Synthesis,characterization, flocculation,and rheological characteristics of hydrolyzed and unhydrolyzed polyacrylamide‐grafted poly(vinyl alcohol)

Graft copolymers of poly(vinyl alcohol) and polyacrylamide (PVA‐g‐PAM) were synthesized using a ceric ion–induced solution polymerization technique at 28°C. Three grades of graft copolymers were synthesized with varying acrylamide concentrations. Three grades of hydrolyzed products of PVA‐g‐PAM were synthesized with varying concentrations of sodium hydroxide solution. Hydrolyzed and unhydrolyzed PVA‐g‐PAM were characterized by viscometry, X‐ray diffractometry, infrared spectroscopy, and thermal analysis. Rheological investigation was also carried out on the aqueous solutions of various samples. The flocculation characteristics of various materials were investigated by the use of jar and settling tests in 0.25 and 5 wt %, respectively, using kaolin and iron ore suspensions. Among the series of graft copolymers, the one with fewest but longest PAM chains showed superior performance. The flocculation characteristics of the best‐performing graft copolymer were compared with those of various commercially available flocculants in the two suspensions under investigation. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2109–2122, 2006     

Synthesis,characterization, and flocculation characteristics of polyacrylamide‐grafted glycogen

The synthesis of glycogen‐g‐polyacrylamide (Gly‐g‐PAM) was carried out by a ceric ion‐induced solution polymerization technique. Six grades of graft copolymers were synthesized by the variation of catalyst and monomer concentrations. These graft copolymers were characterized by intrinsic viscosity measurements, FTIR spectroscopy, and X‐ray diffraction techniques. Flocculation performance of these graft copolymers were done in kaolin suspension. Of the above grades, the graft copolymer Gly‐g‐PAM 5, which has longer PAM chains, showed best flocculation performance. The flocculation performance of the graft copolymer was compared with commercial flocculants and other PAM‐grafted flocculants developed so far in the authors' laboratory. In all the cases, it was found that the graft copolymer performed the best. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 773–778, 2007     

Synthesis and characterization of grafted carboxymethyl guar gum

Graft copolymers of carboxymethyl guar gum (CMGG) and polyacrylamide (PAM) have been synthesized by grafting polyacrylamide chains onto carboxymethyl guar gum backbone using a ceric‐ion‐induced solution polymerization technique. By varying the amount of initiator, three different grades of graft copolymers are synthesized. The characterization of graft copolymer is carried out by FTIR, NMR, intrinsic viscosity measurement, SEM, SLS, DTG, and rheology. A comparison of flocculation efficiency of CMGG and its graft copolymer shows that the graft copolymer exhibits better flocculation performance. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

The flocculation and rheological characteristics of hydrolyzed and unhydrolyzed grafted sodium alginate in aqueous solutions

Sodium alginate is a natural anionic polysaccharide obtained from natural and microbial resources. It is also used as a flocculating agent and thickener. It is grafted with polyacrylamide, in the presence of ceric ammonium nitrate (CAN) as an initiator. The graft copolymer (SAG‐g‐PAM) is again hydrolyzed with some amount of alkali. The flocculation characteristics of hydrolyzed graft copolymer (Hyd SAG‐g‐PAM) are compared with that of the unhydrolyzed ones, in 5 wt % kaolin and 10 wt % iron ore suspensions. The flocculation characteristics of the hydrolyzed graft copolymer are also compared with those of some of the commercial flocculants. The SAG‐g‐PAM and Hyd SAG‐g‐PAM are characterized by IR and intrinsic viscosity measurements. The rheological properties of aqueous solutions of hydrolyzed and unhydrolyzed graft copolymers are measured by Advanced AR‐1000 Rheometer. There is drastic enhancement in flocculation and viscosifying characteristics on hydrolysis of the graft copolymers. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 1480–1488, 2004     

