SYNERGISTIC EXTRACTION OF ZINC(II) BY MIXTURES OF PRIMARY AMINE N1923 AND CYANEX272

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SYNERGISTIC EXTRACTION OF ZINC(II) BY MIXTURES OFPRIMARY AMINE N1923 AND CYANEX272Qiong Jia , Deqian Li & Chunji NiuPublished online: 15 Feb 2007.

To cite this article: Qiong Jia , Deqian Li & Chunji Niu (2002) SYNERGISTIC EXTRACTION OF ZINC(II) BY MIXTURES OF PRIMARYAMINE N1923 AND CYANEX272, Solvent Extraction and Ion Exchange, 20:6, 751-764, DOI: 10.1081/SEI-120016077

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SYNERGISTIC EXTRACTION OF ZINC(II)BY MIXTURES OF PRIMARY AMINE

N1923 AND CYANEX272

Qiong Jia, Deqian Li,* and Chunji Niu

Laboratory of Rare Earth Chemistry and Physics,

Changchun Institute of Applied Chemistry, Chinese

Academy of Sciences, Changchun, 130022, P. R. China

ABSTRACT

The extraction of zinc(II) and cadmium(II) from chloride solu-

tion by mixtures of primary amine N1923 and Cyanex272 (HA)

was studied. The synergistic effect was observed for the

extraction of zinc(II) while no synergistic effect for cadmium(II),

which makes it possible to separate zinc(II) and cadmium(II)

with the mixtures. The results showed that zinc(II) was extrac-

ted as (RNH3Cl)3 �ZnClA instead of ZnA2 � 2HA which was

extracted by Cyanex272 alone. The extraction mechanism was

discussed and the formation constants and thermodynamic func-

tions were determined. The separation factors between zinc(II)

and cadmium(II) were calculated.

Key Words: Extraction; Zinc; Cadmium; Primary amine N1923;

Cyanex272

751

SOLVENT EXTRACTION AND ION EXCHANGE

Vol. 20, No. 6, pp. 751–764, 2002

DOI: 10.1081=SEI-120016077 0736-6299 (Print); 1532-2262 (Online)Copyright # 2002 by Marcel Dekker, Inc. www.dekker.com

*Corresponding author. E-mail: [email protected]

©2002 Marcel Dekker, Inc. All rights reserved. This material may not be used or reproduced in any form without the express written permission of Marcel Dekker, Inc.

MARCEL DEKKER, INC. • 270 MADISON AVENUE • NEW YORK, NY 10016

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INTRODUCTION

Organophosphorus extractants have been widely studied in the past decades.

Earlier works were mainly concentrated on di-(2-ethylhexyl)-phosphoric acid

(D2EHPA) and 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (HEH=EHP)

which led to dramatic improvements in extracting metal ions.[1–3] In recent years,

several new phosphinic acids introduced by the Cyanamid Co. attracted more

attention. The extraction of Zn2þ, Cd2þ and other divalent metal ions from sulphate

and nitrate solutions by Cyanex272, Cyanex302, and Cyanex301 has been studied in

detail.[4–7] Alguacil et al.[8] compared the extraction of Zn2þ in aqueous hydrochloric

media by organophosphorus acids and found that it increased in the order:

Cyanex302>D2EHPA>Cyanex272. The extraction of Cd2þ from chloride solution

by Cyanex302 and Cyanex301 has also been studied.[9–11] However, the extraction of

Zn2þ from chloride medium by Cyanex272 has not been reported in detail yet.

Synergistic effects are an important phenomenon in the solvent extraction

and have been studied extensively.[12–16] Synergistic extraction of Zn2þ and Cd2þ

by organophosphorus extractants or amines has been reported.[17–19] However,

most works were concentrated on H2SO4 and HNO3 media. Chloride solution is

the common medium for extraction and separation of Zn2þ and Cd2þ.[20,21]

Recently, our group has studied the synergistic extraction of Zn2þ from chloride

medium by primary amine N1923 and HEH=EHP.[22]

In the present work, the synergistic extraction of Zn2þ by N1923 and

Cyanex272 was studied. Distribution data were analyzed both graphically and

numerically to determine the composition of the extracted complexes and their

formation constants. Effects of the aqueous acidity, the ratio of two extractants

and experimental temperature on the extraction were discussed. It is possible to

separate the two cations by using mixtures of N1923 and Cyanex272.

EXPERIMENTAL

Reagents

Primary amine N1923 with a purity greater than 99% was supplied by

Shanghai Organic Chemistry Institute. Cyanex272 was kindly supplied by the

CYTEC Canada, Inc. and used without further purification. The extractants were

dissolved in n-heptane to the required concentration. The concentration of

primary amine N1923 was measured by titration with standard hydrochloric acid

solution. The amine was acidified by an equivalent amount of hydrochloric acid

to form the ammonium salt.

