 g/l was introduced into the water at the first treatment stage which resulted in the pH raised to 4.0.
  • Iron hydroxide (Fe(OH) 3 ) formed at the second treatment stage amount to 4.0 g/l.
  • Input water containing heavy metal ions with pH 3.2 was used.
  • the amount of iron hydroxide (Fe(OH) 3 ) formed at the second stage was 3.1 g/l.
  • Composition of the input water, first and second stage treated waters is given in Table 1.
  • Input water containing various heavy metal ions of pH 2.0 was used.
  • calcium hydroxide in an amount of 2.35 g/l was introduced into the water which resulted in pH increase to 6.0.
  • Input water containing various heavy metal ions at pH 2.5 was used.
  • Calcium hydroxide in an amount of 0.21 g/l was introduced into the water at the first treatment stage with the pH value being increased to 4.0.
  • Composition of the input water, first and second stage treated waters is given in Table 1.
  • Input water containing various heavy metal ions at pH 2.5 was used.
  • sodium hydroxide in an amount of 1.5 g/l was used resulting in pH increase to 4.0.
  • water with the first stage formed sediment was supplied into a vessel with a rotation rate of 2 rpm filled with a mixture of iron and coke at the proportion thereof being 3:1 respectively wherein said water was treated for 60 minutes. After the treatment water pH rose to 6.6.
  • Input water containing various heavy metal ions at pH 2.5 was used.
  • sodium carbonate in an amount of 2.9 g/l was introduced into the water with its pH being increased to 5.0.
  • water containing the first stage formed sediment was charged into a vessel having the rate of rotation of 2 rpm and being filled with a mixture of iron and coke at the proportion therebetween equal to 3:1 respectively, wherein said water was treated for 60 minutes which resulted in water pH 6.8.
  • Iron hydroxide sediment after the second stage amounted to 3.1 g/l.
  • the composition of waters is presented in Table 1.
  • water with the first stage formed sediment was directed to a vessel rotating at a rate of 2 rpm and being filled with a mixture of iron and coke at the ratio therebetween of 4:1 respectively, wherein said water was treated for 60 minutes. After such treatment was pH rose to 7.0. The amount of the second stage formed iron hydroxide was 3.8 g/l.
  • Composition of the input water, first and second stage treated water is given in Table 1.
  • Input water containing heavy metal ions with pH 2.5 was used.
  • Calcium hydroxide in an amount of 0.836 g/l was added to the water at the first treatment stage enabling its pH value to be increased to 3.5.
  • the water together with the sediment formed at the first treatment stage was supplied to a vessel rotating at 2 rpm and being filled with iron and coke mixture at a ratio therebetween equal to 4:1 wherein said water was treated for 60 minutes. After said treatment the water pH rose to 5.3.
  • the amount of iron hydroxide (Fe(OH) 3 ) sediment formed at the second stage treatment was 2.5 g/l.
  • Input water containing heavy metal ions with pH 2.0 was treated by adding calcium hydroxide as it is practiced in the known process according to Zapolsky A., "complex treatment of the galvanic industry effluents", Kiev, 1989, p. 29-43).
  • calcium hydroxide was added to the water in an amount of 2.5 g/l which enabled the majority of water contained metal ions to be removed from the water. Due to adding said quantity of calcium hydroxide the water pH value rose to 10.0. The amount of formed sediment was 4.5 g/l.
  • Input water containing heavy metal ions with pH value 2.0 was charged into a cylindrical vessel rotating at a rate of 2 rpm which contained an iron and coke mixture at a ratio therebetween equal to 3:1 respectively.
  • the amount of sediment formed after the above treatment was 1.0 g/l.
  • the composition of the input water and treated water is presented in
  • the process according to present invention allows the water with a considerable amount of heavy metal ions, including iron, to be effectively treated.
  • the combination of two processes in sequence operates to remove heavy metal ions to a much greater extent than any of the two process individually (see comparative examples 18 and 19).
  • the successive two- stage treatment of the present invention it becomes possible to reduce the content of Fe 3+ ions contained in the input water from 410.0-3.5 to 0.004-0.01 mg/l, as well as to decrease the amount of Fe 2+ ions from 975.0-1.1 to 0.03- 0.01 mg/l, with the content of other chemical elements being significantly lowered.
  • the one stage treatment of the input water by adding the alkaline reagent in an amount sufficient to raise its pH value to 3.5, followed by the treatment of said water in a cylindrical vessel resulting in its pH increase to 5.3 does not provide the effective purification of water as achieved in examples 1-16.
  • the content of Fe 3+ and Fe 2 ions in the water treated according to example 17 respectively was 0.15 and 4.6 mg/l. But this was the case when a significant amount of other chemical elements, particularly Zn ions, remained in treated water.
  • Example 19 is not effective either, because in this case the content of Fe 2+ ions is not decreased but rather is increased. This phenomenon results from iron dissolving during the coagulation process. In addition, after the above treatment a considerable amount of other chemical elements remain in the water.
  • the invention can be used for treating and preparing waters containing the considerable amount of heavy metal ions which further could be used to satisfy the production needs as well as be discharged into the water streams without the environment being polluted.