Synthesis,characterization, and flocculation characteristics of hydrolyzed and unhydrolyzed polyacrylamide grafted xanthan gum

The partial hydrolysis of xanthan gum‐g‐polyacrylamide was carried out in alkaline medium. Four grades of partially hydrolyzed products were synthesized by varying the reaction parameters. The neutralization equivalents of these products were determined by titration with standard sodium hydroxide solution. The flocculation characteristics of all the hydrolyzed graft copolymers and the unhydrolyzed xanthan gum‐g‐polyacrylamide were determined in 5 wt % iron ore and kaolin suspensions. The partially hydrolyzed product with neutralization equivalent of 1000 g showed better performance than that of other partially hydrolyzed products, but all hydrolyzed products exhibited poorer performance than that of the unhydrolyzed product in flocculation. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 1411–1419, 2004     

Novel biodegradable flocculating agents prepared by grafting polyacrylamide to Konjac

Grafting copolymers of polyacrylamide (PAM) with Konjac gum (KGM) have been synthesized using ceric‐ion‐induced initiation technique. The copolymers were characterized using several instrumental techniques, including infrared (IR) spectroscopy, elementary analysis, scanning electron microscopy (SEM), size exclusion chromatography (SEC) analysis, and intrinsic viscosity to confirm the success of grafting. The flocculation performance of graft copolymers was characterized by two methods. One was to study the relationship between the flocculants doses in kaolin suspension and the supernatant transmittance, and the other is to examine the time dependence of sediment height of kaolin suspensions. It was found that the graft copolymer is better than KGM and pure PAM. Biodegradation behavior was testified by monitoring the decay of relative viscosities, and approved by KGM ether bonds breaking in IR spectra and the molecule weight reduction in SEC analysis. The results indicate that the grafted KGM copolymers have improved both, flocculation performance and better biodegradable properties than the unmodified parent KGM and pure PAM. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis,characterization and application of novel polyacrylamide‐grafted barley

Polyacrylamide‐grafted barley (BAR‐g‐PAM) was synthesized by ceric ion‐based conventional method. The grafting of polyacrylamide chains on the polysaccharide backbone was confirmed through various physicochemical techniques such as intrinsic viscosity measurement, ¹³C‐NMR spectra, FTIR spectroscopy, elemental analysis, scanning electron microscopy morphology, thermogravimetric analysis study, number‐average molecular weight, and aqueous solubility. Furthermore, flocculation efficacy of the graft copolymers was studied in coal fine suspension through “jar test” procedure, toward its possible application as a novel flocculant for treatment of coal washery effluent. BAR‐g‐PAM is reported as a novel flocculant that can be used for bulk treatment of coal washery effluents. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 41046.     

Development of novel polymeric flocculant based on grafted sodium alginate for the treatment of coal mine wastewater

Sodium alginate-g-polyacrylamide (SAG) was synthesized by ceric ion induced redox polymerization technique. Six grades of graft copolymers were prepared by varying as well as monomer concentrations. The graft copolymers were characterized by intrinsic viscosity measurements, IR, and ¹³C-NMR spectroscopies. Of the above grades, the graft copolymer of grade six (SAG-VI), which has longer polyacrylamide chains, was used for flocculation study. Two coking and noncoking coal fine suspensions were selected for the flocculation study. The flocculation performance of the graft copolymer was compared with commercial flocculants. In all cases, it was found that the graft copolymer showed better performance than the commercial flocculants. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 375–382, 2001     

Grafted polysaccharides based on acrylamide and N,N‐dimethylacrylamide: Preparation and investigation of their flocculation performances

