MD4142C1 - Process for water purification from hydrogen sulfide and sulfides - Google Patents
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Abstract
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Invenţia se referă la un procedeu de purificare a apei de hidrogen sulfurat şi sulfuri şi poate fi utilizată în gospodării comunale, piscicole, în acvarii publice, filtre autonome, precum şi la purificarea apelor subterane. The invention refers to a process for purifying water from hydrogen sulphide and sulphides and can be used in communal households, fish farms, in public aquariums, autonomous filters, as well as for the purification of underground water.
Circa 50% din cantitatea totală de ape subterane de pe teritoriul republicii se caracterizează printr-un conţinut sporit de diferiţi poluanţi (hidrogen sulfurat, nitraţi, fluor, metale grele). Compuşii sulfului (hidrogenul sulfurat, sulfurile) influenţează negativ asupra calităţii organoleptice a apei, au proprietăţi corozive, toxice şi dăunează sănătăţii omului, impunându-se necesitatea eliminării sau reducerea conţinutului lor până la limitele admisibile. About 50% of the total amount of underground water on the territory of the republic is characterized by an increased content of different pollutants (hydrogen sulfide, nitrates, fluorine, heavy metals). Sulfur compounds (hydrogen sulfide, sulfides) negatively influence the organoleptic quality of water, have corrosive, toxic properties and harm human health, imposing the need to eliminate or reduce their content to acceptable limits.
Eliminarea compuşilor sulfului prin aerare în prezenţa unor adsorbanţi şi/sau catalizatori, de exemplu cărbune activ, oxizi superiori ai manganului, complecşi ai flerului are dezavantajul că necesită utilaj şi materiale speciale, procedeele fiind costisitoare. The elimination of sulfur compounds by aeration in the presence of adsorbents and/or catalysts, for example activated carbon, higher manganese oxides, fleur complexes has the disadvantage that it requires special equipment and materials, the processes being expensive.
Este cunoscut procedeul de purificare a apei de hidrogen sulfurat care constă în utilizarea cărbunelui activ BAU-A, unde la barbotarea aerului prin apă, hidrogenul sulfurat şi sulfurile se oxidează [1]. The hydrogen sulfide water purification process is known, which consists in the use of BAU-A activated carbon, where when air is bubbled through the water, hydrogen sulfide and sulfides are oxidized [1].
Dezavantajul procedeului constă în faptul că în procesul de tratare a apei, pe suprafaţa cărbunelui se formează sulf coloidal care blochează porii, scoţându-1 astfel repede din uz. The disadvantage of the process is that in the water treatment process, colloidal sulfur is formed on the surface of the coal which blocks the pores, thus quickly putting it out of use.
La fel este cunoscut procedeul de purificare a apelor de hidrogen sulfurat şi/sau sulfuri prin aerarea apei în prezenţa cărbunelui activ, unde în calitate de cărbune activ se utilizează cărbune activ oxidat, iar aerarea apei se efectuează timp de 30...90 min, cu un debit de aer de 10 ... 15 L/oră la 1 g de cărbune activ oxidat, la un raport de masă cărbune activ oxidat : apă de 1 : (350...450) şi pH-ul apei de 7,5...8,5 [2]. Likewise, the process of purifying hydrogen sulphide and/or sulphide waters by aerating the water in the presence of activated carbon is known, where oxidized activated carbon is used as activated carbon, and the aeration of the water is carried out for 30...90 min, with an air flow rate of 10 ... 15 L/hour per 1 g of oxidized activated carbon, at a mass ratio oxidized activated carbon: water of 1: (350...450) and water pH of 7, 5...8.5 [2].
Dezavantajul acestui procedeu constă în aceea că adsorbanţii carbonici sunt relativ scumpi, în comparaţie cu cei minerali, din care cauză deseori se dă prioritate utilizării adsorbanţilor minerali. The disadvantage of this process is that carbonic adsorbents are relatively expensive, compared to mineral ones, which is why priority is often given to the use of mineral adsorbents.
În calitate de cea mai apropiată soluţie se prezintă procedeul de oxidare a sulfurilor din apă în prezenţa adsorbantului „nisip verde” (greensand) natural sau special prelucrat cu săruri de mangan, apoi cu soluţie de permanganat de potasiu. Forma obţinută de Mn-glauconit şi oxizii manganului servesc în calitate de catalizator şi oxidanţi în procesul de tratare a apelor [3]. As the closest solution, the process of oxidizing sulfides in water in the presence of natural or specially processed "greensand" adsorbent with manganese salts, then with potassium permanganate solution is presented. The obtained form of Mn-glauconite and manganese oxides serve as catalysts and oxidants in the water treatment process [3].
