Adsorption of Sodium Diclofenac in Functionalized Palygoskite Clays
Abstract
:1. Introduction
2. Materials and Methods
2.1. Raw Materials
2.2. Acid and Organic-Functionalization of Raw Palygorskite
2.3. Characterizations
2.4. Experimental Design
2.5. Kinetics and Equilibrium Models
3. Results and Discussion
3.1. Characterization of the Raw and Functionalized Palygorskite
3.1.1. X-ray Diffraction
3.1.2. X-ray Fluorescence Chemical Composition
3.1.3. Thermal Behavior
3.1.4. Specific Surface Area by N2 adsorption (BET)
3.1.5. Zeta Potential
3.2. Influence of pH
3.3. Experimental Design of the Factorial Type of Functionalized Palygorskite Clay
3.4. Adsorption Kinetics
3.5. Adsorption Isotherms
3.6. Characterization after Adsorption by FTIR
3.7. Comparison with Other Adsorbents of Sodium Diclofenac
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Design I | Level | ||
---|---|---|---|
Independent variables | −1 | 0 | +1 |
Mass of acid functionalized (g) | 0.2 | 0.3 | 0.4 |
Concentration of the solution (mg·L−1) | 20 | 30 | 40 |
solution pH | 6 | 8.5 | 11 |
Contact time (h) | 4 | 6 | 8 |
Design II | Level | ||
Independent variables | −1 | 0 | +1 |
Mass of organo-functionalized (g) | −1 | 0 | 1 |
Concentration of the solution (mg·L−1) | 20 | 30 | 40 |
solution pH | 6 | 8.5 | 11 |
Contact time (h) | 4 | 6 | 8 |
Oxides | Raw | Acid | Organic |
---|---|---|---|
SiO2 | 61.9 | 76.0 | 62.0 |
Al2O3 | 18.1 | 11.1 | 18.0 |
Fe2O3 | 8.6 | 5.9 | 8.1 |
MgO | 6.5 | 5.0 | 6.5 |
K2O | 2.8 | 0.6 | 2.7 |
TiO2 | 0.7 | 0.7 | 0.7 |
Cl | - | - | 0.8 |
CaO | 0.5 | - | 0.4 |
Others | 0.9 | 0.7 | 0.8 |
Sample | Specific Surface Area (m2/g) |
---|---|
Raw | 87.233 |
Acid | 142.447 |
Organic | 26.969 |
Experimental Conditions | Acid | Organic | ||||||||
---|---|---|---|---|---|---|---|---|---|---|
Exp. | Mass (g) | Initial Conc. (mg·L−1) | pH | Time (h) | Final Conc. (mg·L−1) | Qt (mg g−1) | Rem (%) | Final Conc. (mg·L−1). | Qt (mg g−1) | Rem (%) |
1 | 0.2 | 20 | 6 | 4 | 2.031 | 1.7969 | 98.25 | 2.015 | 1.7985 | 89.93 |
2 | 0.4 | 20 | 6 | 4 | 2.808 | 0.8596 | 85.96 | 2.931 | 0.8534 | 85.35 |
3 | 0.2 | 40 | 6 | 4 | 2.32 | 3.768 | 94.20 | 5.8 | 3.4200 | 85.50 |
4 | 0.4 | 40 | 6 | 4 | 4.009 | 1.7996 | 89.98 | 6.066 | 1.6967 | 84.84 |
5 | 0.2 | 20 | 11 | 4 | 4.392 | 1.5608 | 78.04 | 8.698 | 1.1302 | 56.51 |
6 | 0.4 | 20 | 11 | 4 | 6.363 | 0.6819 | 68.19 | 8.384 | 0.5808 | 58.08 |
7 | 0.2 | 40 | 11 | 4 | 6.661 | 3.3339 | 83.35 | 10.074 | 2.9926 | 74.82 |
8 | 0.4 | 40 | 11 | 4 | 6.477 | 1.6762 | 83.81 | 18.827 | 1.0587 | 52.94 |
9 | 0.2 | 20 | 6 | 8 | 2.295 | 1.7705 | 88.53 | 2.342 | 1.7658 | 88.29 |
10 | 0.4 | 20 | 6 | 8 | 4.388 | 0.7806 | 78.06 | 3.065 | 0.8467 | 84.68 |
11 | 0.2 | 40 | 6 | 8 | 5.464 | 3.4536 | 86.34 | 6.251 | 3.3749 | 84.38 |
12 | 0.4 | 40 | 6 | 8 | 4.52 | 1.7740 | 88.70 | 5.959 | 1.7020 | 85.10 |