The graft copolymerization of N,N‐dimethylacrylamide (DMA) and acrylamide (AM) were carried out onto different polysaccharide backbones separately. The graft copolymers were synthesized by ceric ion induced redox polymerization technique. Three polysaccharides were used, namely hydroxyethyl starch (HES), hydroxyethyl cellulose (HEC) and Amylopectin (AP), for the grafting reactions. Among the three polysaccharides, HEC has linear structure, while HES and AP have a branch one. The graft copolymers were characterized by intrinsic viscosity measurements, FTIR spectroscopy, NMR (both ¹H and ¹³C) spectroscopy, and thermal analysis. Flocculation performances of the graft copolymers were evaluated in 1 wt % kaolin and in 0.25 wt % iron ore suspensions. A detailed comparative study of the flocculation properties of the synthetic graft copolymers was also made. It showed that graft copolymers based on DMA were better flocculants than those based on AM. Among the synthetic graft copolymers, HES‐g‐Poly (DMA) performed best when compared with the other synthetic graft copolymers as well as to the commercial flocculants in the same suspensions. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

微波辐射下壳聚糖-丙烯酰胺接枝物的合成及其絮凝性能研究

以硝酸铈铵作为引发剂、丙烯酰胺为单体,用微波辐射法合成了壳聚糖-丙烯酰胺接枝共聚物。通过正交试验考察反应条件对接枝率和接枝效率的影响,得出最佳工艺条件为:反应时间12 min,引发剂浓度5 mmol/L,丙烯酰胺和壳聚糖质量比5:1,反应温度40℃。最佳条件下接枝率和接枝效率分别达到148.6%和44.0%。壳聚糖接枝物与聚丙烯酰胺(PAM)对高岭土悬浮液的絮凝对比试验表明:在酸性条件下接枝物与PAM的絮凝效果相近;在中性和碱性条件下接枝物的絮凝性能优于PAM。     

Comparative studies on the flocculation characteristics of polyacrylamide grafted guar gum and hydroxypropyl guar gum

The synthesis of two polysaccharide‐based graft copolymers with acrylamide, guar gum grafted polyacrylamide (GG‐g‐PAM) and hydroxypropyl guar gum grafted polyacrylamide (HPG‐g‐PAM) is described. The graft copolymers have been characterized by viscometry, infrared spectroscopy and thermal analysis. The flocculation characteristics of the graft copolymers have been studied in kaolin, iron ore, and silica suspensions. For the base polysaccharides guar gum (GG) and hydroxypropyl guar gum (HPG), it is observed that GG exhibits better performance than HPG in all three suspensions. For the graft copolymers, HPG‐g‐PAM shows better performance than GG‐g‐PAM. The flocculation characteristics of the best performing graft copolymer (HPG‐g‐PAM) are compared with various commercially available flocculants in the three suspensions mentioned above. © 2001 Society of Chemical Industry     

Characterization of polyacrylamide-grafted sodium alginate: A novel polymeric flocculant

The synthesis of sodium alginate-g-polyacrylamide was carried out by a ceric-ion-induced solution polymerization technique. Six grades of graft copolymers were synthesized by the variation of catalyst and monomer concentrations. These graft copolymers were characterized by intrinsic viscosity measurements, ¹³C-NMR spectroscopy, infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, and X-ray diffraction. From the characterizations, it could be concluded that there was a substantial amount of grafting with a minimum formation of homopolymer. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 3296–3308, 2001     

Enzyme hydrolysis of grafted amylopectin

Previous methods of proof of grafting are based on separation of homopolymers from crude reaction products and further characterization of extracted component. This article reports the proof of grafting by a combined use of viscometry and enzyme hydrolysis that, to our knowledge, has not been reported so far. Two series of graft copolymers of amylopectin with polyacrylamide were synthesized using ceric ion-induced redox initiation technique. In the first series, a variation of ceric ion concentration at fixed acrylamide concentration and in the second series, a variation of acrylamide concentration at fixed ceric ion concentration were undertaken to effect a variation in the number and length of polyacrylamide chains. Qualitatively, it has been observed that there may be some homopolymers formed at a very high acrylamide concentration. The products may at best be a mixture of graft copolymer and homopolymer, but it contradicts the view that the products are purely physical mixtures of polysaccharide and polyacrylamide. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 70: 2627–2633, 1998     

