SSCC 4493

1. SSCC 4493 GROUP ASSIGNMENT SAMPLE : KCC1 CATALYST: LECTURER : DR SITI AMINAH SETU

2. ABSTRACT Suitable instrument to identify the surface area of a sample is nitrogen physisorption analysis by using BET method which undergo process of adsorption-desorption of catalyst. High surface area silica catalyst has wide applications in almost every field.TheImportantly, the inherent properties of silica can be tuned by varying different parameters such as the size, shape, and morphology. The demand for silica nanosphereswith different sizes, dimensions and morphology is continuously growing because modern industries have spurred a tremendous interest for such materials.Theeffectiveness of these materials is mainly due to their micro and mesostructures which allow active molecules to disperse on the large internal surface and improving the activity. The accessibility of active sites inside the nano-silica particles is crucial as poor accessibility will limit their applications when significant mass transport is vital. Therefore, a high surface nano-silica with better accessibility was needed. In this study, the silica material sample called KCC1 was investigated. The surface area obtained is 531.14 .

3. Introduction of BET Brunauer-Emmett-Teller (BET) surface area analysis

4. Assumption

5. Sample preparation

6. BET Equipment Degassing Port Sample Holder Liquid Nitrogen

7. Pore Classification c = Macropore a = Microspore b a c 0.1 1 10 100 1 10 100 1000 b = Mesopore Pore Size

8. Introduction to KCC1 catalyst

9. Properties of KCC1 catalyst The morphology of Mesoporous Silica KCC-1 The FESEM and TEM image of the KCC-1 catalyst

10. BET METHODO L OGY

11. KCC1 Catalyst Methodology

12. GRAPH AND RESULT !!

13. ADSORPTION ISOTHERM

14. BET SURFACE AREA

15. CALCULATION BET constant, C C = = 91 slope = 0.0081 y-intercept = 0.00009 Monolayer volume,Vm : = = 122.01 BET Surface Area S= 4.35 × molar volume S = 4.35 × 122.01 S = 531.14

16. Langmuir Surface Area

17. CALCULATION slope = 0.0086 y-intercept = 0.00004 Monolayer volume, Vm: = 0.00004 Vm = 116.28 Langmuir Surface Area : S= 4.35 × molar volume S = 4.35 × 116.2791 S = 505.818 Langmuir constant K= = 215

18. t-PLOT

19. CALCULATION • Micropore pore volume • = i × 0.001547 = -4.2673 × 0.001547 • = - 0.0066 • = 0. 0000 • MicroporeSurface Area • = SBET- Sext = 531.14 - 5378.92 • = -4847.78 • = 0.000 • External surface area • = s × 15.47 = 347.7 × 15.47 • = 5378.92 • Micropore pore volume • = i × 0.001547 = -4.2673 × 0.001547 • = - 0.0066 • = 0. 0000

20. CALCULATION Total pore volume = 1.0263 mesoporevolume for KCC-1 = 1.0263 micropore volume for KCC-1 = 0.000 1) Percentage of mesoporosity : = 100 % 2) Percentage of microporosity = 0.00 % total pore volume = micropore volume + mesopore volume

21. RESULT K C C 1

22. RESULT

23. DISCUSSION FIGURE 1

24. DISCUSSION Figure 1 shows the nitrogen adsorption-desorption isotherms and the pore size distributions of silica KCC-1 based catalysts. The KCC-1 exhibited a type IV isotherm, with a H1-type of hysteresis loop which indicates that the presence of mesopores with highly uniform cylindrical structure and capillary condensation occur. BET has proved that KCC1 catalyst have higher surface area which is 531.14 and total pore volume of 1.0263 ml/g. At 0.4 pressure, the formation of a few multilayer formed at 0.9 of pressure indicates that all the pores was already filled.

25. DISCUSSION The Langmuir surface area for this KCC1 catalyst is 505.82 The Langmuir surface area depicts that the monolayer of the KCC1 catalyst have been filled. It can be said that the KCC1 have more pores since the monolayer surface area of the KCC1 catalyst is quite bigger. Based on the result, it can be claimed that the KCC1 catalyst is a mesoporous catalyst since it does not show any value of micropore volume.

26. DISCUSSION It is because presence of dendrimerfiber structure due to addition of more silica into the catalyst. Addition of more silica from tetraorthosilicate (TEOS) solution results in the properties of the KCC1 catalyst become a good basic catalyst. From the preparation of KCC1 catalyst, the cetyltrimethylammonium bromide (CTAB) acts as a cationic surfactantwhereas the urea act as hydrolyzing agent to allow the hydrolysis process occur.

27. CONCLUSION Nitrogen physisorption analysis is the most widely used technique to gather insight about textural properties by using Brunauer-Emmett-Teller (BET) method. The KCC1 catalyst which called silica based catalyst is one of the good catalysts that can allow society to use it for any reaction and application due to the dendrimer fibre and strong basic properties .

28. 5 APPLICATION OF KCC1

29. APPLICATION 1 1) Energy storage using DFNS-based supercapacitors

30. APPLICATION 2 2) Bioimaging using fluorescent DFNS coated with quantum dots STEM images and EDS elemental mapping of a) mSiO2@CdTe, b) mSiO2@CdTe@SiO2, and c) an ultramicrotomed mSiO2@CdTe@SiO2 slice

31. APPLICATION 3 TEM image of solid core-fibrous shell silica nanoparticles 3) High-performance liquid chromatography (HPLC) using DFNS-like silica

32. APPLICATION 4 4)Drug delivery using DFNS

33. APPLICATION 5 5) Extraction and detection of pollutants for environmental remedies

34. REFERENCES • Polshettiwar, V., Cha, D., Zhang, X., & Basset, J. M. (2010). High-surface-area silica nanospheres (KCC-1) with a fibrous morphology. AngewChemInt Ed Engl, 49(50), 9652-9656. • Fatah, N. A. A., Triwahyono, S., Jalil, A. A., Salamun, N., Mamat, C. R., & Majid, Z. A. (2017). n-Heptane isomerization over molybdenum supported on bicontinuous concentric lamellar silica KCC-1: Influence of phosphorus and optimization using response surface methodology (RSM). Chemical Engineering Journal, 314, 650-659. • Hamid, M. Y. S., Firmansyah, M. L., Triwahyono, S., Jalil, A. A., Mukti, R. R., Febriyanti, E., . . . Nabgan, W. (2017). Oxygen vacancy-rich mesoporous silica KCC-1 for CO 2 methanation. Applied Catalysis A: General, 532, 86-94.

35. REFERENCES 4) Polshettiwar, V., Thivolle-Cazat, J., Taoufik, M., Stoffelbach, F., Norsic, S., & Basset, J. M. (2011). "Hydro-metathesis" of olefins: a catalytic reaction using a bifunctional single-site tantalum hydride catalyst supported on fibrous silica (KCC-1) Nanospheres. AngewChemIntEdEngl, 50(12), 2747-2751. 5) Maity, A., & Polshettiwar, V. (2017). Dendritic Fibrous Nanosilica for Catalysis, Energy Harvesting, Carbon Dioxide Mitigation, Drug Delivery, and Sensing. ChemSusChem, 10(20), 3866-3913.