Synthesis and properties of carboxymethyl cellulose‐graft‐poly(acrylic acid‐co‐acrylamide) as a novel cellulose‐based superabsorbent

A new cellulose‐based superabsorbent polymer, carboxymethyl cellulose‐graft‐poly(acrylic acid‐co‐acrylamide), was prepared by the free‐radical grafting solution polymerization of acrylic acid (AA) and acrylamide (AM) monomers onto carboxymethyl cellulose (CMC) in the presence of N,N′‐methylenebisacrylamide as a crosslinker with a redox couple of potassium persulfate and sodium metabisulfite as an initiator. The influences of reaction variables such as the initiator content, crosslinker content, bath temperature, molar ratio of AA to AM, and weight ratio of the monomers to CMC on the water absorbency of the carboxymethylcellulose‐graft‐poly(acrylic acid‐co‐acrylamide) copolymer were investigated. The copolymer's structures were characterized with Fourier transform infrared spectroscopy. The optimum reaction conditions were obtained as follows: the bath temperature was 50°C; the molar ratio of AA to AM was 3 : 1; the mass ratio of the monomers to CMC was 4 : 1; and the weight percentages of the crosslinker and initiator with respect to the monomers were 0.75 and 1%, respectively. The maximum water absorbency of the optimized product was 920 g/g for distilled water and 85 g/g for a 0.9 wt % aqueous NaCl solution. In addition, the superabsorbent possessed good water retention and salt resistance. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 1382–1388, 2007     

Preparation and swelling behaviors of a high temperature resistant superabsorbent using tetraallylammonium chloride as crosslinking agent

A new high temperature resistant superabsorbent was synthesized through solution polymerization of acrylamide (AM) and partially neutralized acrylic acid (AA), using tetraallylammonium chloride (TAAC) as crosslinker, ammonium persulfate (APS) as initiator. Parameters that influence water absorbency of the superabsorbent at 25 °C and 200 °C such as molar ratios of AM to AA, TAAC to AA, APS to AA and neutralization degree, were investigated. Swelling behaviors of superabsorbent prepared at the optimum conditions in different pH and saline solutions were studied. The swelling ratios of superabsorbent in distilled water and 1 wt% NaCl solution at 250 °C reach 287 g/g and 69 g/g, respectively.     

Studies on poly(acrylic acid)/attapulgite superabsorbent composite. I. Synthesis and characterization

A novel poly(acrylic acid)/attapulgite superabsorbent composite was synthesized by graft copolymerization reaction of acrylic acid (AA) on attapulgite micropowder using N,N′‐methylenebisacrylamide (MBA) as a crosslinker and ammonium persulfate (APS) as an initiator in aqueous solution. The effects on water absorbency of such factors as reaction temperature, initial monomer concentration, degree of neutralization of AA, amount of crosslinker, initiator, and attapulgite were investigated. These crosslinked superabsorbent composites were characterized by thermogravimetetric analysis and scanning electron microscopy. The graft copolymerization reaction of AA on attapulgite micropowder was characterized by FTIR. The water absorbencies for these superabsorbent composites in water and saline solutions were investigated and water‐retention tests were carried out. Results obtained from this study show that the water absorbency of the superabsorbent composite synthesized under optimal synthesis conditions with an attapulgite content of 10% exhibited an absorption of 1017 g H₂O/g sample and 77 g H₂O/g sample in distilled water and in 0.9 wt % NaCl solution, respectively. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 1596–1603, 2004     

Synthesis,characterization and swelling behaviors of hydroxyethyl cellulose‐g‐poly(acrylic acid)/attapulgite superabsorbent composite

In this work, a series of novel hydroxyethyl cellulose‐ g‐poly(acrylic acid)/attapulgite (HEC‐g‐PAA/APT) superabsorbent composites were prepared through the graft polymerization of hydroxyethyl cellulose (HEC), partially neutralized acrylic acid (AA), and attapulgite (APT) in aqueous solution, and the composites were characterized by means of Fourier‐transform spectroscopy, scanning electron microscopy, and transmission electronmicroscopy. The effects of polymerization variables including concentrations of the initiator and crosslinker and APT content on water absorbency were studied, and the swelling properties in various pH solutions as well as the swelling kinetics in various saline solutions were also systematically evaluated. Results showed that the introduction of 5 wt% APT into HEC‐g‐PAA polymeric network could improve both water absorbency and water absorption rate of the superabsorbent composites. In addition, the superabsorbent composites retained high water absorbency over a wide pH range of 4–10, and the swelling kinetics of the superabsorbent composites in CaCl₂ and FeCl₃ solutions exhibited a remarkable overshooting phenomenon. POLYM. ENG. SCI., 2010. © 2010 Society of Plastics Engineers     