Preparation and characterization of a new coagulant based on the sago starch biopolymer and its application in water turbidity removal

A new organic coagulant, sago starch (SS)‐graft‐polyacrylamide (PAm), was prepared by the ceric‐ion‐induced redox polymerization of acrylamide (Am) onto SS at room temperature. The effects of the variation of the concentration of Am and the initiator on the percentages of yield and total conversion were investigated. The chemical composition, viscosity, and side‐chain‐average molecular weight of the obtained graft copolymers were determined. The newly obtained coagulant was tested for the treatment of the turbidity of water. The SS‐g‐PAm coagulants were found to achieve water turbidity removal up to 96.6%. The results of this study suggest that SS‐g‐PAm copolymer is a potential coagulant for reducing turbidity during water treatment. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Characterization of the collagen–vinyl graft copolymers prepared by the ceric ion method. II. Infrared spectra and electron microscopy

Collagen powder and goat skins were grafted with different vinyl monomers using the ceric ion technique. The graft copolymers were characterized by infrared spectra and electron microscopy. The collagen–vinyl graft copolymers were hydrolyzed by both acid and enzymatic hydrolysis, and the grafted vinyl polymer side chains were isolated. In the grafted poly(methyl methacrylate) (PMMA) side chains isolated by acid hydrolysis, the characteristic amide absorption bands at 1550 and 1660 cm^?1 were not seen prominently. However, in PMMA side chains isolated by enzymatic methods, the amide absorption bands were more prominent as these isolated side chain polymers contained longer fragments of the peptide backbone attached to them. Electron-microscopic observations of grafted collagen fibrils and ultrathin sections of grafted goat skin fibrils did not show any cross-striations. These various evidences indicate that the polymers formed on collagen have penetrated into the fibrils and that they were chemically bound to the collagen molecules.     

Preparation of ultra‐high‐molecular‐weight polyacrylamide by vertical solution polymerization technique

A straightforward and novel methodology has been developed for the synthesis of ultra‐high‐molecular weight polyacrylamide (PAM) by vertical solution polymerization technique. By varying the concentrations of acrylamide monomer, three different grades of polymers (PAM‐V₁, PAM‐V₂, and PAM‐V₃) have been synthesized and compared with the series of different grades of PAM (PAM‐C₁, PAM‐C₂, and PAM‐C₃) synthesized through conventional solution polymerization technique. The synthesized grades PAM‐V₁, PAM‐V₂, PAM‐V₃, PAM‐C₁, PAM‐C₂, and PAM‐C₃ have been characterized by ¹H NMR, infrared spectroscopy, intrinsic viscosity measurement, molecular weight determination by gel permeation chromatography, and thermal analysis. Rheological analysis has been carried out on the aqueous solutions of various grades of PAMs. Swelling behavior of ultra‐high‐molecular weight PAMs has also been investigated. The flocculation performances of all grades have been investigated in kaolin suspension by settling and jar test methods. POLYM. ENG. SCI., 59:1175–1181 2019. © 2019 Society of Plastics Engineers     

Starch–acrylics graft copolymers and blends: Synthesis,characterization, and applications as matrix for drug delivery

