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1. Thesis progress on; Conversion of water hyacinth’s stem in to graphene containing bio-char for Azo - dye removal in textile wastewater B y Mekete Yitayew Advisor : Zenamarkos B. ( Ph.D ) march . 2015 E.C

2. Outlines Introduction Statement of problem Literature Methodology Results and discussion 25 May 2017 BiT 2

3. introductiuon The water hyacinth is perennial, flowering plant that originat from tropical South America in 1824 ( Solms et al. , 2016 ). These plants can increase themselves two times their biomass in six days and occupies new areas very rapidly. The main property of this plant is after flowering, the inflorescence bends downward into the bottom of water and seeds can remain dormant for above twenty years before germinating until the correct conditions prevail ( Williams , 2017). 25 May 2017 BiT 3

4. … water hyacinth is considered as undesirable weed; but various studies have described its uses, such as in the manufacture of ethanol, as an adsorbent for heavy metals present in contaminated water, as a row resources for the production of biogas, as a biofuel, and as a protein complement in ruminant feed ( Solms et al. , 2016) Graphene containing bio-char will be made by the thermal disintegration of biomass over a wide-ranging of temperatures, from 300 to 1000 °C 25 May 2017 BiT 4

5. Cont.… Graphene is a flat single-layer carbon atom film strongly packed in a two-dimensional honeycomb lattice (Liu et al . , 2021). The large surface area (2630 m 2 g −1 ), excellent mechanical strength (Young's modulus: 1 TPa ; fracture strength: 130 GPa ), and superior thermal conductivity (5000 WmK −1 makes the graphene to have a good property ( Balandin et al. , 2008 ). 25 May 2017 BiT 5

6. Problem statement 25 May 2017 BiT 6 Water hyacinth is an aquatic weed that can propagates and breeding rapidly, and cover new area in fast rate .

7. Cont … 25 May 2017 BiT 7 On the other hand textile industries are the main contributor for water pollution by releasing of untreated dyes effluent

8. Cont … 25 May 2017 BiT 8 In similar way, the techniques for pollutants removal Membrane separation These equipments are not easily affordable in all areas of the environment and inevitable generation of untreated chemicals with no economical value Chemical precipitation Ion exchange chromatography

9. Cont … Based on these regard, It is possible to investigate to produce the effective, economically and environmental friendship graphene containing bio-char from water hyacinth’s stem for removal of Azo -dyes in waste water which were released from textile industry. Plus to this, it is also a viable option to control the weed in the invasion of on the aquatic surface in Lake Tana. 25 May 2017 BiT 9

10. General Objective The general objective of this research is to study the conversion and characterization of water hyacinth’s stem into graphene-containing bio-char for azo -dye removal applications from textile wastewater effluent. 25 May 2017 BiT 10

11. Specific objectives Characterization of water hyacinth’s stem Investigate the influences of temperature, and time on the pyrolysis of water hyacinth’s stem for graphene containing bio-char production Analyze the characteristics and properties of graphene containing bio-char produced from water hyacinth Investigate the effect of temperature, flow rate, and PH on the fixed bed adsorption of azo -dye by using graphene containing bio-char of water hyacinth’s stem Evaluate the adsorption capacity and dye removal efficiency of the graphene containing bio-char Evaluate the adsorption of isotherm, kinetics and thermodynamics 25 May 2017 BiT 11

12. Literature review Ecological characteristics of water hyacinth Water hyacinth grows in tropical and subtropical regions where the temperature and water content are high . It is a flowering plant and the seed can live in water for above twenty years in dormant condition until the correct condition is prevailing and this makes water hyacinth is difficult to control ( Solms , 2018). 25 May 2017 BiT 12

13. The physicochemical properties of water hyacinth Physicochemical properties are crucial parameters to know their features application during the thermal transformation process, either pyrolysis or combustion. The researchers discovered that WH has moisture, volatile matter, fixed carbon and ash content in below ( Huang et al. , 2018 ). 25 May 2017 BiT 13 Physical property % wt moisture 9.95 Volatile 56.3 Ash 17.4 Fixed carbon 16.35

14. Graphen based biochar Bio-char reveals high biodegradability, high contents of total and organic carbon, as well as optimal concentrations of micro- and macro element ( Ahmad et al. , 2012 ). Bio-char is an essentially a by-product formed when a huge quantity of organic matter (biomass) is heated at high temperatures in the absence or little quantity of oxygen ( Niinipuu et al. , 2020), (Sharma, Sarmah and Dubey , 2020 ). Process of bio-char manufacture had three stages: pre-pyrolysis; main-pyrolysis and formation of carbonaceous soil products ( Tomczyk , 2020) 25 May 2017 BiT 14

