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1. Program of process engineering Intercalation of kaolin clay with chitosan as adsorbent for removal of lead from paint industry wastewater by using fixed bed adsorption . By: Abrham Gedamu Advisor: Zenamarkos Bantie ( PhD .) March,2023 Bahirdar , Ethiopia 25 May 2017 BiT 1

2. Outline Introduction Statement of the problem Objectives Materials and methods Results and discussion 25 May 2017 BiT 2

3. INTRODUCTION Heavy metals can be toxic, carcinogenic and are harmful to humans and other living species. The paint industry is one of the industry the causes of water pollution . contain variable amounts of heavy metals such as lead, cadmium , copper, and chromium. Lead are particularly common heavy metals found in paint industries wastewater . Lead ( Pb ) are hazardous and toxic nature; they commonly occur at high concentrations in contaminated waters. Lead permissible limit of <0.05 mg/L lead in drinking water. 25 May 2017 BiT 3

4. Cont’d Among several methods, adsorption has attached more attention to heavy metals removal. Kaolin (china clay) is a rock material that is rich in kaolinite. It has a two layer: Tetrahedral sheet of silica (SiO 2 ) & Octahedral sheet of alumina (Al 2 O 3 ) Kaolin can adsorb heavy metals with formation of inner-sphere complexes through Si–O and Al–O groups at the clay particle edges. 25 May 2017 BiT 4

5. Cont’d 25 May 2017 BiT 5 The basal oxygen atoms of the siloxane sheet and the opposing surface hydroxyls of the alumina sheet generate hydrogen bonds. Modification of clay through acid treatment, calcinations, and intercalation to enhance its usability beyond its application in natural form. Integration of an adsorbent with other materials has better adsorption properties than the individual components effects.

6. Cont’d Chitosan is a chitin derivative and also it is naturally found in the cell wall . It can be extracted from mushroom and crustacean shells. Chitosan is synthesized from the deacetylation of chitin . It contain two chemically reactive groups Hydroxyl groups & Highly reactive amino groups Chitosan has some mechanical and chemical deficiency challenges which when improved upon, increases its adsorption capability. 25 May 2017 BiT 6

7. Cont’d Intercalation is the insertion of a guest species in the interlayer region of a clay mineral. 25 May 2017 BiT 7

8. Statement of the Problem Lead metal from the paint industry are adsorbed by kaolin clay intercalated with chitosan ( KIC ) adsorbent. 25 May 2017 BiT 8

9. General objective The general objective of this study is to synthesize kaolin-chitosan nanocomposite adsorbent by intercalation of kaolin clay with chitosan for the removal of lead from the Paint industry wastewater by using fixed bed adsorption. 25 May 2017 BiT 9

10. Specific objectives To purify kaolin clay by chemical beneficiation methods and extract chitosan from mushrooms using a chemical method. To synthesize and characterize intercalated kaolin clay with chitosan adsorbent. To design column adsorption and investigate synthesized intercalated kaolin clay with chitosan adsorbent for adsorption of lead from Paint industry wastewater. To analyze and optimize the effect of selected process variables (pH, flow rate, and initial feed concentration) on the adsorption capacity . 25 May 2017 BiT 10

11. MATERIALS AND METHODS Chemicals 25 May 2017 BiT 11 Row materials & Chemicals Chemical formula Function Kaolin   Main row material Chitosan   Main row material Oxalic acid (COOH)­ 2 .H 2 O Best iron leaching reagent because of its acid strength sodium hydroxide NaOH Chitin deproteinization . Sodium chloride NaCl Determination of point zero charge Hydrochloric acid HCl PH adjustment Acetic acid CH 3 COOH Dissolving chitosan Lead nitrate Pb (NO 3 )2 Make standard solution Nitric acid HNO 3 Clean wastewater sample bottle Distilled water   Wash and use as a dispersant for kaolin preparation.

12. Cont’d Equipment’s 25 May 2017 BiT 12 Equipment Function Analytical balance weighing of raw materials and chemicals Sieve Determine the particle size of row kaolin powder Cutter mill Grinding mushroom sample Disk mill Crushing kaolinite clay Oven Dry samples at a temperature PH Meter Measure different solution of pH Hot plate with magnetic stirrer Heat source & mix a solution. Muffle furnace Calcination of the raw kaolin Vacuum filtration Used for separating a solid-liquid mixture. Ultrasonic bath Create proper homogenous solution UV/VIS Spector photometer Analyze metal and nonmetals in a solution BrunauerEmmett-Teller(BET) Analyze surface area and pore size TGA Determine weight loss as a function of temperature FTIR Determine the functional group of the adsorbent XRD Characterize crystalline or amorphous phase nature of adsorbent SEM Surface morphological view of the kaolin & KIC adsorbent

13. Beneficiation and purification of kaolin 25 May 2017 BiT 13 Calcined kaolin Fe 2 o 3 Acid-treated Soaked Size reduction Supernatant

14. Extraction of Chitosan from Mushrooms 25 May 2017 BiT 14 Chitosan Chitin Deproteinization Protein Draying Mushroom Washing Deacetylation Acetyl

15. KIC synthesize flow diagram 25 May 2017 BiT 15

16. Cont’d 25 May 2017 BiT 16 Figure row kaolin, calcined kaolin, chitosan, and intercalation of kaolin with chitosan adsorbent

17. Column adsorption experiments 25 May 2017 BiT 17 The fixed-bed columns design consisted of: a tube with 1.5 cm internal diameter and 25 cm length