Synthesis of poly(acrylic acid)/sodium humate superabsorbent composite for agricultural use

A novel poly (acrylic acid)/sodium humate superabsorbent composite was synthesized by graft copolymerization reaction of acrylic acid (AA) on sodium humate micropowder using N,N′‐methylenebisacrylamide (MBA) as a crosslinker and potassium peroxydisulfate (KPS) as an initiator in aqueous solution. The effects on water absorbency of factors such as reaction temperature, initial monomer concentration, and degree of neutralization of AA, amount of crosslinker, initiator, and sodium humate were investigated. The superabsorbent composite was characterized by scanning electron microscopy, and the graft copolymerization reaction of AA on sodium humate micropowder was characterized by IR spectroscopy. Results obtained from this study show that the water absorbency of the superabsorbent composite synthesized under optimal conditions for synthesis with a sodium humate content of 5.3% exhibited absorption of 684 g H₂O/g sample in distilled water. Water‐retention in soil is enhanced by the use of the superabsorbent composite. The effect of superabsorbent composite on the growth of corn is reported. The superabsorbent composite may be of use as water management materials for agriculture purposes in desert and drought‐prone areas. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5137–5143, 2006     

Utilization of starch and montmorrilonite for the preparation of superabsorbent nanocomposite

Starch and montmorrilonite (MMT) were used as raw materials for synthesizing starch‐graft‐poly[acrylamide (AM)–acrylic acid (AA)]/MMT superabsorbent nanocomposite by graft and intercalation copolymerization reaction of starch, AM, and AA in the presence of organic MMT micropowder in aqueous solution. Major factors affecting water absorbency such as weight ratio of monomers to starch, weight ratio of AM to AA, neutralization degree of AA, amount of crosslinker, initiator, and MMT were investigated. The superabsorbent nanocomposite synthesized under optimal synthesis conditions exhibits absorption of 1120 g H₂O/g sample and 128 g H₂O/g sample in deionized water and in 0.9 wt % NaCl solution, respectively. IR spectra showed that the graft copolymerization between  OH groups on MMT and monomers took place during the reaction, and that crystal interlayer was pulled open in the superabsorbent nanocomposite. X‐ray diffraction analysis showed that the crystal interlayer of MMT was pulled open to 2.73 nm, and thus formed nanometer exfoliation composite material. Thermogravimetric analysis showed that starch‐graft‐poly (AM–AA) superabsorbent nanocomposite (8 wt % MMT) has good thermal stability. This superabsorbent nanocomposite with excellent water absorbency and water retention, being biodegradable in nature, economical and environment friendly, could be especially useful in industry, agricultural, and horticultural applications. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

A novel polyacrylamide‐based superabsorbent with temperature switch for steam breakthrough blockage

A novel high‐temperature resistant superabsorbent polymer (SAP) with a temperature switch to control its water absorbency was prepared through solution polymerization of acrylamide (AM), using N,N‐methylenebisacrylamide (NMBA) and tetraallylammonium chloride (TAAC) as crosslinking agents. The SAPs were structurally characterized by Fourier transform infrared (FTIR) spectroscopy and energy dispersive X‐ray spectroscopy (EDX). The factors that influence the water absorbency such as total crosslinker concentration, molar ratio of NMBA to TAAC and temperature were investigated. The SAP with optimized crosslinker concentration showed a swelling ratio less than 10 g/g at 25°C, and drastically enhanced water absorption capacity (190 g/g) at 300°C. The water absorption characteristics can be tuned by varying the temperature. Swelling experimental results combined with crosslinking density study and morphology observation by scanning electron microscopy (SEM) clearly demonstrated that the hydrolysis of amide bonds on NMBA played a critical role in creating these previously unreported SAPs, and that the use of TAAC with an appropriate amount rendered the SAPs high‐temperature resistance. This kind of SAPs has high application potentials as plugging material for steam breakthrough and channeling in heavy oil reservoirs. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42067.     