15. Cont … The first step (from ambient temperature to 200 o C ) is attributed to evaporation of moisture and light volatiles. The moisture evaporation causes breakage of bonds and formation hydro peroxide, –COOH and –CO groups. The second stage (from 200 to 500 o C ) was a devolatilized and decomposed of hemicelluloses and cellulose at a fast rate. The last stage (above 500 o C ) is degradation of lignin and other organic matter with stronger chemical bonds ( Tomczyk , 2020). 25 May 2017 BiT 15

16. Cont … Graphene, is hybridized carbon atoms and due its high surface area, excellent π-π interactions, large electron mobility, improved mechanical strength and more thermal conductivity, excellent sorption/absorption capacity toward various contaminants (e.g. dyes, oils, heavy metals) Makes it an excellent wastewater treatment media (Fang et al. , 2020 ). Graphene-containing bio-char showed excellent sorption capacity toward numerous pollutants such as organic pesticides, antibiotics and dye in water ( Fang, Gao , Bolan, Sabry M. Shaheen , et al. , 2020). 25 May 2017 BiT 16

17. Physicochemical properties of graphene containing bio-char Graphene containing bio-char has a good physicochemical properties which are the main parameters that determine its applications . Surface area, Pore size, and Functional group etc . Wastewater of textile industry One of the major contributors to water pollution is the release of untreated dye effluents from industry specially textile. These dyes are not only harmful to the plants and aquatic life, but also to human beings. 25 May 2017 BiT 17

18. Cont … Cancer, allergies, skin diseases are some of the health complications that may arise due to the ingestion and absorption of dye-contaminated water by humans ( Srivatsav et al. , 2020). 25 May 2017 BiT 18

19. Materials and methodology Material used 25 May 2017 BiT 19 S.no_ Material name Specification Function 1 Water hyacinth   Raw material 2 Sickle   Harvesting of water hyacinth 3 Muffle furnace   Ignition of water hyacinth   Oven dryer Model- DHG-9053A   4 x-ray diffractometer (XRD)   To determine elemental composition or surface or surface composition 5 Brunauer , Emmett and Teller (BET) NOVA 4000e To determine surface area, pore size and pore volume 6 Scanning electron microscopy (SEM)   To determine the surface morphological properties

20. Cont … 7 Fourier transforms infrared spectroscopy (FTIR   To determine the surface structure and functional group 8 Thermo-gravimetric analysis (TGA) Model- HCT-1 To determine the thermal stability properties and to know the burning temperature 9 UV-Vis spectrophotometer   To measure the concentrations of all adsorbates . 10 p H meter   To measure the pH 11 Beakers   Used as a reactor and measurement. 25 May 2017 BiT 20

21. Chemicals used S.no_ Chemicals Function 1 Distilled Water For washing of water hyacinth 2 Methylene blue (MB) Model compound for determining adsorption capacity of contaminants 3 HCl and NaOH For the adjustment of the initial pH of the solution 4 MgCl 2 , FeCl 3 , and Fe (NO 3 ) 3 For surface charge modification but FeCl 3 is better for good physicochemical properties formation 5 H 2 SO 4, H 2 PO 4, and NaCl Used to as modification and oxidizing agent 6 KMnO 4 Used as a strong oxidant agent to oxidize the bio-char to form graphene containing bio-char or graphene-like bio-char 7 H 2 O 2 Used to stop the further oxidation reaction 8 NaCl For PZC determination 25 May 2017 BiT 21

22. Methodology 25 May 2017 BiT 22 Flow diagram for the preparation of graphene containing bio-char Preparation of graphene containing bio-char from water hyacinth’s stem

23. cont … 25 May 2017 BiT 23 The image of for production process of graphene containing bio-char

24. Result and discussion Characterization of water hyacinth 25 May 2017 BiT 24

25. The physical properties of fresh water hyacinth Parameter Percent in weight (% wt ). Moisture content 89.47 Volatile matter 8.77 Fixed carbon 0.01 Ash 1.75 25 May 2017 BiT 25 The physical properties of water hyacinth

26. TGA analysis of water hyacinth for preliminary analysis 25 May 2017 BiT 26 .

27. The effect of temperature on Pyrolysis of water hyacinth’s stem for production of graphene containing bio-char at 25 May 2017 BiT 27 ( effect of temperature on the yield of bio-char)

28. The effect of time on Pyrolysis of water hyacinth’s stem for production of graphene containing bio-char 25 May 2017 BiT 28 The effect of time on the % yield of pyrolysis bio-char .

