Extraction of iron ions from water solutions with vegetable oils

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention can be applied in chemical industry, metallurgy and purification of industrial and domestic sewages. Extraction of iron with vegetable oils is realised from water solution with ratio water (W) to organic (O) phase W:O≥3 for Fe (III) and W:O= 3-6 for Fe(II); at pH 2-3 for Fe (III) and 9-11 for Fe (II) and Fe (III). Time of extraction for Fe (III) is 1-3 min and not more than 60 min for Fe (II).

EFFECT: method ensures high degree of efficiency of iron extraction from water solutions with simultaneous efficiency and safety of the process.

2 cl, 10 dwg, 3 tbl

 

Extraction of iron from aqueous solutions relates to the field of extraction of substances organic extractants from aqueous solutions and can be used in ferrous and nonferrous metallurgy, as well as for the treatment of industrial and domestic wastewater.

A method of obtaining iron recovery of iron ore to metal [Rian R., Cetanu I. Inorganic chemistry, part 2. - M.: Mir, 1972, s].

The disadvantage of this method is the high consumption of energy and the formation of environmentally hazardous emissions into the atmosphere.

The closest technical solution is the extraction of iron ions from aqueous hydrochloric acid solutions by tributyl phosphate (TBP) in the processing of natural and technogenic raw materials [I.D. Reznik, G.P. Ermakov, AM Schneerson. Nickel, part 3. - M.: OOO "Science and technology", 2004. 608 S. proceedings of VII International conference "Sustainable development of mountain territories in the conditions of global changes", Vladikavkaz. 2010. P.45].

The disadvantage of this method is the contamination of the final products of phosphorus due to the solubility of TBP in hydrochloric acid solutions. In addition, the extractant is subjected to hydrolysis, degradation and destruction by deterioration extraction properties.

The objective of the invention is the use of efficient and effective method for extracting iron from aqueous solutions.

The technical result is, which can be obtained by use of the invention is economy and efficiency in the extraction of iron from aqueous solutions.

This technical result is achieved by the fact that in the known method of extraction of iron from aqueous solution, comprising contacting the extractant and the solution, stirring the mixture, settling and phase separation, extraction is carried out on an aqueous solution of vegetable oils in relation to the water (In) organic (O) phase In:O≥3 for Fe (III) and O=3-6 for Fe (II) at pH 2-3 for Fe (III) and 9-11 for Fe (III) and Fe (II) and time of extraction 1-3 min for Fe (III) and not more than 60 min for Fe (II).

The essence of the method is illustrated with data figure 1-10, which indicate the concentration of iron in the original solution, extraction time at a given pH, iron concentration and pH value in the clarified aqueous phase, the distribution coefficient D calculated as the ratio of the equilibrium concentrations of iron in the organic and aqueous phases, removing ε, % mass. from the source, the separation factor β=DFe(III)/DFe(II).

Stirring and maintaining the given value of pH was carried out up until further acid-base characteristics of the system were changed slightly. However, for greater assurance of achieving equilibrium contact organic and aqueous phases was carried out at least one day. Upon reaching the AI balance between organic (O) and a clarified water phase (C) the organic phase was separated from the water, in the latter determined the pH-value and the residual concentration of iron. To maintain a given pH value of the solution in the extraction process as neutralizers used the solutions of alkali NaOH and acid (H2SO4.

Using the values of the concentrations of iron in aqueous solution - the original and after extraction was calculated distribution coefficient of iron D between the organic and aqueous phases.

For studies used a crystalline salts FeCl3·6H2O and FeSO4·2H2O.

Examples of practical applications

Example 1 (1)

Figure 1 is given the dependence of the residual ion concentration of Fe (III) from the pH value of the solution. With0=1.26 g/DM3; O:=1:3, time of day. Extraction is carried out at pH=2-3 and 9-11. At pH≤1 iron ion is not extracted, and at pH>11 precipitation is formed black. In the range of pH=4-8 precipitation is formed brown. We can assume that near pH hydrate education Fe (III) extraction at the expense of the ionic bond between oleic acid anion and cation Fe (III), and in the range of pH 9-11 formed complex of Fe (III) with the components of the extractant ions and HE-, collateralise in the organic phase. The best results were obtained at pH 10, the day of extraction, the residual concentration is equal to C=0,1025 g/DM3D=33,88. The structure of the oil phase heliopan what I color brown. In these conditions, Fe (II) extracted only at pH 10, from a solution With0=1.28 g/DM3within 1 hour of extraction of the residual concentration of Fe (II) is equal to C=0,094 g/DM3; D=34,46. In the range of pH 4-9 precipitation is formed brown. Probably the extraction of Fe (II) associated with the oxidation of Fe (II) ion to Fe (III) and the last extraction of the oil phase. This is evidenced by the close values of the distribution coefficients D as Fe (II)ion and ion Fe (III).