Preparation of starch‐graft‐poly(acrylamide)/attapulgite superabsorbent composite

A novel starch‐graft‐poly(acrylamide)/attapulgite superabsorbent composite was synthesized by graft copolymerization reaction of starch, acrylamide (AM), and attapulgite micropowder using N.N‐methylene‐bisacrylamide (MBA) as a crosslinker and ammonium persulphate (APS) as an initiator in aqueous solution, followed by hydrolysis with sodium hydroxide. The effects on water absorbency, such as amount of crosslinker, initiator, attapulgite, weight ratio of acrylamide to starch in the feed, gelatinization conditions of starch and molar ratio of NaOH to acrylamide, and so forth, were investigated. These superabsorbent composites were characterized by Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). The water absorbencies for these superabsorbent composites in water and saline solution were investigated, and water retention tests were carried out. Results obtained from this study showed that the water absorbency of superabsorbent composite synthesized under optimal synthesis conditions with an attapulgite content of 10% exhibit absorption of 1317 g H₂O/g sample and 68 g H₂O/g sample in distilled water and in 0.9 wt % NaCl solution, respectively. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 1351–1357, 2005     

Microwave irradiation copolymerization of superabsorbents from cornstarch and sodium acrylate

Sodium acrylate was grafted onto cornstarch by microwave irradiation to synthesize a superabsorbent, in which potassium persulfate (PPS) was used as the initiator and polyethyleneglycol diacrylate as the crosslinker. It was found that microwave irradiation could substantially accelerate the synthesis, without the need to remove O₂ or inhibitor. Catalyzed by p‐toluene sulfonic acid, polyethyleneglycol was esterified with acrylate to synthesize the crosslinker. An orthogonal test of L₉(3⁴) was designed to study the effects of relevant factors on absorbency and yield of products, including microwave power, irradiation time, initiator amount, and crosslinker content. Microwave power was believed to be the most significant factor affecting the swelling ratio and solubility of the product. Optimized experimental results showed that 10 min of microwave irradiation at 85–90 W could produce a cornstarch‐based superabsorbent with a swelling ratio of 520–620 g/g in distilled water and solubility of 8.5–9.5 wt %. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 95: 264–269, 2005     

Utilization of waste polystyrene and starch for superabsorbent composite preparation

A superabsorbent composed of waste polystyrene, starch, and acrylic acid was prepared through emulsion polymerization. The effects of major factors such as starch, acrylic acid, initiator, crosslinker, and bentonite contents and the neutralization degree of acrylic acid on water absorbency were investigated to obtain optimum conditions with high swelling capacity. The superabsorbent hydrogel was characterized by scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectroscopy, and thermogravimetric analysis (TGA). The FTIR results confirmed that the grafting polymerization took place among the polystyrene, acrylic acid, starch, and bentonite. The introduction of bentonite particles into the polystyrene‐g‐poly (acrylic acid)‐co‐starch system could increase the water absorbency. The superabsorbent composite containing 3 wt % bentonite had the highest water absorbency (500 g/g in distilled water and 49 g/g in 0.9 wt % NaCl solution). © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation of acrylic acid and AMPS cointercalated layered double hydroxide and its application for superabsorbent

This article reports the cointercalation of acrylic acid (AA) and 2‐acrylamido‐2‐methylpropane sulfonic acid (AMPS) in the interlayer region of Mg₂Al layered double hydroxide (LDH) and the application of this inorganic–organic composite material in the field of water superabsorbent. The monomers of AA and AMPS were cointercalated into galleries of Mg₂Al−LDH (denoted as AA−AMPS/LDH) with various molar ratios by ion‐exchange method, which was confirmed by powder X‐ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), and elemental analysis. The polymer‐based superabsorbent was prepared through in situ free‐radical aqueous copolymerization of AA and AMPS, with AA−AMPS/LDH as additive, N,N′‐methylenebisacrylamide (NMBA) as crosslinker and potassium persulfate (KPS) as initiator. The composition of this poly(AA‐co‐AMPS)/LDH was demonstrated as a good water superabsorbent. The LDH content, water absorbency, thermal stability, and swelling rate of this superabsorbent were also investigated in detail. Results showed that the incorporation of a 5 wt % AA−AMPS/LDH into polymer matrix increased its water absorbency significantly by 27.7% (in water) and by 51.5% (in 0.9 wt % NaCl solution). © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis and properties of a superabsorbent from an ultraviolet‐irradiated waste nameko mushroom substrate and poly(acrylic acid)

