Hydrothermal Synthesis of Nano Crystals (A.M.) Zeolite using Variable Temperature Programs

June 22, 2017 | Autor: A. M.Mahmoud | Categoria: Nanoscience
Share Embed


Descrição do Produto

Hassan and Mahmoud, J Nanomater Mol Nanotechnol 2015, 4:4 http://dx.doi.org/10.4172/2324-8777.1000169

Journal of Nanomaterials & Molecular Nanotechnology

Research Article

Hydrothermal Synthesis of Nano Crystals (A.M.) Zeolite using Variable Temperature Programs Hassan AZA1 and Abdel Wahab M Mahmoud2*

Abstract Objective: The synthesis and characterization of (A.M. zeolite) was designed for the unique cation exchange, adsorption, hydrationdehydration, catalytic properties, soil remediation, could be load with macro& micronutrients, and become slow-release fertilizer. Methods: The zeolite was hydro thermally synthesized by varying the concentrations of Si and Al at different crystallization temperature. Different visual instrumental techniques were used to characterize the product of nano (A.M. zeolite) which obtained at different synthesis parameters using X. ray diffraction, FTIR (fourier transform infrared spectroscopy), TEM (transmission electronic microscope), SEM (scan electronic microscope), TGA (thermogravimetric analysis) and TDA (differential thermal analysis), CEC (cation exchange capacity) and AEC (anion exchangeable capacity). Results: The temperature was found to be a crucial factor for the control of the crystal size. Broad and sharp peaks obtained in diffractogram shows the amorphous and crystalline nature of the materials respectively. We found that, the composition of (A.M zeolite) was approximately close to the concentrations of the precursors taken during synthesis. The FTIR spectra of these A.M. zeolites in framework vibration region also shows sharp feature for A.M zeolite. High crystalline nature of the material is reveals by absorption bands. On the other hand, BET illustrate that AM zeolite had a high value of surface area at 1000ºC and nano pore size distribution. CEC recorded high value, while AEC gave lowest value. EDX results showed that, Si/Al ratio for AM Nano zeolite tends to be hydrophilic. Conclusion: We can conclude that, synthesized A.M. nano zeolite can potentially be used in industries, conventional agriculture, horticulture, environmental protection, safety agriculture, biomedicine proposes and water retention and purity specially in arid zones. Keywords A.M. zeolites; Catalytic properties; Hydrothermal synthesis

*Corresponding authors: Abdel Wahab M Mahmoud, Cairo University, Faculty of Agriculture, Plant Physiology Department, Giza, Egypt, E-mail: mohamed. [email protected] Received: July 14, 2015 Accepted: September 01, 2015 Published: September 08, 2015

International Publisher of Science, Technology and Medicine

a SciTechnol journal

Introduction Nanotechnology is the engineering and art of manipulating matter at the nano scale (1-100 nm). The existence of nano sized particles at the workplace is not a new phenomenon as early as in 1997, the Deutsche Forschungsgemeinschaft, Commission for the Investigation of Health Hazards of chemical compounds in the work area, defined the term “ultrafine particles” in its List of Maximale ArbeitsplatzKonzentration (MAK) and Biologischer Arbeitsstoff-Toleranzwert (BAT) values. The definition of “ultrafine particles” relates to the workplace corresponds primarily to the term nanoparticles is currently being used in research and technology. Nano sized particles differ from coarser particles by their increasing tendency to form agglomerates, such agglomerates are macroscopically perceived as one particle and may break down into their primary particles in biological material [1]. In the fact Nano particles are formed by two different processes called the top-down and the bottom-up. The difference between the two processes is that, the top-down method generally leads to crystalline samples, from a previously “thermodynamically” formed product usually complies with the ideal crystal structure (ideal structure) [2,3]. While the bottom-up procedure results in the formation of small particles from crystalline areas that do not correspond to the ideal lattice (defect structure). These previous structures, which are difficult to describe, are not have enough time for an ideal or real crystal growth [4], Such defect or real structures are classified according to different defect classes: 0-dimensional defects (non-stoichiometry), 1-dimensional defects (dislocations), 2-dimensional defects (grain boundaries) and 3-dimensional defects (pores) [5]. Therefore our main target from present research is to design nano zeolite clinoptilolite (A.M.) with 3-dimensional defects (pores) as real crystal growth in short time and high purity, this synthesized nano zeolite clinoptilolite (A.M.) could be use as soil remediation, biomedicine, catalysis, water retention and purity specially in arid zones, possibility for loading of micro and macro elements(slow release fertilizers) which has an important effect in reducing environmental pollution rates and economical values compare with commercial fertilizers.