Dezavantajul acestui procedeu constă în faptul că materialul necesar, adică adsorbantul (nisipul verde) este foarte costisitor fiind un material importat. The disadvantage of this process lies in the fact that the necessary material, i.e. the adsorbent (green sand) is very expensive, being an imported material.
În componenţa diatomitului, resurse însemnate ale căruia sunt localizate în lungul fluviului Nistru, recomandate pentru utilizare în procese sorbtive, de floculare-sedimentare la epurarea apelor reziduale, de rând cu materialul silicios provenit din diatomee, există aşa minerale, cum sunt montmorilonitul, ilitul, caolinitul, precum şi componente amorfe - alumosilicaţi, oxizi ai aluminiului şi fierului. Compoziţia chimică generalizată a diatomitului este prezentată în felul următor (%): SiO2 - 85, A12O3 - 3, Fe2O3 - 2, MgO - 0,5, CaO - 2, pierderi la calcinare - 7. In the composition of diatomite, significant resources of which are located along the Dniester river, recommended for use in sorption, flocculation-sedimentation processes for the purification of waste water, along with the siliceous material from diatoms, there are such minerals as montmorillonite, illite, kaolinite, as well as amorphous components - aluminosilicates, aluminum and iron oxides. The generalized chemical composition of diatomite is presented as follows (%): SiO2 - 85, A12O3 - 3, Fe2O3 - 2, MgO - 0.5, CaO - 2, calcination losses - 7.
Problema pe care o rezolvă invenţia constă în elaborarea unui procedeu simplu şi ieftin de purificare a apei de hidrogen sulfurat şi sulfuri. The problem that the invention solves consists in the development of a simple and cheap process for purifying water from hydrogen sulphide and sulphides.
Comparativ cu alţi adsorbanţi, diatomitul este mai ieftin, iar compoziţia poliminerală a lor, precum şi modificarea chimică permite de a manifesta proprietăţi catalitice de adsorbţie sporite. Compared to other adsorbents, diatomite is cheaper, and their polymineral composition, as well as the chemical modification, allows to show increased catalytic adsorption properties.
Procedeul, conform invenţiei, constă în utilizarea diatomitului modificat, obţinut prin tratarea preventivă a diatomitului cu soluţie de 24% de NaOH, luate în raport de 1 : (10…15), timp de 12 ore, după care suspensia obţinută se încălzeşte pe baie de apă la temperatura de fierbere timp de 2 ore, se adaugă în exces o soluţie de 30% de MnCl2 şi se menţine timp de 24 ore la temperatura camerei, faza solidă se filtrează, se imersează şi se menţine în soluţie de 24% de NaOH timp de 24 ore la temperatura camerei, supernatantul se decantează şi faza solidă se expune la aer, după care se spală cu apă distilată până la reacţia negativă la ionii de Cl-, se granulează şi se usucă la temperatura de 105…200ºC, totodată raportul adsorbantului la apa purificată este de 1 : 800. The process, according to the invention, consists in the use of modified diatomite, obtained by preventive treatment of diatomite with a 24% solution of NaOH, taken in a ratio of 1: (10...15), for 12 hours, after which the obtained suspension is heated in a bath of water at boiling temperature for 2 hours, a 30% solution of MnCl2 is added in excess and maintained for 24 hours at room temperature, the solid phase is filtered, immersed and maintained in 24% NaOH solution for 24 hours at room temperature, the supernatant is decanted and the solid phase is exposed to air, after which it is washed with distilled water until the negative reaction to Cl- ions, granulated and dried at a temperature of 105...200ºC, at the same time the ratio of the adsorbent to purified water is 1:800.
Rezultatul invenţiei constă în elaborarea unui procedeu simplu şi ieftin de purificare a apei de hidrogen sulfurat şi sulfuri prin sporirea eficienţei utilizării diatomitului. The result of the invention consists in the development of a simple and cheap process for purifying water from hydrogen sulphide and sulphides by increasing the efficiency of the use of diatomaceous earth.
Conform invenţiei, procedeul posedă următoarele avantaje: According to the invention, the process has the following advantages:
- În procesele de purificare a apelor de hidrogen sulfurat şi sulfuri este utilizat diatomit autohton, cationic modificat în formă de Mn(IV)-diatomit. - In the water purification processes of hydrogen sulphide and sulphides, native, cationically modified diatomite in the form of Mn(IV)-diatomite is used.
