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العنوان
Synthesis and applications of some new phthalimide polymers /
المؤلف
alazrak, Alshimaa mahmoud elsayd.
هيئة الاعداد
مشرف / شيرين عوض عبد القادر
مشرف / محمد جمعة محمد عاصى
مشرف / عبدالحميد عبده على إسماعيل
مشرف / وجدي ابراهيم الدجدج
تاريخ النشر
2021.
عدد الصفحات
200 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
Organic Chemistry
تاريخ الإجازة
1/10/2021
مكان الإجازة
جامعة بنها - كلية العلوم - علم الكيمياء
الفهرس
Only 14 pages are availabe for public view

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from 243

Abstract

SUMMARY
The polymers industry has become a vital field for chemists’ research, so that its use has recently become a necessary part in daily life as a basic material in daily industrial sectors such as building materials, adhesives, paper, clothing, plastics, fibers, ceramics, liquid crystals, concrete, medicines, containers, Preserving blood, cosmetics and detergents. Polymers are one of the materials that are very light in comparison with their strength, and this is clearly evident when compared with other synthetic materials. Researchers are continually aiming to design new polymer materials with new properties in many ways, including co-polymerization and exchange reactions, for use in various industrial applications.
The present thesis is composed of three main chapters, each of which can be summarized as follows:
Chapter one:
contains general introduction about polymer, classification of polymers based on Source, structure, mode of polymerization, types of monomers, copolymerization, methods for determination of monomer reactivity ratio, surface active agents (surfactants), classification of surfactants (nonionic, ionic, cationic, zwitterionic surfactants), polymeric surfactants and its applications, Corrosion; definition and causes. Also contains classification of corrosion (electrochemical, chemical corrosion, corrosion in other fluids), types of corrosion (general corrosion, localized, crevice, pitting, stress corrosion cracking, intergranular, galvanic), corrosion resistance, methods of corrosion protection, application of protective coatings, classification of corrosion protection (cathodic protection and corrosion inhibitor), factors influencing the effectiveness of cathodic protection such as protective coatings, environment and temperature, inhibitors classifications, mechanism of action of inhibitors and methods used for measuring corrosion. Finally it contains a literature survey that connected to the previous works.
Chapter two:
Includes; chemical materials used and various analyzers such as infrared (IR), nuclear magnetic resonance spectroscopy (1HNMR), Tensiometer (for surface tension measurement), Conductiometer (for electrical conductivity measurements) and potentiostat (for electrochemical measurements). It also includes practical experiments for preparation of N-methacryloxypethalide (NMP), N-phthalimidomethyl methacrylate (PMMA) as well as N-phthalimidomethyl acrylate (NPMA) monomers, co-polymerization of the monomer N-phthalimidomethyl methacrylate with 1-vinylimidazole, determination of monomer reactivity ratio, the polymerization of the three monomers and exchange reactions of the them with N-N-dimethylpropylamine and N-N-dimethyl aminoethanol as well as the preparation of surfactant polymers and measuring their surface properties and thermodynamics such as surface (ST) and interfacial tension (IFT), krafft point (Tkp), foaming power, emulsion stability, critical micelle concentration (CMC) by (ST) and electrical conductivity (E.C), and also the different air/ water interface parameters including effectiveness (πCMC), efficiency (Pc20), maximum surface excess (Γmax) and minimum surface area (Amin). Standard free energy (ΔGº) for both micellization and adsorption processes were also recorded, HLB for all and biodegradability for most of these cationic surfactants has been investigated, testing some compounds as corrosion inhibitors and also measuring the biological activity of some of the resulting compounds.
Chapter three:
1- Study of the synthesis of N-methacryloxyphthalimide (NMP), N-phthalimidomethyl methacrylate (PMMA), and N- phthalimidomethyl and acrylate (NPMA) monomers using N,N-Dicyclo-hexylcarbodiimide (DCCI) as a condensing agent as following:
2- Copolymerization reaction of (NPMMA) monomer with 1-vinylimidazole monomer was carried out by solution polymerization in dimethylformamide (DMF) at 65oC in the presence of 1 mol % benzoyl peroxide (BzO2).
3- Study co-polymerization of NMP and NPMMP monomers with styrene in the same way as the previous polymerization.
4- The copolymer composition was calculated from 1HNMR spectroscopy for Copolymerization of (NPMMA with VIM) and from nitrogen analysis for co-polymerization of NMP and NPMMP monomers with styrene. The monomer reactivity ratios (r1 and r2) of each system were calculated according to Fineman-Ross and Kelen-Tudos methods.
The r1r2 values for the system (0.781, 0. 853, 1.153) respectively indicate that the copolymer should have a random distribution of the monomer units with a tendency toward alternation and it is found that NPMMA-Co-VIM system gave no azeotropic composition according to composition the experimental results and the composition curves calculated on the bases of the determined monomer reactivity ratios.
5- Then polymerization of NMP (III)a, NPMMA (III)b and NPMA (III)c monomers using benzoyl peroxide (BzO2) as initiator as following:

6- Also study the exchange reactions of poly- (NMP, NPMMA and NPMA) with N,N-dimethyl-1,3-diaminopropane .
The three polymers also was tested for their ability to enter an exchange reactions with N,N-dimethylaminoethanol as following scheme:
7- A new series of cationic polymeric surfactants was synthesis from copolymer system and exchangable polymers by their reaction with excess amount of DMS in the absence of solvent in a closed system with stirring at 95oC for 48 hrs, the reaction yielded compounds as brown, pale yellow and deep yellow viscous oily. Scheme for co-polymeric surfactants:
Scheme for un soluble exchangable polymeric surfactants:
Scheme for soluble exchangable polymeric surfactants:
The chemical structure of the produced monomers, polymers, copolymers, exchangable polymers and polymeric surfactants of copolymers and exchangable polymers was confirmed by spectroscopic tools.
Chapter four:
Study the surface properties included:
1- Surface tension; (PS)6 recorded the highest value of surface tension (42.5 mNm-1) and (Co-PS)4 recorded the lowest value (32.28 mNm-1).
2- Interfacial tension; the compounds showed low values ranged from (3.0- 6.5 mNm-1), these lower values indicate the ability of using these surfactants in several applications as corrosion inhibitors and biocides.
3- Critical micelle concentration (CMC) has been measured in aqueous medium by traditional procedures by surface tension (ST) and electrical conductivity (E.C) methods, (Co-PS)4 recorded the lowest CMC and be economically very important in industrial fields. Also PS11 recorded the highest CMC. CMC recorded by (ST) was more accurate than that of the (E.C).
4- Krafft point; its lower under 0 oC for all polymeric cationic surfactants within this study gives it the tendency to be used in wide range application in industrial fields at low temperatures.
5- Foaming power; (Co-PS)5 which is the most stable one and recorded the higher foam height and (PS)11 recorded the lower foam height.
6- Emulsion stability; (PS)10 was the most stable compound and (PS)6 was the less stable.
7- Effectiveness (πcmc); (Co-PS)4 that gives the maximum reduction of the surface tension (38.89 mNm-1) and (PS)6 gives the minimum reduction of the surface tension (25.2 mNm-1).
8- Maximum surface excess (Γmax); (PS)11 recorded the highest value of Γmax (8.91 mol/cm2) and (Co-PS)5 recorded the lowest value of Γmax (3.40 mol/cm2).
9- Minimum surface area (Amin); (Co-PS) 5 recorded the highest value (0.488 nm2) and (PS)9 recorded the lowest value (0.186 nm2).
10- Efficiency (Pc20); (PS)11 was found to be the most efficient polymeric surfactants with value (7.79x10-3).
11- Standard free energy (ΔGº) for both micellization (ΔGomic) and adsorption (ΔGoads) processes were recorded negative values.
12- Biodegradability for most of these cationic surfactants had been investigated and their (D %) was ranged from 61 to 100 % after 15 days.
13- HLB for all prepared cationic surfactants has been calculated and PS9-11 was the most hydrophilic compound and record higher value of HLB (17.63) and PS8 was more hydrophobic compounds and record lower value (6.95).
Some of prepared compounds were tested as the prepared compounds were evaluated as corrosion inhibitors against C-steel (42CrMo) electrode in 1 M HCl solution corrosive medium using chemical methods, corrosion rate (r) and inhibition efficiency (IE %) were computed and was ranged from 87.5 to 94.0%.
The antimicrobial activity of some of the synthesized compounds were screened using the diffusion agar techniques and were tested against some bacterial and fungal species and the study showed varying results, the compound XIa exhibited the more activity against Escherichia coli, VI4, XIIIc, XIV5, XVIXb against Pseudomonas aeruginosa, XIa and XVIXc against Klebsiella pneumonia, VI5 against Aspergillus flavus, IIIa against Penicillium notatum, IIIa and VI1 against Aspergillus niger.