Material and Methods Nano Zeolite clinoptilolite named (A&M) has been synthesized by hydrothermal method. The reaction mixture is (TEOS) as tetrahedral molecule, many analogues exit, and most are prepared by alcoholysis of silicon tetrachloride, and used as the silica source for synthesis of zeolites. Aluminum nitrate (Al{NO3}3) and Potasium nitrate (KNO3) are used as starting materials for the synthesis of zeolites. The sodium hydroxide (NaOH) solution is used as template and alkali source. The reaction mixture was performed according to the following gel composition of 10 (KNO3): 1.0 Al2O3 15 SiO2: 300 H2O (molar ratio). A.& M. zeolite had been synthesized by hydrothermal treatment at various crystallization temperatures. The crystallization of A.M. zeolites controlled by a two stages variable-temperature program. The reaction mixture was transferred to a Teflon lined stainless steel pressure vessel and placed in preheated (75ºC, 100ºC, 125ºC and 150ºC) oven at autogeneous pressure(2 PSI) and static conditions for

All articles published in Journal of Nanomaterials & Molecular Nanotechnology are the property of SciTechnol, and is protected by copyright laws. Copyright © 2015, SciTechnol, All Rights Reserved.

Citation: Hassan AZA, Mahmoud AWM (2015)Hydrothermal Synthesis of Nano Crystals (A.M.) Zeolite using Variable Temperature Programs. J Nanomater Mol Nanotechnol 4:4.

doi:http://dx.doi.org/10.4172/2324-8777.1000169 72hrs and then transferred into an autoclave, where the hydrothermal crystallization was carried out at 313 for 24h, subsequently at 333 Cº for 48 hrs., respectively. After completion of crystallization, the solid products were washed several times with distilled water until PH=78, then calcined at 1000ºC overnight. The materials thus synthesized were thoroughly characterized by instrumental techniques viz . X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), model JSM.6390 LA (JEOL) analytical scanning electron microscope at Holding Company For Drinking Water and Waste Water, Greater Cairo Company For Drinking Water, Central Laboratory. The work was done in TEM lab (FA-CURP) Faculty of Agriculture Cairo University Research Park as follow:

Specimen Preparation: Acceptable specimens: Sonicate the dilution 5 min. Place two 2-5 µl drops of specimen onto sheet of Parafilm Make EM grids carbon-coated (400-mesh copper grids) directly off on specimen Use filter paper to wick away specimen drop and place grids, specimen-side up in specimen petri dish. Examined by transmission electron microscope JEOL (JEM1400 TEM) at the candidate magnification. Images were captured by CCD camera model AMT, optronics camera with 1632 x 1632 pixel formate as side mount configuration. This camera uses a 1394 fire wire boared for acquision. Thermo gravimetric analysis (TGA) by using TGA/DC2Thermogravimetric analyzer, broad temperature scale – analyze samples from ambient to 1000ºC. Differential thermal analysis (DTA), Energy Dispersive X-ray (EDX) using High Sensitivity Energy Dispersive X-ray Fluorescence Spectrometer - Shimadzu EDX-7000/8000. The pH titration method was used to determine the cation and anion exchange capacity of the natural and synthetic zeolites. The test work involved measurement of total cation and total anion exchange capacities.

Porosimetry of the synthesizedl A.M. nano Zeolite The A.M. nano zeolite clinoptilolite volume, pore size distribution and specific surface area BET determination by uing Nova 2000 series (America) Quantahrome at Central metallurgical research and development institute. For the adsorption-desorption curves the adsorbate was N2 and pore size distribution was calculated from the desorption branch using the BET model.