- Datorită porozităţii pronunţate (de cca 30 ori mai mare decât a glauconitului), în particulele de diatomit pot fi fixate cantităţi mai mari de compuşi de mangan per unitate de masă, asigurând o durată de utilizare mai mare. - Due to the pronounced porosity (about 30 times higher than that of glauconite), larger amounts of manganese compounds can be fixed in the diatomite particles per unit of mass, ensuring a longer duration of use.
- Densitatea mică (cca 0,3 g/cm3) a diatomitului, comparativ cu cea a „nisipului verde”, permite utilizarea altor tipuri de aparate de tratare a apei, cu adsorbant/catalizator în suspensie, ceea ce face ca procedeul de purificare a apei propus să fie mai ieftin, mai avantajos şi deosebit de cel luat ca cea mai apropiată soluţie. - The low density (approx. 0.3 g/cm3) of diatomite, compared to that of "green sand", allows the use of other types of water treatment devices, with adsorbent/catalyst in suspension, which makes the purification process water proposed to be cheaper, more advantageous and different from the one taken as the closest solution.
- Diatomitul autohton, ca materie primă pentru obţinerea adsorbanţilor/catalizatorilor, este mai ieftin şi prezintă perspective reale pentru solicitări de un spectru mai larg de utilizatori. - Native diatomite, as a raw material for obtaining adsorbents/catalysts, is cheaper and presents real prospects for requests from a wider spectrum of users.
Exemplu concret de realizare Concrete example of realization
Pentru exemplificare s-a folosit diatomitul din localitatea Ghidirim. Mostra de diatomit (fracţiunea <0,14 mm) a fost modificată prin tratarea preventivă a diatomitului cu soluţie de 24% de NaOH, luate în raport de 1 : (10…15), timp de 12 ore, după care suspensia obţinută se încălzeşte pe baie de apă la temperatura de fierbere timp de 2 ore, se adaugă în exces o soluţie de 30% de MnCl2 şi se menţine timp de 24 ore la temperatura camerei, faza solidă se filtrează, se imersează şi se menţine în soluţie de 24% de NaOH timp de 24 ore la temperatura camerei, supernatantul se decantează şi faza solidă se expune la aer, după care se spală cu apă distilată până la reacţia negativă la ionii de Cl-, se granulează şi se usucă la temperatura de 105…200ºC, totodată raportul adsorbantului la apa purificată este de 1 : 800. As an example, the diatomaceous earth from Ghidirim was used. The diatomite sample (fraction <0.14 mm) was modified by preventive treatment of the diatomite with a 24% solution of NaOH, taken in a ratio of 1: (10...15), for 12 hours, after which the obtained suspension is heated on a water bath at boiling temperature for 2 hours, a 30% solution of MnCl2 is added in excess and maintained for 24 hours at room temperature, the solid phase is filtered, immersed and maintained in a 24% solution of NaOH for 24 hours at room temperature, the supernatant is decanted and the solid phase is exposed to air, after which it is washed with distilled water until the negative reaction to Cl- ions, granulated and dried at a temperature of 105...200ºC, at the same time, the ratio of adsorbent to purified water is 1:800.
Reacţia de oxigenare a Mn(II) în Mn(IV) prezintă un proces autocatalitic, schematic incluzând etapele: The oxygenation reaction of Mn(II) in Mn(IV) presents an autocatalytic process, schematically including the stages:
Mn(II) + O2 MnO2(s)\tab(a) Mn(II) + O2 MnO2(s)\tab(a)
Mn(II) + MnO2(s) Mn(II)-MnO2(s)\tab (b) Mn(II) + MnO2(s) Mn(II)-MnO2(s)\tab (b)
Mn(II)-MnO2(s) +O2 2MnO2(s)\tab (c) Mn(II)-MnO2(s) +O2 2MnO2(s)\tab (c)
Testarea capacităţii de adsorbţie/oxidare a ionilor de sulfură în prezenţa adsorbanţilor minerali s-a efectuat folosind soluţie model de Na2S (având pH-ul 8,86, ajustat cu soluţie tampon de tetraborat de sodiu), cu un conţinut recalculat la ioni de S2- circa 250 mg S2- per litru. Contactarea soluţiei model cu adsorbanţii exemplificaţi s-a efectuat în condiţii statice, la raportul solid : lichid egal cu 1 : 800, timp de 24 ore la temperatura de cameră, după care s-a determinat concentraţia de echilibru a ionilor de sulfură în supernatant, folosind metoda colorimetrică cu săruri de plumb. Testing the adsorption/oxidation capacity of sulfide ions in the presence of mineral adsorbents was performed using a model solution of Na2S (having a pH of 8.86, adjusted with sodium tetraborate buffer solution), with a recalculated content of S2- ions around 250 mg S2- per liter. Contacting the model solution with the exemplified adsorbents was carried out under static conditions, at a solid:liquid ratio equal to 1:800, for 24 hours at room temperature, after which the equilibrium concentration of sulfide ions in the supernatant was determined, using the colorimetric method with lead salts.