To better use the waste nameko mushroom substrate (WNMS) and prevent its pollution into the environment, a novel superabsorbent polymer was synthesized via the UV irradiation copolymerization of acrylic acid and WNMS in the presence of an initiator (dimethoxy‐2‐phenylacetophenone and ammonium persulfate) and crosslinker N,N′‐methylenebisacrylamide. The factors that had an influence on the water absorbency of the superabsorbent polymer were investigated and optimized. Under the optimized conditions, WNMS–poly(acrylic acid) was obtained. Its swelling behaviors, which followed the pseudo‐second‐order swelling kinetic model, were investigated in distilled water (1701 g/g) and a 0.9 wt % NaCl solution (388 g/g). The water absorbency was 1011 g/g in a 0.1 wt % urea solution and 80% amount of urea diffused into the gels. The urea diffusion followed a Fickian diffusion mechanism. Moreover, the product showed excellent water retention capabilities under the condition of high temperature or high pressure. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40471.     

Preparation of superabsorbent based on the graft copolymerization of acrylic acid and acrylamide onto konjac glucomannan and its application in the water retention in soils

A new konjac glucomannan (KGM)-based superabsorbent polymer, KGM-g-poly(acrylic acid-co-acrylamide), was prepared by the free radical grafting solution polymerization of acrylic acid (AA) and acrylamide (AM) monomers onto KGM in the presence of N,N′-methylenebisacrylamide as a crosslinker with potassium persulfate as an initiator. The effects of reaction parameters, including the amount of crosslinking agent and initiator, the weight ratio of both (AA + AM) to KGM and AM to (AA + AM), neutralization degree of AA, bath temperature, and reaction time, on the water absorbency of the superabsorbent were investigated. The Fourier transform infrared spectroscopy was used to characterize the structures of the copolymer. The maximum water absorbency of the optimized product was 650 g/g for distilled water and 70 g/g for a 0.9 wt % aqueous NaCl solution. Furthermore, the water retention of the copolymer in soils was studied. The effect of the copolymers on the aggregate distribution of soils was also evaluated. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Collagen-g-poly(Sodium Acrylate-co-Acrylamide)/sodium montmorillonite superabsorbent nanocomposites: synthesis and swelling behavior

Nanocomposite superabsorbents were synthesized by graft copolymerization of mixture of acrylamide (AAm) and acrylic acid (AA) onto collagen using potassium persulfate (KPS) as a free radical initiator and methylenebisacrylamide (MBA) as a crosslinker. Nanoclay sodium montmorillonite (MMt) was introduced as filler into superabsorbent. The chemical structure of the Collagen-g-poly(Sodium Acrylate-co-Acrylamide)/MMt nanocomposite was characterized by means of FTIR spectroscopy, XRD patterns, and TGA thermal methods. Morphology of the sample was examined by scanning electron microscopy (SEM). The effects of reaction variables were systematically optimized to achieve a superabsorbent with swelling capacity as high as possible. Under the optimized conditions concluded, the maximum swelling capacity in distilled water was 950 g/g. Dewatering of nanocomposite and clay-free superabsorbent revealed that inclusion of nanoclay into superabsorbents can improve water retention of superabsorbent under heating. The swelling ratio in various salt solution and kinetic of dewatering was also determined and additionally, the swelling of nanocomposite superabsorbent was measured in solution with pH ranged 1–13. The synthesized nanocomposite exhibited a pH-responsive characteristic.     

Preparation of polyacrylamide/graphite oxide superabsorbent nanocomposites with salt tolerance and slow release properties

Novel polyacrylamide/graphite oxide (PAM/GO) superabsorbent nanocomposites were synthesized by a simple solution polymerization of acrylamide using N,N ′‐methylenebisacrylamide as crosslinker and ammonium persulfate as initiator. The well dispersion of GO nanoplatelets in the polymeric network results in a remarkable improvement on the comprehensive swelling performance of the resulting superabsorbent nanocomposites. The water absorption experimental results show that the superabsorbent nanocomposites could absorb water as twice as that of crosslinked polyacrylamide (PAM) superabsorbent with a weight gain of 400 g g^?1 with a low loading of GO. The salt tolerance and water‐retention ability of the resulting PAM/GO superabsorbent nanocomposites are also enhanced compared with PAM. Moreover, by embedding of ammonium salt into PAM/GO network, the PAM/GO superabsorbent nanocomposites also exhibit a slow release behavior of ammonium salt from network when swelling in water, which makes the PAM/GO superabsorbent nanocomposites multifunctional absorbent materials with great potential for agricultural and horticultural applications. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

耐盐型丙烯酸-丙烯酰胺接枝共聚高吸水树脂的合成及其性能研究

采用溶液聚合法,以丙烯酸(AA)和丙烯酰胺(AM)为单体,N,N＇-亚甲基双丙烯酰胺(NMBA)为交联剂,过硫酸钾(KPS)为引发剂.合成出丙烯酸-丙烯酰胺接枝共聚高吸水树脂.探讨了单体比[m(丙烯酸):m(丙烯酰胺)]、交联剂和引发荆用量、单体中和度及聚合温度对树脂吸水率的影响.IR光谱表明,丙烯酸和丙烯酰胺发生了接...     