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

L'invention concerne un procédé amélioré à deux étapes pour éliminer les ions de métaux lourds de l'eau acide de pH compris entre 2.0 et 3.3. Une quantité spécifique de réactif alcalin est d'abord ajoutée dans l'eau d'alimentation pour élever le pH entre 4.0 et 6.0. La quantité spécifique de réactif alcalin est déterminée selon la formule: (0.03 à 4.2) grammes/litre + (2.0 à 2.8) x [Fe3+] grammes/litre dans laquelle [Fe+3] représente la concentration en ions Fe+3 présente dans l'eau acide, le cas échéant. Ensuite, le mélange résultant, ainsi que les sédiments formés à la suite de la précipitation partielle à partir de métaux lourds, est transféré dans un récipient rempli de substances formant des paires galvaniques, c'est-à-dire le fer et le coke, le fer et le cuivre, l'aluminium et le coke ou l'aluminium et le cuivre, ou leurs combinaisons. Le mélange est maintenu en contact étroit avec les substances formant des paires galvaniques pendant 5 à 60 minutes, provoquant une précipitation augmentée supplémentaire d'ions de métaux lourds du mélange.
PCT/CA1994/000012 1993-02-15 1994-01-05 Procede pour eliminer les ions de metaux lourds de l'eau Ceased WO1994018126A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU58307/94A AU5830794A (en) 1993-02-15 1994-01-05 Process for removing heavy metal ions from water

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
UA93030245 1993-02-15
UA93030245 1993-02-15
UA93051341 1993-07-22
UA94051341 1993-07-22

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WO1994018126A1 true WO1994018126A1 (fr) 1994-08-18

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997036829A1 (fr) * 1996-03-28 1997-10-09 Geo2 Limited Procede pour traiter des eaux usees acides
AU704342B2 (en) * 1996-03-28 1999-04-22 Geo2 Limited Method for treating acidic waste water
US6139753A (en) * 1997-03-21 2000-10-31 Geo2 Limited Method for treating acidic waste water
US6932909B2 (en) 2002-01-15 2005-08-23 Kroff Chemical Company, Inc. Method of treating mine drainage
MD4297C1 (ro) * 2013-02-06 2015-03-31 Государственный Университет Молд0 Procedeu de epurare galvanochimică a apelor reziduale de coloranţi organici

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SU1527183A1 (ru) * 1987-12-02 1989-12-07 Всесоюзный Научно-Исследовательский Институт По Охране Вод Способ очистки сточных вод от ионов т желых металлов
DE3841590A1 (de) * 1987-12-10 1989-06-22 Nippon Kokan Kk Verfahren zur raffination von eisenion-haltiger saurer loesung
SU1730048A1 (ru) * 1988-07-08 1992-04-30 Государственный научно-исследовательский и проектный институт по обогащению руд цветных металлов "Казмеханобр" Способ удалени ионов т желых металлов из сточных вод
SU1740326A1 (ru) * 1989-03-20 1992-06-15 Украинский Институт Инженеров Водного Хозяйства Способ очистки отработанных щелочных медно-хлоридных травильных растворов
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