Pentru comparaţie, s-a testat diatomitul natural integru (fracţiunea <0,14 mm) şi adsorbantul obţinut după tratare cu sare de mangan în condiţiile descrise mai sus, rezultatele fiind prezentate în tabel. For comparison, the intact natural diatomite (fraction <0.14 mm) and the adsorbent obtained after treatment with manganese salt were tested under the conditions described above, the results being presented in the table.
Tabel Table
Capacitatea de eliminare a hidrogenului sulfurat din soluţia model The ability to remove hydrogen sulphide from the model solution
Raportul solid:lichid 1 : 800. Concentraţia iniţială C0=268 mg/L, pH=8,86 Solid:liquid ratio 1 : 800. Initial concentration C0=268 mg/L, pH=8.86
Adsorbantul Concentraţia de echilibru Ce, mg/L Capacitatea de adsorbţie/oxidare Caracteristicile organoleptice ale apei tratate mg/g % Diatomit natural. Mostră uscată la 105°C 80 150 70 Soluţia de echilibru este opacă, are miros de H2S Diatomit tratat cu sare de mangan. Mostră uscată la 105°C 0 214 100 Soluţia de echilibru este uşor opalescentă, colorată în roz pal, miros de H2S nu se simte Diatomit tratat cu sare de mangan. Mostră uscată la 200°C 0 214 100 Soluţia de echilibru nu este colorată, miros de H2S nu se simte Adsorbent Equilibrium concentration Ce, mg/L Adsorption/oxidation capacity Organoleptic characteristics of the treated water mg/g % Natural diatomite. Sample dried at 105°C 80 150 70 The equilibrium solution is opaque, has the smell of H2S Diatomite treated with manganese salt. Sample dried at 105°C 0 214 100 The equilibrium solution is slightly opalescent, colored in pale pink, the smell of H2S is not felt Diatomite treated with manganese salt. Sample dried at 200°C 0 214 100 The equilibrium solution is not colored, the smell of H2S is not felt
Adsorbantul sintetizat prin impregnarea diatomitului cu hidraţi de oxizi Mn(IV) posedă o capacitate de circa 1,5 ori mai înaltă de eliminare a hidrogenului sulfurat din soluţii, în comparaţie cu diatomitul iniţial. Adsorbantul poate fi granulat (brichetat în diferite dimensiuni), iar granulele după calcinare la temperatura de 200°C posedă o duritate mecanică suficientă, nu dispersează în mediu apos şi nu colorează apa tratată, ceea ce prezintă perspective reale de utilizare în practică pentru purificarea apelor. The adsorbent synthesized by impregnating diatomite with hydrates of Mn(IV) oxides has an approximately 1.5 times higher capacity to eliminate hydrogen sulphide from solutions, compared to the original diatomite. The adsorbent can be granulated (briquetted in different sizes), and the granules after calcination at a temperature of 200°C possess sufficient mechanical hardness, do not disperse in aqueous medium and do not color the treated water, which presents real prospects for use in practice for water purification .
1. MD 2480 G2 2004.06.30 1. MD 2480 G2 2004.06.30
2. Николадзе Г. И. Улучшение качества подземных вод. М.: Стройиздат, 1987, с. 240 2. Nikoladze G. И. Improvement of underground water quality. M.: Стройиздат, 1987, с. 240
3. Kogel J.E., Trivedi N.C., Barker J. M., Krukowski S. T. Industrial Minerals and Rocks: commodities, markets, and uses. soc. for Mining. Metallurgy and exploration, Colorado, 2006, p. 495-505 3. Kogel J.E., Trivedi N.C., Barker J.M., Krukowski S.T. Industrial Minerals and Rocks: commodities, markets, and uses. shock. for Mining. Metallurgy and exploration, Colorado, 2006, p. 495-505
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