13 | 0.2 | 20 | 11 | 8 | 4.378 | 1.5622 | 78.11 | 9.791 | 1.0209 | 51.05 |
14 | 0.4 | 20 | 11 | 8 | 6.445 | 0.6778 | 67.78 | 8.262 | 0.5869 | 58.69 |
15 | 0.2 | 40 | 11 | 8 | 6.827 | 3.3173 | 82.94 | 10.366 | 2.9634 | 74.09 |
16 | 0.4 | 40 | 11 | 8 | 7.039 | 1.6481 | 82.41 | 19.343 | 1.0329 | 51.64 |
17 | 0.3 | 30 | 8.5 | 6 | 4.332 | 1.7112 | 85.56 | 4.569 | 1.6954 | 84.77 |
18 | 0.3 | 30 | 8.5 | 6 | 3.99 | 1.7340 | 86.70 | 4.225 | 1.7183 | 85.92 |
19 | 0.3 | 30 | 8.5 | 6 | 4.002 | 1.7332 | 86.66 | 4.523 | 1.6985 | 84.92 |
Variation Source | SQ | DF | MS | Fcal | Ftab | R2 |
---|---|---|---|---|---|---|
Regression | 15.8543 | 11 | 1.4413 | 318.53 | 3.605 | 0.9949 |
Residual | 0.0317 | 7 | 0.0045 | |||
Total | 15.8860 | 18 |
Variation Source | SQ | DF | QM | Fcal | Ftab | R2 |
---|---|---|---|---|---|---|
Regression | 19.0551 | 11 | 1.73228 | 282.99 | 3.605 | 0.9942 |
Residual | 0.0428 | 7 | 0.00612 | |||
Total | 19.0979 | 18 |
(a) | |||
Terms | Effects | Regression Coefficient | p-Value |
Mass | −1.3332 | −0.6666 | 0 |
Concentration | 1.3939 | 0.697 | 0 |
pH | −0.1931 | −0.0965 | 0.001 |
Time | −0.0616 | −0.0308 | 0.11 |
Mass and Conc. interation | −0.4161 | −0.2081 | 0 |
Mass and pH interation | 0.0606 | 0.0303 | 0.115 |
Mass and time interation | 0.0274 | 0.0137 | 0.442 |
Conc. and pH interation | −0.0207 | −0.0104 | 0.557 |
Conc. and time interation | −0.0401 | −0.0201 | 0.272 |
pH and time interation | 0.0497 | 0.0249 | 0.183 |
(b) | |||
Terms | Effects | Regression Coefficient | p-Value |
Mass | −1.2624 | −0.6322 | 0 |
Concentration | 1.5246 | 0.7623 | 0 |
pH | −0.5106 | −0.2553 | 0 |
Time | −0.0305 | −0.0153 | 0.461 |
Mass and Conc. interation | −0.7173 | −0.3591 | 0 |
Mass and pH interation | 0.0507 | 0.0253 | 0.236 |
Mass and time interation | 0.0253 | 0.0126 | 0.539 |
Conc. and pH interation | −0.2431 | −0.1216 | 0 |
Conc. and time interation | −0.0148 | −0.0074 | 0.716 |
pH and time interation | −0.0108 | −0.0054 | 0.791 |
Pseudo-First Order Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
K1 = 0.0264 min−1 | Regression | 9410.097 | 2 | 4705.048 | 738.72 | 1.24 | 0.96 |
Qef = 36.0295 mg/g | Residual | 63.690 | 10 | 6.36913 | |||
Total | 9473.788 | 12 | |||||
Pseudo-Second Order Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
K2 = 0.000729 g·min−1·min−1 | Regression | 9421.694 | 2 | 4710.847 | 904.31 | 1.96 | 0.97 |
Qef = 42.424 mg/g | Residual | 52.093 | 10 | 5.209 | |||
Total | 9473.788 | 12 | |||||
Elovich Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
α = 5.27131 mg/g·min | Regression | 9404.827 | 2 | 4702.414 | 681.9 | 1.51 | 0.95 |
β = 0.04598 g/mg | Residual | 68.960 | 10 | 6.89605 | |||
Total | 9473.788 | 12 |
Pseudo-First Order Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