calculated using Eq.( 1). Moisture W (%)=(m2-m3)/ (m2-m1)*100 (1) Where; m1 - weight of pill vial with lid, m2 - weight of closed pill vial with (1-2 g) synthesize A .M .zeolite m3 – weight closed pill vial with dried synthesize A .M zeolite sample. For the total cation exchange capacity (CEC) test, 5 g of pulverized sample of synthesized A.M. zeolite was mixed with 500 ml of 0.1M H Cl for 24 hours in a rolling bottle. Solids were separated from solution by filtration. A 10 ml filtrate was titrated with 0.1 M NaOH solution to determine the H Cl concentration after adsorption. Three drops of a mixed indicator were added to the 10 ml filtrate solution and the solution turned from colourless to purple. Upon titrating with Na OH the solution turned green. Equations (1), (2) and (3) were used to calculate the CEC. C2 HCL= C NaOH x V NaOH / V s (2) Q (total cat., meg/g )= C1 HCl –C2 HCl )(V)(100-W)/100/m (3) Where: C1 HCl - initial concentration of HCl (0.1 M); C2 HCl - concentration of HCl after cation exchange (M); C NaOH - concentration of NaOH (0.1 M); V NaOH - volume of NaOH required for titration of the sample of filtrate (ml); V s - volume of filtrate for titration (10 ml); V – volume of HCl solution (500ml); m – mass of zeolite (5g) . W- was defined by eq. (1) The determination of the anion exchange capacity (AEC) involved thoroughly mixing 5 g of a pulverized sample of zeolite with 500 ml of 0.1 M NaOH for 24 hours in rolling bottle. 10 ml of filtrate was titrated with 0.1 M HCl solution to determine the HCl concentration after adsorption. Phenolphthalein was used as an indicator. About 3 drops were added to the 10 ml solution, which remained colourless until the addition of HCl. The end point was reached when the solution turned pink. Equations (1), (4) and (5) were used to determine the AEC. C2NaOH=C HCl x V HCl / Vs (4) m Q (total an., meg / g) = C1 NaOH – C2 NaOH (V)(100- W) 100 /m (5)

Ion exchange capacity analysis

Where: C1NaOH - initial concentration of NaOH (0.1 M);

The pH titration method was used to determine the cation and anion exchange

C2 NaOH - concentration of NaOH after anion exchange (M);

Capacity of the natural and synthetic zeolites clinoptilolite. The test work involved measurement of the moisture content,total cation and total anion exchange capacities. For moisture content determination a pill vial was weighed with a lid closed, then an amount of zeolite (1-2 g) was placed inside and weighed again. The pill vial with the sample was placed open into the oven for 24 hours at 600ºC. Upon the removal of the pill vial from the oven, the pill vial was weighted with a closed lid and a dried sample. The moisture content of each sample was Volume 4 • Issue 4 • 1000169

C HCl - concentration of HCl (0.1M); V HCl - volume of HCl required for titration of the sample of filtrate (ml), V s - volume of the sample titrated (10 ml); V - Volume of NaOH solution (500ml); m – Mass of zeolite (5g). W- was defined by eq. (1) • Page 2 of 6 •

Citation: Hassan AZA, Mahmoud AWM (2015)Hydrothermal Synthesis of Nano Crystals (A.M.) Zeolite using Variable Temperature Programs. J Nanomater Mol Nanotechnol 4:4.

doi:http://dx.doi.org/10.4172/2324-8777.1000169

Results and Discussion X-Ray Diffraction (XRD) The sample synthesized at temperatures lower than 125°C indicated that, the amorphous phase material as shown in XRD patterns Figure 1 (a-d). The material synthesized at 150ºC shows the most prominent reflection peak at 26ө indicating highly crystalline nature of the material Figure 1(d). At lower synthesis temperatures 75°C, 100°C and 125°C Figure 1 (a- c) the materials exhibited the surface area typical to the amorphous materials. Crystals obtained at 150°C and above have much higher surface area. It has to be pointed out that the resolution of XRD patterns improves as the Si/Al ratio increases. This is due to Al incorporation in the framework which reduces the degree of order [6].

FTIR study of synthesized A.M. nano zeolites It can be concluded that, the FT-IR peaks of nano A.M zeolite (150°C) which presented in Figure 2 are found to exhibit typical infrared spectroscopic patterns which exist in two ranges. The first is due to internal vibration which found in range 950-125° cm-1 and second found in range 420-500 cm-1 of primary unit of structure (tetrahedron), that is not sensitive to other structural vibration, these previous strongest vibrations are assigned to T-O stretching and T-O

