Search In this Thesis
   Search In this Thesis  
العنوان
Synthesis, characterization and applications of some heteropoly acids supported on mesoporous silica coated metal ferrites nanoparticle catalysts /
المؤلف
Hayes, Ola Ragab Abd Alaziz.
هيئة الاعداد
باحث / علا رجب عبدالعزيز حايس
مشرف / عوض إبراهيم أحمد
مشرف / وفاء صلاح الدين أبواليزيد
مناقش / عوض إبراهيم أحمد
الموضوع
Chemistry, Physical and theoretical. Heteropoly acids. Nanoparticle catalysts.
تاريخ النشر
2019.
عدد الصفحات
online resource (146 pages) :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
الكيمياء
الناشر
تاريخ الإجازة
8/3/2020
مكان الإجازة
جامعة المنصورة - كلية العلوم - الكيمياء
الفهرس
Only 14 pages are availabe for public view

from 172

from 172

Abstract

ABSTRACT: Development of new methods for the preparation of recyclable catalysts of environmental is importance in chemical technologies and pharmaceutical industries. Catalytic reactions are important for green chemistry due to decrease the small amount of waste generated. Mesoporous materials have a unique structure, thermal and high stability, engineering of acid sites and selectivity. Mesoporous materials designated as M41S such as MCM-41. In this thesis, we can modify properties of MCM-41by NF, PWA and SO42-. In this thesis we prepared different solid catalysts. 1-Synthesis MCM-41, synthesis of NF-MCM-41, several catalysts containing NF-MCM-41 with different percentage by weight of PWA (10, 25, 35, 45, 55 and 65) were prepared by impregnation method then calcined at 450 °C for 4 hrs ,the sample 55W/NF-MCM-41 was calcined at 400 and 550 0C and synthesis 25W/ MCM-41 and calcined at 450 0C for 4 hrs. 2- Several catalysts containing 10W/NF-MCM-41-III with different percentage by weight of SO42-(5, 10, 15, 20, 25, 30, 35 and 50%) were prepared by soaking 10W/NF-MCM-41-III with different wt. % of H2SO4 acid (3M) and then calcined at 450°C for 4 hrs. 20 S/10W/ NF-MCM-41 was calcined at 400 and 550 0C for 4 hrs, synthesis 20 S/10W/ MCM-41, 20 S/NF-MCM-41 and 20 S/MCM-41 and were calcined at 450 0C for 4 hrs. 3- Structural characterization of the prepared catalysts and the phase changes were determined using X-ray, FTIR, TEM and SEM techniques. 4- The total surface acidity and the acid strength of prepared catalysts were determined by titration with n-butylamine in acetonitrile. •Pure MCM-41 is weakly acidic in nature. NF-MCM-41was accompanied by increasing both surface acidity and acid strength (Ei =+195.8mV). The addition of W to NF-MCM-41 was accompanied by a gradually increase in both surface acidity and acid strength to reach a maximum a 55 W/NF-MCM-41 –II (Ei =+592.4mV). • Modification of 10W/NF-MCM-41-III because it has the smallest surface acidity and acid strength by the addition of sulfated. The total acidity and acid strength increase by the addition of sulfated to 10W/NF-MCM-41-III till reach the maximum at 20S/10W/NF-MCM-41.The total acidity and acid strength decrease by increasing the calcinations temperatures. • 5- The catalytic activity of the prepared catalysts was measured by two reactions: The synthesis of 7-hydroxy-4-methylcoumarin:• The formation of 7-hydroxy-4-methylcoumarin in presence of MCM-41 and NF-MCM-41 have no yield. The formation of 7-hydroxy-4-methylcoumarin increases gradually with increasing the amount of PWA loaded on NF-MCM-41 till reach the maximum at 55 W /NF-MCM-41-II. The yield of 7-hydroxy-4-methylcoumarin decreased by increasing the calcinations temperatures. •The formation of 7-hydroxy-4-methylcoumarin increases gradually with increasing the amount of S loaded on 10W/NF-MCM-41 till reach the maximum at 20 S/10W/NF-MCM-41-II. Increasing the calcination temperatures for the sample 20 S/10W/NF-MCM-41 from 400 to 450 0C, the formation of 7-hydroxy-4-methylcoumarin increases then decreases by raising the temperature to 550 0C. The synthesis of xanthene :•The best results were obtained using a molar ratio of 1:2 benzaldhyde: B-napthol , the reaction was finished after 1 1/2 hrs (as indicated by TLC).• 0.05 g of the catalyst is an appropriate amount for xanthene to be formed in a good yield.• The formation of xanthene in presence of MCM-41 is small, addition of NF leads to increase in the formation of xanthene because the reaction depends on the number of Bronsted or Lewis acid sites. The formation of xanthene increases gradually with increasing the amount of PWA loaded on NF-MCM-41 till reach the maximum at 55 W /NF-MCM-41-II. The yield of xanthene decreased by increasing the calcinations temperatures.• The formation of xanthene increases gradually with increasing the amount of SO42- loaded on 10W/NF-MCM-41 till reach the maximum at 20S/10W/NF-MCM-41-II. By increasing the calcination temperatures for 20S/10W/NF-MCM-41 from 400 to 450 0C, the formation of xanthene increases then decreases by raising the temperature to 550 0C.• All the catalysts can be separated from the product by a magnet and reused several times Key words: MCM-41, NF-MCM-41,PWA and catalytic activity.