K1 = 0.27775 min−1 | Regression | 16,561.380 | 2 | 8280.69 | 4933.21 | 0.41 | 0.985 |
Qef = 38.09673 mg/g | Residual | 18.464 | 11 | 1.67856 | |||
Total | 16,579.842 | 13 | |||||
Pseudo-Second Order Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
K2 = 0.01722 g·min−1·min−1 | Regression | 16,573.664 | 2 | 8286.83 | 14,753.23 | 0.28 | 0.995 |
Qef = 39. 06836 mg/g | Residual | 6.178 | 11 | 0.56 | |||
Total | 16,579.842 | 13 | |||||
Elovich Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
α = 5.107 mg/g·min | Regression | 16,556.29 | 2 | 8278.146 | 3866.58 | 1.84 | 0.981 |
β = 0.23802 g/mg | Residual | 23.55 | 11 | 2.14 | |||
Total | 16,579.84 | 13 |
Langmuir Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
KL = 0.00545 | Regression | 53,210.65 | 2 | 26,605.33 | 655.69 | 0.91 | 0.97795 |
Qmax = 179.87849 | Residual | 486.91 | 12 | 40.5761 | |||
Total | 53,697.57 | 14 | |||||
Freundlich Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
KF = 3.40006 | Regression | 52,332.94 | 2 | 26,166.47 | 230.096 | 1.07 | 0.93891 |
N = 1.63677 | Residual | 1364.63 | 12 | 113.72 | |||
Total | 53,697.57 | 14 | |||||
Temkin Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
αt = 0.08844 | Regression | 20,587.27 | 1 | 20,587.27 | 164.793 | 0.65 | 0.93212 |
βt = 0.03178 | Residual | 1499.134 | 12 | 124.927 | |||
Total | 22,086.41 | 13 |
Langmuir Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
KL = 0.00371 | Regression | 71,632.444 | 2 | 35,816.222 | 1373.097 | 0.49 | 0.99 |
Qmax = 253.34452 | Residual | 313.011 | 12 | 26.084 | |||
Total | 71,945.455 | 14 | |||||
Freundlich Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
KF = 2.78045 | Regression | 70,937.93 | 2 | 35,468.97 | 422.45 | 0.71 | 0.965 |
N = 1.47776 | Residual | 1007.52 | 12 | 83.96 | |||
Total | 71,945.455 | 14 | |||||
Temkin Model | |||||||
Parameters | Variation Source | SQ | DF | MS | Fcal | Error | R2 (adj) |
αt = 0.08236 | Regression | 28,839.644 | 1 | 28,839.644 | 119.194 | 0.65 | 0.908 |
βt = 0.02685 | Residual | 2903.45 | 12 | 241.95 | |||
Total | 31,743.095 | 13 |
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Sousa, M.U.; Rodrigues, A.M.; Araujo, M.E.B.; Menezes, R.R.; Neves, G.A.; Lira, H.L. Adsorption of Sodium Diclofenac in Functionalized Palygoskite Clays. Materials 2022, 15, 2708. https://doi.org/10.3390/ma15082708
Sousa MU, Rodrigues AM, Araujo MEB, Menezes RR, Neves GA, Lira HL. Adsorption of Sodium Diclofenac in Functionalized Palygoskite Clays. Materials. 2022; 15(8):2708. https://doi.org/10.3390/ma15082708
Chicago/Turabian StyleSousa, Matheus Urtiga, Alisson Mendes Rodrigues, Maria Eduarda Barbosa Araujo, Romualdo Rodrigues Menezes, Gelmires Araújo Neves, and Hélio Lucena Lira. 2022. "Adsorption of Sodium Diclofenac in Functionalized Palygoskite Clays" Materials 15, no. 8: 2708. https://doi.org/10.3390/ma15082708