Stock solutions of ZnCl2 and CdCl2 were prepared with AR chemicals. The

metal ions were analysed by titration with EDTA. All extraction experiments were

752 JIA, LI, AND NIU



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performed at constant ionic strength (1.5 mol=L). All the other reagents were of

analytical reagent grade.

Apparatus

A pHS-3C digital pH meter made by Shanghai Rex Instruments Factory

was used for pH measurements.

Methods

For the equilibrium experiments, equal volumes (5 mL each) of aqueous

and organic phases were mixed and shaken for 30 min at 293� 1K (except for the

temperature experiments), which was sufficient for equilibrium attainment. After

phase separation, Zn2þ and Cd2þ in the aqueous phase were determined by titration

with EDTA. The concentration of metal ions in the organic phase was determined

by difference. These concentrations were used to obtain the distribution ratio, D.

RESULTS AND DISCUSSION

Extraction of Zn2þ by N1923

Le et al.[23] have determined that N1923 exists predominantly as trimeric

species and the following reaction occurs when ZnCl2 is extracted.

ZnCl2ðaÞ þ ðRNH3ClÞ3ðoÞ !K1

ðRNH3ClÞ3 � ZnCl2ðoÞ ð1Þ

The equilibrium constant (K1) is:

K1 ¼D1ð1þ

P4i¼1 bi½Cl�iðaÞÞ

b2½Cl�2ðaÞ½ðRNH3ClÞ3�ðoÞ¼

D1Y

½ðRNH3ClÞ3�ðoÞð2Þ

where D1 is the distribution ratio of the metal; ‘‘a’’ and ‘‘o’’ denote aqueous and

organic phase respectively; Y can be expressed as:

Y ¼1þ

P4i¼1 bi½Cl�i

b2½Cl�2

where bi represents the stability constant of ZnCli.[24]

The analytical data for the extraction of Zn2þ from 1.5 mol=L NaCl

solutions by N1923 are given in Table 1. log K1 was calculated to be 1.73� 0.04.

SYNERGISTIC EXTRACTION OF Zn(II) 753



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Extraction of Zn2þ by Cyanex272

If the extraction of Zn2þ by Cyanex272 from chloride medium is expressed

as follows:

ZnCl2ðaÞ þ 1þp

2

� �ðHAÞ2ðoÞ !

K2ZnA2 � pHAðoÞ þ 2HþðaÞ þ 2ClðaÞ ð3Þ

The relationship between the distribution ratio D2 and the extraction constant K2

can be described as follows:

log D2 2pH ¼ 1þp

2

� �log½ðHAÞ2�ðoÞ þ log K2 log Y 2 log½Cl�ðaÞ

ð4Þ

The plots of log D27 2pH vs. log[(HA)2](o) are shown in Fig. 1, giving straight

lines with a slope of about 2. The extraction reaction of Zn2þ from chloride

solution by Cyanex272 can thus be expressed as:

ZnCl2ðaÞ þ 2ðHAÞ2ðoÞ !K2

ZnA2 � 2HAðoÞ þ 2HþðaÞ þ 2ClðaÞ ð5Þ

log K2 was calculated to be 0.93� 0.04.

Extraction of Zn2þ by N1923 and Cyanex272 Mixtures

The results of the extraction of Zn2þ by N1923 and Cyanex272 mixtures

in n-heptane are given in Fig. 2, showing an evident synergistic effect.

The synergistic enhancement factor, Dmax=(DN1923þDCyanex272), was calculated

following Xu[25] to be 1.79.

Table 1. Data of Concentration of Zn2þ and (RNH3Cl)3 and Equilibrium Constants

(pH¼ 1.56, m¼ 1.50 mol=L)

No.

[Zn2þ](a),

mol=L

[Zn2þ](o),

mol=L

[(RNH3Cl)3](o),

mol=L log K1

Average

log K1

1 0.017 0.003 0.0055 1.76

1.73� 0.04

2 0.016 0.004 0.011 1.73

3 0.015 0.005 0.017 1.71

4 0.014 0.006 0.023 1.69

5 0.013 0.007 0.029 1.73

6 0.012 0.008 0.035 1.75




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Figure 1. Relationship between distribution ratio D2 and equilibrium concentration of

Cyanex272. s—[Zn2þ](a)¼ 0.02 mol=L, pH¼ 1.56, m¼ 1.50 mol=L; 4—[Zn2þ](a)¼

0.04 mol=L, pH¼ 1.56, m¼ 1.50 mol=L.