18. Experimental design Factor 1 Factor 2 Factor 3 Response 1 Std Run A:Intial pH B:Flow rate C:Initial feed concentration Removal efficiency mL/min mg/L % 11 1 6 3 1200 4 2 9 5 900 15 3 6 4 1200 20 4 6 4 1200 19 5 6 4 1200 5 6 3 3 1500 17 7 6 4 1200 12 8 6 5 1200 10 9 9 4 1200 7 10 3 5 1500 3 11 3 5 900 6 12 9 3 1500 13 13 6 4 900 9 14 3 4 1200 14 15 6 4 1500 1 16 3 3 900 8 17 9 5 1500 18 18 6 4 1200 2 19 9 3 900 16 20 6 4 1200 25 May 2017 BiT 18

19. Results and discussion Characterization of chitosan 1. Solubility test in acid solution The results acid solubility of chitosan are triplicate determination 83.77±0.067 . Chitosan's solubility in acetic acid was a sign of its purity . 2. Degree of Deacetylation The value of the chitosan made from mushroom was found to be 84% deacetylated . The greater elimination of inorganic components is shown by the chitosan's higher degree of deacetylation value. 25 May 2017 BiT 19

20. Characterization of Adsorbent 1. Moisture content The produced results with a moisture content of 1.0722 ± 0.1154 kaolin intercalation of chitosan adsorbent . 2. Bulk Density The calculation produced a bulk density of 1.57 g/cm 3 for the kaolin intercalated with chitosan adsorbent . 3.Determination of point zero charge The pHpzc means that the net charge on the adsorbent surface is zero. The pHpzc of calcined kaolin particles is found to be 3.74 ± 0.045. 25 May 2017 BiT 20

21. Cont’d The pHpzc of kaolin intercalation with chitosan particles is found to be 6.476 ± 0.05. The above diagram is PZC determination for calcined kaolin and kaolin intercalation with chitosan adsorbent respectively. 25 May 2017 BiT 21

22. Cont’d 25 May 2017 BiT 22 4.Thermo Gravimetric Analysis Figure , TGA graph of KIC adsorbent

23. Cont’d 5. Fourier Transforms Infrared Spectroscopy 25 May 2017 BiT 23 Wave number (cm -1 ) Bond Functional group Calcined kaolin chitosan KIC     3610 3320 3370 O-H stretching, hydrogen-bonded alcohols 1634 1628 1640 O-H deformation alcohols   3327 3314 N–H stretch primary, secondary amines,amides     1722   C=O stretch carboxylic acids     2841 2923 C-H stretch Alkanes   1363   C-H deformation       1618 Alkyl amine groups amine     1275 Si-OH       1035 C-OH alcohol groups 1028   1022 Si-O stretch   1085   1091 Al-O stretch     1230   C-O stretch alcohols, carboxylic acids   738   NH-out of plane bending amine 573   624 Al-O-Si deformation   536   554 Si-O-Si deformation  

24. Cont’d 25 May 2017 BiT 24 The most intense peak is seen at 27.51º. The average d-spacing KIC adsorbent was 2.734Å. The average crystallite size was 2.01 nm. The crystallinity index (CI) of KIC adsorbent is 82.187%. 6. X-ray diffraction

25. Cont’d 25 May 2017 BiT 25 7. Scanning Electron Microscopy Figure, SEM image of the calcined kaolin and KIC adsorbent Mean length of calcined kaolin & KIC 27.194 & 121.9 nm .

26. Physicochemical characteristics of kokeb paint industry waste water 25 May 2017 BiT 26 Using a calibration curve, it is possible to estimate the total lead metal concentration. The overall lead concentration in the wastewater from the paint industry is 6.215 mg/L.

27. Cont’d 25 May 2017 BiT 27 Physicochemical characteristics of kokeb paint industry waste water

28. ANOVA of KIC Source Sum of Squares df Mean Square F-value p-value Model 237.81 9 26.42 6.47 0.0037 significant A-Initial pH 28.56 1 28.56 7.00 0.0245 significant B-Flow rate 47.30 1 47.30 11.59 0.0067 significant C-Initial feed concentration 84.61 1 84.61 20.73 0.0011 significant AB 0.2018 1 0.2018 0.0494 0.8285 Non significant AC 0.8501 1 0.8501 0.2083 0.6579 Non significant BC 20.39 1 20.39 5.00 0.0494 significant A² 31.12 1 31.12 7.62 0.0201 significant B² 5.07 1 5.07 1.24 0.2911 Non significant C² 11.91 1 11.91 2.92 0.1184 Non significant Residual 40.81 10 4.08 Lack of Fit 40.81 5 8.16 Pure Error 0.0000 5 0.0000 Cor Total 278.62 19 25 May 2017 BiT 28

29. Checking of data and adequacy of the model 25 May 2017 BiT 29 Std. Dev. 2.02 R² 0.8535 Mean 80.22 Adjusted R² 0.7217 C.V. % 2.52 Predicted R² 0.0051 Adeq Precision 9.4837

30. Predicated Vs Actual Graph 25 May 2017 BiT 30

31. Perturbation model graph of three factors 25 May 2017 BiT 31

32. Interaction effect of flow rate with initial concentration 25 May 2017 BiT 32

33. 3D Surface graph of flow rate with initial concentration 25 May 2017 BiT 33

34. O ptimization of removal efficiency of lead 25 May 2017 BiT 34 Goal Lower Limit Upper Limit Initial pH is in range 3 9 Flow rate is in range 3 5 Initial feed concentration is In range 900 1500 Removal efficiency maximize 73.5607 87.3621 Number Initial pH Flow rate Initial concentration Removal efficiency Desirability 1 7.028 3.221 922.214 88.073 1.000 Selected

35. Feature works 25 May 2017 BiT 35

36. Thank you for attractive attention 25 May 2017 BiT 36