İtakonik asit-akrilamid kopolimerlerinde monamer reaktiflik oranlarının belirlenmesi
Determination of the monomer reactivity ratios for itaconic acid and acrylamtde copolymers summary
- Tez No: 66532
- Danışmanlar: DOÇ. DR. NURSELİ UYANIK
- Tez Türü: Yüksek Lisans
- Konular: Kimya, Chemistry
- Anahtar Kelimeler: Belirtilmemiş.
- Yıl: 1997
- Dil: Türkçe
- Üniversite: İstanbul Teknik Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Kimya Ana Bilim Dalı
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 83
Özet
ÖZET Bu çalışmada 5 adet poliitakonik asit (PIA) ve 3 adet poliakrilamid (PAAm) homopolimeri ile 11 adet itakonik asit, akrilamid ve bir adet itakonik asit, N- izopropil akrilamid kopolimeri sentezlenmiştir. Herikiside suda çözünen monomerlerden olan itakonik asit ve akrilamidin polimerizasyonu için sulu çözeltide K2S2O8 ile, Ce(TV) ile ve Ce(IV)-NTA redoks çifti ile N2 atmosferinde, 50°C'da deneysel çalışmalar yapılmıştır. Bu çalışmalarda, dönüşüm yüzdesine bağlı olarak farklı sürelerde reaksiyona devam edilmiştir. Elde edilen homopolimer ve kopolimerlerin FTIR spektrumlan çekilerek ve 0,333 gr/100ml konsantrasyonda r|sp/c değerleri belirlenerek karakterizasyonlan yapılmıştır. Polimerizasyon dönüşüm yüzdesi, %15'in altında tutulan 4 örnek kullanılarak reaktiflik oranlan hesaplanması amaçlanmıştır. Hazırlanan kopolimerlerin potansiyometrik ve kondüktometrik yöntemlerle bileşim yüzdeleri belirlenerek elde edilen verileri Kelen-Tüdos yöntemi uygulanmış ve monomer reaktiflik oranlan riA=0,546 ± 0,116 ve rAAm= 0,4408 + 0,0342 olarak bulunmuştur.
Özet (Çeviri)
Copolymerization may be defined as any process whereby two or more monomers are incorporated as integral parts of a high polymer. A copolymer is a product resulting from such a process. If the chains are long, the composition of the copolymer and the arrangment of units along the chains are determined by the relative rates of the various chain propagation reactions. The chain propagating reactions that occurs when two monomers, Mi and M2 are present, may be written as follows. M^+M^Mi* vn=kii[Mi*][Mi] Mi*+M2-*M2* vi2=ki2 [M!*][M2] M2*+Mı -» Mı * v21=k2ı [M2*][Mi] M2*+M2-»M2* v22=k22[M2*][M2] where Mi* and M2* represent chain radicals having monomers Mi and M2 respectively as their terminal units. The steady state condition reduces in approximation to k2ı[M2*][M,]=k12[Mı*][M2] VI- d[Mı] /dt=kn[M1*][Mı]+k2ı [M2*][Mı] -d[M2] /dt=kı2[Mı*][M2]+k22 [M2*][M2] Dividing of the last two equations with simplifing d [Mi] \M{\ rı[M,]+[M2] d[M2] [M2] r2[M2]+[Mi] is obtained there n and r2 are the monomer reactivity ratios defined by n- J^l and n- M kl2 k21 In this work, itaconic acid (IA) copolymerized with acrylamide (AAm) in aqueous solution with K2S20g at 50°C. The copolymerization of IA with styrene, methylmethacrylate, vinyl acetate, vinyl chloride acrylonitril, ethly methacrylate monomers worked under different conditions and the monomer reactivity ratios were calculated. The purpose of this study was to obtain the reactivity ratios of IA-AAm. First of all, the homopolymers of IA and AAm were synthesized by using different methods (Table 1.). The polymerization conditions were chosen as starting with K2S20g in aqueous solution at 50°C at nitrogen blanket. The compositions of the monomer feed and of the polymer formed may be expressed as mole fractions. Is while reactivities of the two radicals may be different, the polymer composition is expressed as to the monomer composition throughout the range in the chain. To investigate the difference of the rates of the radicals, the polymerization must be cut at maximum 15% conversion. For the time needed to this conversion, some copolymers were synthesized at high conversion for long polymerization time. The copolymerization conditions of the samples that were used to determine the reactivity ratios were given in Table 2. The homopolymers and copolymer obtained were also characterized by DR.. After the synthesise of the copolymers, the copolymer composition was determined by conductometric and potentiometric methods. vuTable 1. Polymerization Conditions of Homo PIA and Homo AAm T = 50°C Polymerization period 48h, at N2 atmosphere a [Ce (TV)] = lxl0“2 mol.lt”1 b Polimerization in vacua c [Ce (IV)] = 1.5xl0“2 mol. It'1 and [NTA] = l.OxlO”2 mol.lt'1 as redox system. d Polimerization period 4.5 h e Polimerization period 0.75 h For the determination of the copolymer compositions, before using the conductometric and potentiometric methods, the solutions of PIA with different concentrations were prepared in 0,1N NaCl aqueous solutions. The total volume of 0.1N NaOH required for titration of PIA solutions were obtained by PH and by conductivity measurements using potentiometric and conductometric methods, respectively. The volumes of 0,1N NaOH were plotted against the concentrations of PIA (Fia (Theoretical)). The calibration curves were given in Figures 1 and 2. The copolymer composition given in Table 2 were performed insolutions using 0.1N NaCl. The volume required for the titration was labeled on the calibration curves depending on the used method to obtain monomer composition incorporated to copolymer. The composition of the monomer feed to the copolymer formed were plotted by using the results obtained with two methods (Fig.3).The equation, a.J a via> Figure 1. The Calibration Curve Obtained From The Results of the Conductometric Titration Against The Theoretical Value of Fia- > Figure 2. The Calibration Curve Obtained From the Results of the Potentiometric Titration Against The Theoretical Value of Fia. IX80 r Figure 3. Dependence of the Mole Fractions of IA in the Copolymers (Fia) on the Mole Fractions of IA in the Initial Mixtures (fk) The Curves are Calculated by Using Conductometric Method (- ); Potentiometric Method (-- -). Table 2. Polymerization Conditions for IA - AAm Copolymers (T = 50°C, at Nitrogen Blanket)is known as Kelen-Tudos equation, the application of the monomer feed (Table 3 and 4.) A least square plot of the data in the final two columns of Table 3 calculated as riA = 0.662 and rAAm=0,407 ( y=0,965) by conductometric, in Table 4 calculated as riA=0,43 and rAAm=0>475 ( y=0,986) by potentiometrie methods. The values calculated by the two methods were averaged with standart deviations as riA=0,546±0.116 rAAm=0.441 ± 0.0342 Table 3. Data for Copolymerization of IA and AAm Including Kelen - Tudos Parametres (Conductometric Method) Where n = G/ (cc+F), Ç = F / (a+F), G = x(y-l)/y, F=x2/y, x= WW y^FiA/FAAm and a is the geometric mean of the lowest and the highest F values. a = 0.106 ri = 0.662 r2 = 0.407 Y = 0.965 Table 4. Data for Copolymerization of IA and AAm Including Kelen- Tudos Parameters. (Potentiometrie Method) cc = 0.135 ri = 0.430 r2 = 0.475 7 = 0.987 XI
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