Figure 2. Synergistic extraction of Zn2þ by N1923 and Cyanex272. [Zn2þ](a)¼

0.02 mol=L, pH¼ 1.56, m¼ 1.50 mol=L, [N1923](o)þ [Cyanex272](o)¼ 0.20 mol=L.

s—N1923; u—Cyanex272; 4—N1923þCyanex272.




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Since Cyanex272 exists predominantly as dimeric species and N1923 as

trimeric species in the range of concentrations considered, the synergistic

extraction equation can be described as:

ZnCl2ðaÞ þx

3ðRNH3ClÞ3ðoÞ þ

y

2ðHAÞ2ðoÞ !

K12ðRNH3ClÞxZnCl2yAyðoÞ

þ yHþðaÞ þ yClðaÞ ð6Þ

Then the distribution ratio, D12 of the mixed system should be:

log D12 ¼x

3log½ðRNH3ClÞ3�ðoÞ þ

y

2log½ðHAÞ2�ðoÞ þ ypHþ log K12

log Y y log½Cl�ðaÞ

ð7Þ

In order to examine the composition of the extracted complexes in the

N1923þCyanex272 system, the distribution ratio D12 was obtained at various

acidities at fixed concentrations of N1923 and Cyanex272. As shown in Fig. 3,

the plots of log D12 vs. pH give a straight line with a slope of about 1. In the same

way, when the concentration of one extractant is varied at fixed aqueous acidity

and concentration of the other extractant, the plots of log D127 pH vs. the

concentration of extractants are shown in Fig. 4. The plots are linear with slopes

of about 1.0 and 0.5 for [(RNH3Cl)3](o) and [(HA)2](o) respectively.

The synergistic extraction can thus be written as:

ZnCl2ðaÞ þ ðRNH3ClÞ3ðoÞ þ1

2ðHAÞ2ðoÞ !

K12

ðRNH3ClÞ3 � ZnClAðoÞ þHClðaÞ

ð8Þ

The value of K12 is shown in Table 2.

The following hypothetical synergistic reactions can be derived from the

Eqs. (1), (5) and (8):

ðRNH3ClÞ3 � ZnCl2ðoÞ þ1

2ðHAÞ2ðoÞ !

b1

ðRNH3ClÞ3 � ZnClAðoÞ þ HClðaÞ

ð9Þ

ZnA2 � 2HAðoÞ þ ðRNH3ClÞ3ðoÞ þ HClðaÞ !b2

ðRNH3ClÞ3 � ZnClAðoÞ

þ3

2ðHAÞ2ðoÞ ð10Þ

ðRNH3ClÞ3 � ZnCl2ðoÞ þ ZnA2 � 2HAðoÞ þ ðRNH3ClÞ3ðoÞ

!b3

2ðRNH3ClÞ3 � ZnClAðoÞ þ ðHAÞ2ðoÞ ð11Þ




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where b1, b2 and b3 are equilibrium constants which can be expressed as:

log b1 ¼ log K12 log K1

log b2 ¼ log K12 log K2

log b3 ¼ 2 log K12 log K1 log K2

The b1, b2, b3 values follow the order: b3> b2> b1 (shown in Table 2). Among

the Eqs. (9), (10), and (11), Eq. (11) contributes most to the synergistic

extraction. The extracted complexes ZnA2 � 2HA and (RNH3Cl)3 �ZnCl2 are more

prone to form the final synergistic complex (RNH3Cl)3 �ZnClA. Comparing

Eq. (9) with Eq. (10), it follows that b2> b1. A possible explanation is that

the extracted complex of Zn2þ with N1923 is more stable than that with

Cyanex272 and the reaction of ZnA2 � 2HA with N1923 is easier than that of

(RNH3Cl)3 �ZnCl2 with (HA)2. This phenomenon is similar to that observed for

the synergistic extraction of Zn2þ by mixtures of N1923 and HEH=EHP.[22]

Influence of Temperature

The distribution ratios D12 of the synergistic extraction of Zn2þ by N1923

and Cyanex272 were studied at different temperatures (20 C� 50 C) at fixed

aqueous acidity and concentrations of N1923 and Cyanex272. The plot of

Figure 3. Relationship between distribution ratio D12 and pH. [Zn2þ](a)¼ 0.02 mol=L,

m¼ 1.50 mol=L, [N1923](o)¼ [Cyanex272](o)¼ 0.10 mol=L.




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Figure 4. Relationship between distribution ratio D12 and equilibrium concentration

of N1923 and Cyanex272, [Zn2þ](a)¼ 0.02 mol=L, pH¼ 1.56, m¼ 1.50 mol=L. (a)

4—[Cyanex272](o)¼ 0.08 mol=L; s—[Cyanex272](o)¼ 0.04 mol=L. (b) 4—[N1923](o)¼

0.10 mol=L; s—[N1923](o)¼ 0.06 mol=L.