Example 2 (figure 2, 3)

Figure 2 given the dependence of the distribution coefficient D, the ratio of aqueous phase (In) organic (O):O from solutions of salts of Fe (III) at pH 10. Extraction of the ions Fe (III) is carried out In:O≥3 almost immediately, the residual concentration is approximately the same and equal to C=0,095 g/DM3. Extraction of the ions Fe (III) is formed on the bottom of a glass plaque brown.

Figure 3 given the dependence of the distribution coefficient D ions Fe (II) from the relationship:o Extraction of ions Fe (II) is within O=3-6. For relationships:O=3 and 4 With0=1, 56 and 1.71 g/DM3accordingly, and for O=5 and 6 With0=1, 16 and 1.28 g/DM3respectively. In:O≥7 precipitation is formed black. In the extraction process is the oxidation of the ions Fe (II) to Fe (III), so the curve 1 obtained in the calculation of the total iron, and curve (2) - Fe (II).

Example 3 (4-6, table 1)

Figure 4 is given the dependence is of efficient distribution D on the initial concentration of the ions Fe (III) and Fe (II), g/DM3their individual solutions. Conditions of extraction: pH 10, O:=1:3. Extraction of the ions Fe (III) is carried out almost immediately, the residual concentration is approximately the same and equal to C=0,095 g/DM3. C0>3 g/DM3precipitation is formed brown. Extraction of the ions Fe (II) is carried out within 1 hour. C0>1.6 g/DM3precipitation is formed black. Dependence D=f(C0) - line:

Fe(III)D=31,620-3,533(R2=0,997)
F(II)D=11,18 C0+16,75(R2=0,919)

Figure 5 is given the dependence of the residual ion concentration of Fe (II) from the time of extraction. Conditions of extraction: pH 10, O:=1:3, t=22°C. the Process is terminated during 30 min at O:=1:3 and 70 min at O:V=1:4,5.

Figure 6 shows the isotherm extraction of ions Fe (II) - dependence of the distribution coefficient D from the equilibrium ion concentration of Fe (II), g/DM3. Conditions of extraction: pH 10, O:=1:3, t=22°C.

The data in table 1 characterize the dependence of C=f(τ), ln(C0/(C)=f(τ), 1/S=f(τ), 1/S2=f(τ). It is seen that when the ratio A:B=1:4.5 and t=22°C the process is described by a kinetic equation of zero order, it is likely that it does not depend on concentration, and determines the I area of the interfacial surface.

0,975
Table 1
The correlation coefficient for dependency:=f(τ), ln(C0/C)=f(τ), 1/C=f(τ), 1/C2=f(τ), obtained according to figure 5
t/CB:OC, g/DM3R2
C=(τ)ln(C0/C)=f(τ)1/C=f(τ)1/S2=f(τ)
223:11,590,7230,9640,9580,835
223:10,990,6460,9480,9430,833
223:10,510,6840,9910,8700,790
224,5:11,420,9480,7510,602

From the data of table 1 it follows that when the ratio A:B=1:3

ln (C0/(C)=f(τ) is linear and views

ln(C0/(C)=τ, (1)

where K is the rate constant of the process.

According to figure 5 the calculated values of K in equation (1):

With0, g/DM30,510,991,59
K, min-10,0640,0500,041

In the interval of the initial concentrations0or =0.51-1,59 g/DM3with increasing concentration the rate of the process decreases.

Example 4 (Fig.7-9, table 2)

7 given the dependence of the residual ion concentration of Fe (II) temperature.

Data table 2 characterize the dependence of C=f(τ), ln(C0/C)=f(τ), 1/C=f(τ), I/S2=f(τ) according to Fig.7.

From the data of table 2 it follows that when the ratio A:B=1:3 and t=15-35°C function ln(C0/(C)=f(τ) is linear and described by equation (1).

According to Fig.7. calculated values of K in equation (1):

t, °C15223
To, min-10,0230,0500,093

In the temperature range t=15-35°C increase in temperature the rate of the process increases.