bending mode (T=Si or Al) respectively. The stretching modes are sensitive to the Si-Al composition of the framework and may shift to a lower frequency [7]. While the bending mode may be related to the linkages between tetrahedral. The vibration which are sensitive to the overall structure and the joining of the individual tetrahedral in secondary structural unit as well as their existence in the large pore openings are of second types of vibration as shown in Figure 2. The bimodal absorbance in spectra is indicated by the hydroxyl bond (-OH stretch) near 3550 cm-1. The band at 3445.71 cm-1 indicates the loosely bound water molecules. while a strong characteristic structure sensitive bands due to the presence of attached water molecule indicates a water (H 2O) bending vibration at 1650.30 cm-1. Thereby sorption and desorption of water (hydration and dehydration) may be easily monitored by FTIR [8,9,10]. Going with the band at 550-580 cm-1 can be associated with ring of tetrahedral and /or octahedral [11]. Focuses on absorption bands at 520-570 cm-1 indicate the high crystalline nature of nano A.M zeolite. These bands indicate pronounced crystallization and thus confirmed the XRD investigations as described earlier [7]. The assigned peak which observed around 730 cm-1 is distinctive peak of stretching frequencies of six-coordinated aluminum and four member ring deformation mode of the network along with other modes [12,13]. Whereas the peaks below 550 cm-1 are generally due to (O-T-O) bending and rotation mode. As for peaks between 700-850 cm-1 and 1000 to 1150 cm-1 are assigned to symmetric and anti symmetric T-O-T stretching vibration.

DTA/TGA study of synthesized A.M. nano zeolites

Figure 1 (a, b, c, d): XRD of synthesized AM Nano zeolite as affected by different crystallization hydrothermal systems.

The number of water molecules attached with the hydrothermally synthesized of nano A.M. zeolite and its thermal stability was investigated using DTA/TGA. Upon heating the sample from room temperature to 500°C a continuous weight loss of 8.12% and 17.3% is clearly observed. This weight loss is may be due to dehydration of physically adsorbed water. When the sample is further heated in the temperature range of 200 to 500°C the weight loss observed is attributed to desorption of remaining water enclosed in the material matrix. Reduced weight loss in this region was observed with increase in crystallization temperature (when calcined appeared at 1000°C) as well as Si/Al ratio of the sample which is consistent with the fact that A.M. nano zeolite becomes more hydrophobic as the Al content decreases [6].

SEM &TEM study of synthesized A.M. nano zeolite materials TEM have the ability to resolve and show individual particles clearly in an aggregation of particles mass. TEM observation shows that the nano size crystals can be obtained from hydrothermal synthesis method. The very small size of synthesized material can accurately be determined by TEM rather than SEM (Figure 3 (a-d)). From Figure 4, we can concluded that A.M. nano zeolite components arranged in descending order of their atoms capacities, are Oxygen, silica, Alumina, carbon, sodium and potassium. The images of specimen atoms mapping of nano zeolite after calcinations process enhanced that the silica was the majority component of nano zeolite while Allumina is the second component. Figure 2: FT-IR Spectrograph of A.M. Nano Zeolite at crystallization hydrothermal at 150°C.

Volume 4 • Issue 4 • 1000169

SEM & TEM images of nano A.M. zeolite shows nano particles of size (19.2-24.6) nm (Figure 5). • Page 3 of 6 •

Citation: Hassan AZA, Mahmoud AWM (2015)Hydrothermal Synthesis of Nano Crystals (A.M.) Zeolite using Variable Temperature Programs. J Nanomater Mol Nanotechnol 4:4.

doi:http://dx.doi.org/10.4172/2324-8777.1000169

Figure 3: SEM image of as-synthesized A.M Nano Zeolite by different hydrothermal stages.

Moreover [15] reported that the specific surface area of the calcined product of phosphate rock decreased with increasing calcination temperature [14]. They carried out their tests on two different phosphate samples from Morocco and Utah. There was a sharp decrease in specific surface area with increasing temperature in both samples between 500ºC and 800ºC, with the Morocco sample more pronounced in the density decrease. They attributed this remarkable change in surface area to the aggregation of elementary fine grains in this temperature range suggesting that consolidation of these very small grains occurs at these temperatures. It may also be possible that the destruction of the pore structure of the rock in this temperature range contributes to the drastic decrease in specific surface area of the sample as will be discussed later. According to literature, common industrial adsorbents like activated carbon have surface areas in the range of 500-2000 m2/g, with polymeric adsorbents having 150-1000 m2/g. For the natural zeolites analyzed the surface areas were found to be in the range of 33.4-65.5 m2/g. These surface areas are generally lower than those of adsorbents currently used in the catalysis industry. This could imply that the use of natural zeolites in such applications may not be ideal, but in agricultural purposes we can used A.M. nano zeolite as soil amendment, adsorption heavy metals loading macro-micro nutrients, slow release fertilizers. EDX: The average elemental composition of the synthesized A.M. nano zeolite sample is presented in Table 1 and Figure 7. From the real elemental composition of A.M. nano zeolite were

Figure 4: Specimen atoms mapping of Nano Zeolite A.M.