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log D12 vs. 1=T is shown in Fig. 5, giving a slope of 524.4. The change of

enthalpy of the reaction DH can be determined according to the equation:

D log D12

Dð1=T Þ¼DH

2:303R

DH was calculated to be DH¼10.04 kJ mol1.

The synergistic extraction is an exothermic reaction, that is, the distribution

ratio D12 decreases with an increase of the experimental temperature. DG and DS

of the system at 20 C can be calculated as:

DG ¼ RT ln K12 ¼ 5:24 kJ mol1

DG ¼ DH TDS ) DS ¼DH DG

T¼ 16 J K1 mol1 < 0

Table 2. Equilibrium Constants and Formation Constants of Zn2þ Extracted by N1923

and Cyanex272

log K1 log K2 log K12 logb1 logb2 log b3

1.73� 0.04 0.93� 0.04 1.94� 0.03 0.21� 0.02 2.87� 0.03 3.08� 0.02

Figure 5. Relationship between distribution ratio D and temperature. [Zn2þ]¼ 0.02 mol=L,

pH¼ 1.56, m¼ 1.50 mol=L, [N1923](o)¼ [Cyanex272](o)¼ 0.10 mol=L.




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The signs of the DH and DS change indicate that the synergistic extraction is

enthalpy driven. The negative value of DS indicates that more order is introduced

in the system upon metal extraction, that is, the disorder caused by metal ion

dehydration is more than compensated by the reduction of the number of particles

brought about by the formation of the synergistic complex.

Extraction of Cd2þ by N1923 and Cyanex272 Mixtures

Figure 6 shows the extraction of Cd2þ by N1923 and Cyanex272 mixtures.

It is obvious that there is no synergistic effect between N1923 and Cyanex272.

Separation of Zn2þ and Cd2þ with Mixtures of

N1923 and Cyanex272

The effect of the extractant concentration on the extraction of Zn2þ and

Cd2þ by mixtures of N1923 and Cyanex272 is shown in Fig. 7. It is difficult to

separate Zn2þ and Cd2þ with Cyanex272 alone. The separation factors of Zn2þ

and Cd2þ with the mixtures are given in Table 3. It is obvious that Zn2þ and Cd2þ

can be separated at a proper ratio of the extractants, i.e., it is feasible and

Figure 6. Extraction of Cd2þ by N1923 and Cyanex272. [Cd2þ]¼ 0.02 mol=L,

pH¼ 1.50, m¼ 1.50 mol=L, [N1923](o)þ [Cyanex272](o)¼ 0.20 mol=L. s—N1923;

u—Cyanex272; 4—N1923þCyanex272.




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advantageous to separate Cd2þ from bulk zinc at a low proportion of Cyanex272

in the mixture, while to separate Zn2þ from bulk cadmium a high proportion of

Cyanex272 must be used.

CONCLUSION

Mixtures of N1923 and Cyanex272 exhibit evident synergistic effects when

used to extract Zn2þ from chloride solution. The synergistic enhancement factor

was calculated as 1.79. The stoichiometries of the extracted complexes have been

determined by graphical and numerical methods to be (RNH3Cl)3 �ZnClA with

the synergistic mixture, and ZnA2 � 2HA with Cyanex272 alone. The equilibrium

constants and formation constants were calculated and an extraction mechanism

proposed. The extraction is an exothermic process and the thermodynamic

functions were determined. The mixture exhibits no synergistic effects for Cd2þ,

Figure 7. Extraction of Zn2þ and Cd2þ by N1923 and Cyanex272. [Zn2þ]¼ 0.02 mol=L,

pH¼ 1.56, m¼ 1.50 mol=L, [Cd2þ]¼ 0.02 mol=L, pH¼ 1.50, m¼ 1.50 mol=L, [N1923](o)þ

[Cyanex272](o)¼ 0.20 mol=L.

Table 3. bZn=Cd for Mixtures of N1923 and Cyanex272

XCyanex272 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

bZn=Cd 0.80 0.69 0.78 0.90 0.97 1.23 1.38 1.63 2.15 3.56 —




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which provides possibilities for Zn2þ and Cd2þ separations at a proper ratio of the

extractants.

ACKNOWLEDGMENTS

The authors wish to thank Dr. W. A. Rickelton of Cytec Canada for

supplying Cyanex272. This project was supported by the State Key Project of the

Foundation Research (G1998061301) and National Natural Science Foundation

of China (29771028, 29801004).

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Documents

SYNERGISTIC EXTRACTION OF ZINC(II) BY MIXTURES OF PRIMARY AMINE N1923 AND CYANEX272