A series of acrylic monomers–starch graft copolymers were prepared by ceric ion initiation method by varying the amount of monomers. These graft copolymers were characterized by IR and ¹³C‐NMR spectroscopy. It was seen that as the concentration of monomer [acrylic acid (AA), methacrylic acid (MA), and methyl methacrylate (MMA)] increased the percent add‐on increased in all the graft copolymers, whereas grafting efficiency increased initially but showed a slight decrease with further increase in the monomer concentration (except for MMA). The release rate of paracetamol as a model drug from graft copolymers as well as their blends was studied at two different pH, 1.2 and 7.4, spectrophotometrically. The release of paracetamol in phosphate buffer solution at pH 1.2 was insignificant in the first 3 h for St‐g‐PAA‐ and St‐g‐PMA‐graft copolymers, which was attributed to the matrix compaction and stabilization through hydrogen bonding at lower pH. At pH 7.4, the release rate was seen to decrease with increase in add‐on. The tablet containing poly(methyl methacrylate) (PMMA) did not disintegrate at the end of 30–32 h, which may be attributed to the hydrophobic nature of PMMA. These results indicate that the graft copolymers may be useful to overcome the harsh environment of the stomach and can be used as excipients in colon‐targeting matrices. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

An investigation of the flocculation characteristics of polyacrylamide‐grafted chitosan

To investigate the flocculation characteristics of polyacrylamide (PAM)‐grafted chitosan, a series of PAM‐grafted chitosan copolymer (Chito‐g‐PAM1 to Chito‐g‐PAM4) have been synthesized by ceric ammonium nitrate‐induced solution polymerization technique in nitrogen atmosphere. The flocculation characteristics of the polymer samples (PAM, grafted and ungrafted chitosan) were studied by settling test and jar test methods in the colloidal suspensions of kaolin, iron ore, silica, and bentonite powder. It was found that the settling performance of Chito‐g‐PAM3 is best among the polymer samples. The jar test results indicate that the ungrafted chitosan has better water clarifying performance than both the PAM and grafted chitosan. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis and characterization of butyl acrylate graft sodium salt of partially carboxymethylated starch

Graft copolymers were synthesized by graft copolymerization of butyl acrylate (BA) onto sodium salt of partially carboxymethylated starch (Na‐PCMS). Ceric ammonium nitrate (CAN), a redox initiator, was used for initiation of graft copolymerization reaction. All the experiments were run with Na‐PCMS having degree of substitution, DS = 0.35. The grafting reaction was characterized by parameters such as % total conversion (%Ct), % grafting (%G), % grafting efficiency (%GE), and % add‐on. Graft copolymers were characterized by infrared spectral analysis and scanning electron microscopy. Variables affecting graft copolymerization reaction such as nitric acid concentration, reaction time, reaction temperature, and ceric ion concentration were investigated. The results revealed that 0.3M CAN as initiator, 0.3M HNO₃, with reaction time 4–4.5 h at 25–30°C were found as suitable parameters for maximum yield of graft copolymerization reaction. © 2006 Wiley Periodicals, Inc. JAppl Polym Sci 102: 3334–3340, 2006     

Phase behavior of temperature‐ and pH‐sensitive poly(acrylic acid‐g‐N‐isopropylacrylamide) in dilute aqueous solution

Several different composition temperature‐ and pH‐sensitive poly(acrylic acid‐g‐N‐isopropylacrylamide) (P(AA‐g‐NIPAM)) graft copolymers were synthesized by free‐radical copolymerization utilizing macromonomer technique. The phase behavior and conformation change of P(AA‐g‐NIPAM) in aqueous solutions were investigated by UV–vis transmittance measurements, fluorescence probe, and fluorescence quenching techniques. The results demonstrate that the P(AA‐g‐NIPAM) copolymers have temperature‐ and pH‐sensitivities, and these different composition graft copolymers have different lower critical solution temperature (LCST) and critical phase transition pH values. The LCST of graft copolymer decreases with increasing PNIPAM content, and the critical phase transition pH value increases with increasing Poly(N‐isopropylacrylamide) (PNIPAM) content. At room temperature (20°C), different composition of P(AA‐g‐NIPAM) graft copolymers in dilute aqueous solutions (0.001 wt %) have a loose conformation, and there is no hydrophobic microdomain formation within researching pH range (pH 3 ～ 10). In addition, for the P(AA‐g‐NIPAM) aqueous solutions, transition from coil to globular is an incomplete reversible process in heating and cooling cycles. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008