1,50
Table 2
The correlation coefficient for dependency=f(τ), ln(C0/(C)=f(τ), 1/S=f(τ), 1/C2=f(τ), obtained according to Fig.7
t, °CIn:C, g/DM3R2
C=(τ)ln(C0/C)=f(τ)1/S=f(τ)l/C2=f(τ)
153:11,500,9620,9640,8720,802
223:11,590,7230,9640,9580,835
353:10,8280,9700,9650,850

On Fig given the dependence of the distribution coefficient D temperature, °C, of the individual solutions of salts of Fe (III) and Fe (II). Conditions of extraction: pH 10, O:=1:3, Co, g/DM3: 2 Fe (III), 1 Fe (II). Extraction from solutions of salts of Fe (III) occurs almost instantaneously, and from solutions of salts of Fe (II) - within hours.

Figure 9 according to Fig.7. the obtained dependence of the logarithm of the residual ion concentration of Fe (II) from the inverse temperature T=288, 295, 308°K (t=15, 22, 35°C). The extractant - olive oil, C0=1.5 g/DM3at pH 10, O:V=1:3.

According to figure 9 for the equation of Arrhenius equation of the form

lnk=lnk0-E/RT,

where ln k0- preexponent,

E - the activation energy of the extraction process, j/mol,

R=8,314 j/(mol·C) is the universal gas constant,

the calculated value of activation energy equal to E=52378 j/mol.

Based on kinetic analysis of reaction, we can assume that the first order process and the average value of activation energy E=52,4 kJ/mol indicate that, probably, the process of extraction of iron ions (II) vegetable oil lies in the kinetic region and is limited by the oxidation of Fe (II) to Fe (III) and the subsequent formation of the complex ion Fe (III) with the components of the extractant, which is laterals in the organic phase.

Example 5 (figure 10).

Figure 10 is given the dependence of the distribution coefficient D from vegetable oil: 1 apricot, 2 - pumpkin, 3 - cedar, 4 - soybean, 5 - grape, 6 - corn, 7 - walnut, 8 - sunflower, 9 - linen, 10 - olive.

Conditions of extraction: O:=1:3, pH 10, t=20°C, C0=1.4 to 1.5 g/DM3.

All investigated oils are well extracted ions Fe (III).

High rates of extraction of ions Fe (II) was obtained for apricot, soybean, sunflower and linseed oils and poorly extracted ions Fe (II) olive, pumpkin, pine and corn.

Example 6 (table 3)

In table 3 are given the results of extraction of iron ions from a mixture of salts of Fe (II) and Fe (III). Conditions of extraction: pH 10; O:=1:4,5; t=20°C, extraction time 1-3 min, initial concentration of C0and the final concentration, g/inch Obtained the distribution coefficient D, the separation factor β=DFe(III)/DFe(II), removing ε, in % of the original. It is seen that with increasing concentration of the separation factor increases.

Table 3
The results of extraction of iron ions from a mixture of salts of Fe (II) and Fe (III)
With0, g/DM3C, g/DM3 Dε, %β
Fe (II)Fe (III)Fe (II)Fe (III)Fe (II)Fe (III)Fe (II)Fe (III)
0,540,540,100,1019,819,881,4881,481,00
0,920,920,110,1033,1436,9088,0489,131,11
1,992,050,850,186,0346,7557,2991,22of 7.75

During extraction, the extract has a gel structure, its volume increases by 5-10% of the volume of the extractant.

Precipitation Fe (III) are brown, and precipitation of Fe (II) - black color. Precipitation of black color after drying, magnetic and have the composition FeO·Fe2O3or Fe3O4.

High rates of extraction obtained, probably because the composition of vegetable oils containing oleic acid and other components, is able to extract heavy metal ions. Vegetable oil is a saturated or unsaturated (with one, two and three double bonds) monobasic fatty acids with unbranched carbon chain and an even number of carbon atoms (mainly C16and C18). So, oleic acid, % wt.: in sunflower oil 24-40, in corn oil - 30-49, in olive oil - about 80 in soy oil - 23-29. In addition, vegetable oils found in small quantities of fatty acids with odd numbers of carbon atoms (C15to C23).

High rates of ion extraction of non-ferrous metals, vegetable oils also suggest that the zone of influence of the industrial enterprises of non-ferrous metals ions can accumulate in plants from the soil, especially when the discharge of untreated industrial wastewater. This shows the high level of ecological danger for plants and animals ions of non-ferrous metals in the soil as a result of activity of industrial enterprises.

The method of extraction of the ion is in iron from aqueous solution, including the contacting of the solvent and solution, stirring the mixture, settling and separation of the phases, wherein the extraction is carried out on an aqueous solution of vegetable oils in relation to the water (In) organic (O) phase V:≥3 for Fe (III) and O=3-6 for Fe (II); at pH 2-3 for Fe (III) and 9-11 for Fe (II) and Fe (III) and time of extraction 1-3 min for Fe (III) and not more than 60 min for Fe (II).



 

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