Figure 6: Surface area of A.M Nano Zeolite. Figure 5: TEM image of as-synthesized A.M Nano Zeolite after calcined at 1000°C.

BET (surface area) The results and Figure 6 explained that A.M. nano zeolite has 68.71 m2/g, this value is agreement with the fact that, the areas where nano-scale high surface area materials may have the greatest future impact are difficult to predict, but some signs point to the possibility of substantial advancement in the areas of adsorption/separations, particularly in gas sorption, separations and in novel chemical catalysis as well using Nano scale catalyst particles. Volume 4 • Issue 4 • 1000169

Table 1: Average elemental composition of the synthesized nano A.M. zeolite sample. Element, at. % (mass) Si/Al ratio at Element, at. % (atom) Atomic A.M.nanoZeolite % (mass) A.M.nanoZeolite ratio(Si/Al) Si Al K Na O C Yield (g)

24.81 5.40 13.12 12.08 39.31 5.28 –

4.59

19.46 4.41 6.71 5.52 54.10 9.80 Yield (g) –

4.41

• Page 4 of 6 •

Citation: Hassan AZA, Mahmoud AWM (2015)Hydrothermal Synthesis of Nano Crystals (A.M.) Zeolite using Variable Temperature Programs. J Nanomater Mol Nanotechnol 4:4.

doi:http://dx.doi.org/10.4172/2324-8777.1000169 A.M. nano zeolite sample investigated in the study. A typical plot of the relationship between pore size and pore volume for A.M. nano zeolite is depicted in Figure 8.

Figure 7: Elements dispersive X-ray pattern (EDX) of A.M Zeolite. Samples

Total cation exchange meq/g) Total anion exchange (meq/g)

A.M.nano zelite

4.5

0.2

Table 2: Ion exchange capacity analysis results.

observed for the elements O,K, Na, Si and Al. In A.M nano zeolite, Si content was a higher (24.81%) than theoretical, which may result in a high increase in C.E.C (cations exchange capacity). The calculated value of chemical formula of nano A.M. zeolite is equal to 4.41, which given as atomic ratio of Si to Al approximately. EDX was used to distinguish whether the nano A.M. zeolite is hydrophobic or hydrophilic. The EDX analysis results of the A.M. nano zeolite presented in Table 1 and Figure 7. The results showed a high composition of silicon in A.M nano zeolite. Potassium (K) and Sodium (Na) were the major single extra-framework cations in synthesized A.M. nano zeolite. According to the International Mineralogical Association, Commission on New Minerals and Mineral Names’s (IMACONMMN) third rule [15], who enhance that only heulandite and clinoptilolite zeolites can solely be distinguished on the basis of the silica and aluminium framework . Heulandite has a Si/Al ratio of less than 4, whilst clinoptilolite has a Si/Al of equal or more than 4. The Si/Al ratio of the synthesized A.M. nano zeolite was found to be 4.59, as shown in Table 2. All natural zeolites have a Si/Al ratio of more than 4, thus making them clinoptilolite type. The advantage of high Si/Al ratios is that in low pH environments, the structure is less likely to be damaged. The most abundant single extra-framework cation in A.M. nano zeolite was found to be potassium (K), making the synthesized zeolite type rich with K. Zeolites of low Si/Al ratio (less than 4), meaning with high aluminium atoms content, tend to be hydrophilic and organophillic, while a high silica zeolite will tend to be hydrophobic. The EDX results of A.M. nano zeolite showed that the Si/Al ratio was above 4, about(4.59%) resulting the A.M. nano zeolite approached to be hydrophilic synthesized materials.

