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العنوان
Synthesis and characterization of Some Aminophosphonates Nano-composites and Their Applications for Removal of Some Heavy Metals /
المؤلف
Elshal, Shymaa Ismail Adel.
هيئة الاعداد
باحث / شيماء إسماعيل عادل إسماعيل الشال
مشرف / إبراهيم الطنطاوى السيد
مناقش / محمد فوزي عبد المنعم عميرة
مناقش / شيماء محمد السعيد
الموضوع
Materials-Surfaces. Nanostructures.
تاريخ النشر
2020.
عدد الصفحات
155 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
Organic Chemistry
تاريخ الإجازة
12/4/2020
مكان الإجازة
جامعة المنوفية - كلية العلوم - الكيمياء
الفهرس
Only 14 pages are availabe for public view

from 155

from 155

Abstract

The present thesis is divided into five chapters.
1- Chapter one: Introduction;
This chapter reported α-aminophosphonates, their importance in diverse fields. It also cleared nanomaterials definition and the novelty in the nanomaterials properties. This chapter showed the importance of removal of heavy metals from water .On this chapter different synthetic approaches to synthesize α-aminophosphonates and nanomaterials were investigated and implemented. Also this chapter presented three different types of adsorbents materials such as α-aminophosphonates, nano titanium oxide and nano titanium oxide that bounded to α-aminophosphonates for the adsorptive removal of the diverse kinds of heavy metals as divalent lead Pb(II) and copper cu(II) ions. Finally, this chapter was illustrated the three adsorbents and their contributions in the elimination of divalent lead and copper ions from water by detecting different controlling parameters with taking in the consideration both of the kinetic and adsorption models.
2- Chapter two: Experimental;
In this section all the chemicals, reagents and instruments used to synthesize and characterize the diverse sorbents were reported and illustrated. This section included the experimental procedures used for the synthesis and preparation of the different nanosorbents accompanied with schematic diagram for each synthetic approach. This section also reported all the technical procedures for the diverse controlling factors during the adsorptive removal process of the divalent ionic lead and copper by using (the batch technique and the column technique). The controlling factors for the batch technique include the reaction pH, contact time between the sorbent and sorbates, the nanosorbent dosage, the metal ion concentration, and the effect of interfering ions. In the other hand the controlling factors
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for the column technique were the flow rate of the effluent, the sorbent dosage, and the width-highest of the microcolumn.
3- Chapter three: Results and Discussion;
This chapter is divided into two main parts:
The First part; this part established and investigated the sorbents characterization by using different instruments like Fourier Transform infrared analysis (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and high resolution transmission electron microscope (TEM. The acquired FT-IR spectra of sorbents were achieved in the frequency range of 400-4000 cm-1. The FT-IR spectrum was characterized by the presence of the diverse peaks for each sorbent due to the different chemical structures and functional groups of each sorbent. Thermal gravimetric analysis (TGA) was acquired in the heating temperature range 20-600oC to identify the possible thermal degradation steps for each nanosorbent. In some cases the TGA-thermogram of sorbent was identified to refer to undetected mass loss which means highly thermal stability of this sorbent.
The XRD diagrams of nanosorbents were identified by a series of peaks within the range 2θ (0-80) according to the different 2θ value for each nanosorbent. The high resolution transmission electron microscopic (HR-TEM) of sorbents was acquired using 200 kV. The shape of N-TiO2-α-Am.Ph nanosorbent was completely different from those of N-TiO2 and α-Am.Ph sorbents to confirm the success of combination of these two materials to form the new designed nanosorbent. The characterized particle size of α-Am.Ph is 458.18 nm, while N-TiO2 recorded 62.78-120.99 nm. The HR-TEM image of N-TiO2-α-Am.Ph is illustrated with the distribution of average particle size in the range 75.35-153.55 nm to confirm the direct immobilization of α-Am.Ph molecules on the surface of N-TiO2 to form the aimed N-TiO2-α-Am.Ph nanocomposite.
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The second part; this part was reported the adsorptive removal of the divalent lead and copper using the diverse sorbents in the presence of different controlling parameters like;