29. Cont … 25 May 2017 BiT 29 The normal plot

30. Cont … 25 May 2017 BiT 30 Residual vs predicted graph

31. Cont … 25 May 2017 BiT 31 Prediction value (% yield) with respect to time and temperature in contour plot

32. Cont … 25 May 2017 BiT 32 3D graph that was similar to the model graph

33. Proximate analysis graphene containing biochar 25 May 2017 BiT 33 Physical parameter % in weight Volatile matter 53.53 Ash content 10.1 Fixed carbon 36.37

34. Characterization of graphene containing bio-char by using BET 25 May 2017 BiT 34 . Graphene containing Bio-char Residence time (min) Pyrolysis temperature ( o c ) BET surface area (m 2 /g) Average Pore volume (cm 3 /g) Average pore diameter/size (nm) Water hyacinth 30 350 o c 549.5 0.054154 3.9407 Water hyacinth 40 450 o c 530.8 0.05537 3.7957 Water hyacinth 60 550 o c 556.1 0.055417 3.9227

35. The effect of temperature on surface area graphene containing biochar 25 May 2017 BiT 35

36. Continuous fixed bed adsorption of azo -dye by using graphene containing biochar . 25 May 2017 BiT 36

37. Set up of the fixed bed adsorption 25 May 2017 BiT 37

38. Determination of point of zero charge 25 May 2017 BiT 38 p H of PZC = 5.8

39. preparation of the standard calibration curve for determination the concentration the methylene blue dye 25 May 2017 BiT 39

40. The adsorption efficiency of graphene containing biochar for metylene blue dye Factor 1 Factor 2 Factor 3 Response 1 Std Run A:pH B:Temperature C:Flow rate Adsorption effeiciency AU Oc ml/min % 1 1 4 25 3 35.0557 16 2 7 30 4.5 99.5113 14 3 7 30 6 99.5435 19 4 7 30 4.5 99.5113 5 5 4 25 6 99.8081 18 6 7 30 4.5 99.5113 2 7 10 25 3 99.9145 10 8 10 30 4.5 99.7435 9 9 4 30 4.5 99.5855 20 10 7 30 4.5 99.5113 3 11 4 35 3 96.1274 15 12 7 30 4.5 99.5113 7 13 4 35 6 97.2177 17 14 7 30 4.5 99.5113 12 15 7 35 4.5 99.6242 13 16 7 30 3 99.7952 8 17 10 35 6 97.0952 11 18 7 25 4.5 98.921 6 19 10 25 6 97.9242 4 20 10 35 3 99.3629 25 May 2017 BiT 40

41. The colour of methylene blue after adsorption 25 May 2017 BiT 41 Before adsorption After adsorption

42. The effect of Ph , temperature and flow rate on continuous fixed bed adsorption 25 May 2017 BiT 42

43. Cont … 25 May 2017 BiT 43

44. The contour plot in fixed bed adsorption 25 May 2017 BiT 44

45. The 3D plot of fixed bed adsorption 25 May 2017 BiT 45

46. Optimization and limits of process parameter in continuous fixed bed adsorption The constraints and its response were described as Name Goal Lower Limit Upper Limit A:pH is in range 4 10 B:Temperature is in range 25 35 C:Flow rate is in range 3 6 Adsorption effeiciency maximize 35.0557 99.9145 25 May 2017 BiT 46

47. Cont … 25 May 2017 BiT 47

48. Cont … 25 May 2017 BiT 48 From this optimization, the maximum adsorption capacity was 99.9145 %. This was occurred at Ph =10, temperature = 25 oc and flow rate 3 ml/min.

49. Cont … From the optimization design solution when the Ph = 10, temperature =35 oc , and flow rate = 3 ml/min, the adsorption efficiency was become 111.385 % with the desirability 1. 25 May 2017 BiT 49

50. Future work Break through curve Adsorption kinetics Adsorption isotherm Thermodynamics feasibility of adsorbent 25 May 2017 BiT 50

51. Thank you 25 May 2017 BiT 51