Generally fall within a diameter of (2-5) nm for A.M .nano zeolite. There are significant implications to be derived from the results of pore size and surface area measurement: according to literature, common industrial adsorbents like activated carbon have surface areas in the range of 500 – 2000 m2/g, with polymeric adsorbents having 150-1000 m2/g. For the natural zeolites analysed the surface areas were found to be in the range of 33.4-65.5 m2/g. These surface areas are generally lower than those of adsorbents currently used in the catalysis industry. This could imply that the use of A.M. nano zeolite in such applications may not be ideal. According to literature clinoptilolite zeolites with a pore size range of 2 nm-10 nm can be used for biomedicine purposes. Since the pore sizes of all natural zeolites are in the range of 2-10 nm, these zeolites can be candidates for use in biomedicine. This however, needs to be investigated further, particularly the effect of various impurities on the biocompatibility of the synthesize zeolites. This result are agreement with previous studies which included that The porosity of the phosphate rock sometimes increases with increasing temperature up to about 700ºC and then decreases from this level on as in the case of the Utah phosphate rock [14]. In some other phosphates, such as the Morocco phosphate, the porosity gradually decreased with increasing temperature and then suddenly fell to minimum at about 700ºC. The porosity trends suggest the destruction of the pore systems in both samples for both the macro pores and Micro pores, but particularly the fine pores. For the Morocco sample the destruction of pores was quite severe which may be reflected on the reactivity of the calcined product. It is worthy to mention that in the case of the Utah sample, the gradual increase of porosity in the lower range of temperature (below 500ºC) may be explained on the basis of volatilization of organic matter [14].

Study on the ion exchange capacity The results of the determined total cation and anion exchange capacities are summarised in Table 2. The natural zeolites analyzed have a low but acceptable cation exchange capacity compared to the theoretical capacity of clinoptilolite (according to literature CEC is 2.16 meq/g) [16]. The synthetic A.M. nanozeolite had the highest cation exchange capacity of (4.5 meq/g). The anion exchange capacity of the A.M. nano zeolite

Porosimetric study of the A.M. nano zeolite adsorption / desorption Isothermal curves were used to determine zeolite pore morphology. The different zeolite material’s specific surface area were measured using the Brunauer-Emmett-Teller (BET) equation isotherm. The pore size distribution (PSD) was estimated using Barret-Joyner- Halenda (BJH) model. The adsorption/ desorption isotherms of the A.M. nano zeolite was obtained. It shows that the desorption and adsorption branches meet to form a closed loop for Volume 4 • Issue 4 • 1000169

Figure 8: Pore volume and pore diameter plot showing most of the pores.

• Page 5 of 6 •

Citation: Hassan AZA, Mahmoud AWM (2015)Hydrothermal Synthesis of Nano Crystals (A.M.) Zeolite using Variable Temperature Programs. J Nanomater Mol Nanotechnol 4:4.

doi:http://dx.doi.org/10.4172/2324-8777.1000169 proved to be extremely low (0.2 meq/g), confirming that A.M. nano zeoliteS are not ideal for anion exchanging, unless modified or pre-treated. According to these results the A,M nano zeolite could potentially be used as cation exchangers, but not anion exchangers.

9. Prasad PSR, Prasad KS (2007) Dehydration and rehydration of mesolite: An in situ FTIR study. Micropor Mesopor Mater 100: 287-294.

Conclusion

11. Flanigen EM, Khatami H, Seymenski HA (1971) Infrared Structural Studies of Zeolite Frameworks, Molecular Sieve Zeolites-I. Adv. Chemistry Series 101: 201-228.

From the last invention it can be enhanced that the crystallization of A.M. nano-zeolites clinoptilolite controlled by a two stages variable-temperature program. It has a pronounced effect on crystal size and morphology. For a given Si/Al ratio, at synthesis temperature of above 1000ºC the smallest crystals were obtained whereas at crystallization temperatures lower than 150ºC, amorphous phase was observed. Nano Zeolite named A.M. with K, Al and Si in the molar ratio of 10 : 1 : 15 was synthesized at crystallization at two stages variable temperature program, and characterized by various techniques. The results indicate that the morphology, physical and chemical properties of crystals is also affected by crystallization temperature it can be concluded that crystallization temperature of 150ºC is appropriate for the synthesis of crystalline materials. While the crystallization temperature rise sequence till calcined at 1000 ºC the A.M nano zeolite approached to be hydrophilic, TEM enhanced the size of nano particles ranged between 19.2-24.6 nm. CEC recorded 0.45 meq./g while AEC recorded 0.2 meq/g. One can imagine how this ion-exchange property could be exploited commercially to soften water or to remove toxic or radioactive metal ions from water. BET recorded 68.71 m2/g and the pore size distribution is 1-5 nm. The A.M. nano zeolite type studied can potentially be used in industries such as agriculture, horticulture and for environmental protection. In summary, it is important to recognize that the use of nanostructuring or nanostructures to generate, fabricate or assemble high surface area materials is at an embryonic stage. The effect of the nanostructure and our ability to measure it will be increasingly important for future progress and development of materials for the marketplace. That said, it is apparent that so-called “mature” technologies such as catalysis, coatings, separations, etc., are already being impacted. Thus, one may eagerly anticipate exciting new advances in many diverse technological areas growing from our increasing understanding of nanostructuring and nanostructured materials.