pH Effect on the adsorption capacity values. The results of this study were expressed in mmolg-1 versus the initial pH value of metal ion solution. It was found that the surface of N-TiO2, was loaded with –OH groups. These functional groups were directly responsible for the metal binding via ion exchange or complex formation mechanism. The reactivity of the surface loaded –OH groups was directly dependent on the pH value of contact solution. Metal ion solutions with low pH values (≤ 3.0) were generally facing strong competition due to the presence of the high concentrations of hydrogen ions which occupied and protonated the surface active binding sites to increase the positive charge density on the surface of metal oxides. This condition led to increase the repulsive forces between the positively charged metal ions and the positively charged protonated surface functional groups. By increasing the pH value of metal ion solution the degree of surface protonation became small and the surface -OH will had a strong binding affinity with the target metal ions.
Contact time effect on the adsorption capacity values was indicated in the presence of various time intervals (1, 5.0, 10, 15, 20, 30, 40, 50 and 60 min) where the reaction pH and initial metal ion concentration were optimized. Nanosorbents were found to have different behaviors with the contact time values gradually increase the metal capacity upon increasing the time from 1 to 20, 30, 40, 50, and 60 min according to the equilibrium for each one. In some cases after the equilibrium was obtained a decreasing in the metal capacity was obtained. This behavior may be attributed to the possible desorption of the loaded metal ions from the nanosorbents surface at higher reaction times.
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The adsorbent dosage effect on the adsorption capacity values was identified by using different sorbents doses ranging from 5.0 to 100.0 mg to evaluate the variation in the metal adsorption capacity values. The metal adsorption capacity values were found to decrease upon increasing the nanosorbent dosage from 5 to 100 mg. The highest metal capacity value of the divalent ionic lead and copper was obtained upon using 5.0 mg and the lowest value was identified upon using 100 mg of each sorbent. The observed behavior in low sorbent dosages was mainly attributed to the greater availability of metal ions compared to the active surface functional groups on the sorbents. In addition, the high metal capacity values at lower adsorbent dosage may be also explained on the basis of an increased metal to sorbent ratio. The low metal adsorption capacity values at higher masses were mainly due to the less availability of functional groups compared to the number of available metal ions in the aqueous solution.
Initial metal ion concentration effect on the adsorption capacity values was characterized by using different initial metal concentrations ranged from 0.1 to 2.0 ml of 0.1mol L-1. The outlined results indicated that the increasing in the initial metal ion concentration would enforce an increase in the metal adsorption capacity values of the divalent ionic lead and copper. The generated driving force by increasing the initial metal ion concentration affected the mass transfer barrier between the adsorbent and the metal ion in the contact solution therefore, a higher initial concentration of metal ion was expected to enhance and increase the adsorption capacity of the divalent ionic lead and copper using the diverse sorbents. Based on this assumption, the adsorption capacity values were found to gradually increase with increasing the metal ion concentration from 0.1 to 2.0 ml of 0.1 mol L-1.
Coexisting ions effect on the adsorption capacity values of the divalent ionic lead and copper using the diverse sorbents were studied upon using
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Na(I), K(I), NH4+, Mg(II) and Ca(II). The obtained results of metal capacity values were found to exhibit different trends of metal capacity values according to the chemistry of sorbents and the chemistry of interfering ions. Finally the applications of sorbents in the removal of 1.0 mg L-1 of the divalent ionic lead and copper from water samples were determined and studied using multi-stage microcolumn system packed each with different doses of sorbents. The collected results confirm a good correlation values between the removal of the divalent ionic lead and copper ions from water. The highest percentage removal values were established after the third run of extraction with the percentage recovery values were corresponded to 89 to 94 % using the different nanosorbents.
4- Chapter Four: General Conclusion
This chapter outlines our findings, conclusion and recommendations based on the collected results from this study.
5-Chapter Five: References
List of references were cited at the end of this thesis.