10. Mozgawa W (2001) The relation between structure and vibrational spectra of natural zeolites. J Mol Struct 596: 129-137.

12. Poe BT, Mc Millal PFM, Angell CA, Sato R (1992) Al and Si coordination in SiO2-1bAl2O3 glasses and liquids: A study by NMR and IR spectroscopy and MD simul ations. Chem Geol 96: 333-349. 13. Farmer VC, Fraser AR, Tait JM (1979) Characterization of the chemical structures of natural and synthetic aluminosilicate gels and sols by infrared spectroscopy. Geochim Cosmochhim Acta 43: 1417-1420. 14. Freeman HP, Caro JH, Heinly N (1964) Effect of Calcination on the Character of Phosphate Rock. J Agric Food Chem 12: 479-486. 15. Coombs DS,Alberti A, Armbruster T, Artioli G, Colella C, et al. (1997) Recommended Nomenclature for Zeolite Minerals: Report of the Subcommittee on Zeolites of the International Mineralogical Association, Commission on New Minerals and Mineral Names. The Canadian Mineralogist 35: 1571-1606. 16. Breck DW (1974) Zeolite Molecular, chemistry and use. Wiley: New York, USA.

References 1. Oberdِrster G, Maynard A, Donaldson K, Castranova V, Fitzpatrick J, et al. (2005) Principles for characterizing the potential human health effects from exposure to nanomaterials: elements of a screening strategy. Part Fibre Toxicol 2:8. 2. Shiyun S, Zhongmin L, Peng T, Ziyu L, Lihong Q, Yangyang Z (2006) Synthesis of small crystals zeolite NaY. Materials Lett 60: 1131-1133. 3. Bhardwaj D, Tomar R, Khare SP, Goswami Y, Srivastva P (2013) Hydrothermal synthesis and characterization of zeolite: Effect of crystallization temperature. Res J Chem Sci 3: 1-4. 4. Galwey AK, Brown ME (2000) Thermal decomposition of ionic solids. Elsevier, Amsterdam. 5. Schmalzried H, Navrotsky A (1975) Festkörperthermodynamik/Chemie des festen Zustandes Verlag Chemie. Weinheim, Germany. 6. Camblor MA, Corma A, Valencia S (1998) Synthesis in fluoride media and characterization of aluminosilicate zeolite beta. J mater Chem 8: 2137-2145. 7. Mintova S, Valtchev V, Onfroy T, Marichal C, Knozinger H, et al. (2006) Variation of the Si/Al ratio in nanosized zeolite Beta crystals. Micropor Mesopor Mater 90: 237-245. 8. Tarte P (1967) Infra red spectra of inorganic aluminates and characteristic vibrational frequencies of AlO4 tetrahedra and AlO6 octahedra. Spectro Chim Acta 23: 2127-2143.

Volume 4 • Issue 4 • 1000169

Author Affiliation

Top

Agriculture research center, Soil and water and environment institute, Giza, Egypt 2 Cairo University, Faculty of Agriculture, Plant Physiology Department, Giza, Egypt 1

Submit your next manuscript and get advantages of SciTechnol submissions ™™ ™™ ™™ ™™ ™™ ™™

50 Journals 21 Day rapid review process 1000 Editorial team 2 Million readers Publication immediately after acceptance Quality and quick editorial, review processing

Submit your next manuscript at ● www.scitechnol.com/submission

• Page 6 of 6 •

Lihat lebih banyak...

Comentários

Copyright © 2017 DADOSPDF Inc.