Synthesis and characterization of chitosan‐graft‐poly(acrylic acid)/nontronite hydrogel composites based on a design of experiments

A 2^4–1 fractional factorial design was used to evaluate the effect of some parameters, such as the acrylic acid (AA)/chitosan (CTS) molar ratio, crosslinker concentration, initiator concentration, and filler concentration, in the swelling capacity of superabsorbent hydrogel composites based on CTS‐graft‐poly(acrylic acid) and nontronite clay. The data from wide‐angle X‐ray scattering and Fourier transform infrared spectroscopy confirmed the syntheses of the hydrogel composites. Main and interaction effects were analyzed by analysis of variance, F tests, and p values. We found that the AA/CTS and crosslinker were the most influential effects in the evaluated response. The proposed statistical model presented a high coefficient of determination (R² = 0.985). In addition to the swelling kinetics, the effects of pH and salt for the both compositions (with and without filler), which presented the best water uptake, were evaluated. Both hydrogels showed responsive behavior in relation to the pH and the salt solution, presenting good potential for application as devices in the controlled release of solutes. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Synthesis and characterization of a salt‐resisting superabsorbent based on poly(acrylic acid) with sodium tungstate as a crosslinker

A novel salt‐resistant superabsorbent polymer was synthesized by solution polymerization from the monomer acrylic acid (AA) with potassium persulfate as the initiator. Sodium tungstate was first employed as a crosslinker in the preparation to achieve a better crosslinked polymer (WPAA). In addition to the xerogel WPAA, sodium hydroxide and tris(2‐hydroxyethyl)amine (TEA) were introduced for the preparation of WPAA–sodium and WPAA–TEA hydrogels, respectively. The effect on the water absorbency of factors such as the reaction temperature, degree of neutralization of AA, and amounts of the crosslinker sodium tungstate and the initiator were investigated. The crosslinked xerogels were characterized with infrared spectroscopy. These crosslinked superabsorbent composites with sodium tungstate were characterized with thermogravimetric analysis and scanning electron microscopy. The water absorbencies of these superabsorbent composites in water and saline solutions were investigated. Results obtained from this study showed that under the same synthesis conditions, in comparison with superabsorbent composites with an aluminum salt as a crosslinker and styrene as a graft copolymer, the salt resistance of the superabsorbent composite synthesized with sodium tungstate as a crosslinker was obviously enhanced. Moreover, the WPAA–TEA xerogel had absorbency values of 223.6 and 81.9 g/g for distilled water and a 0.9 wt % NaCl solution, respectively, and it showed better salt resistance and a better water‐absorbing rate than the WPAA–sodium xerogel because of the modification with triethanolamine. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis and properties of silk sericin-<Emphasis Type="Italic">g</Emphasis>-poly(acrylic acid-co-acrylamide) superabsorbent hydrogel

A novel superabsorbent hydrogel has been synthesized with the crosslinking graft copolymerization of acrylic acid (AA) and acrylamide onto the chain of silk sericin. Potassium persulfate (KPS)–sodium sulfite (NaHSO₃) as redox initiation system and N,N′-methylenebisacrylamide (MBA) as crosslinker were used. The structure of the product characterized by Fourier transform infrared absorption spectroscopy and the surface morphology of the hydrogel were observed by scanning electron microscopy. The certain parameters of the graft copolymerization including the monomer, the initiator, the crosslinker concentration, neutralization degree of AA, reaction temperature, and time were systematically optimized to achieve a hydrogel with maximum swelling capacity (2150 g/g). The optimal conditions were initiator 8 mmol/L, MBA 2.5 mmol/L, neutralization degree of AA 75%, reaction temperature 55 °C, and time 6 h. The swelling ratio in salt solutions was also determined (in 0.9% NaCl aqueous solution: 98 g/g). In addition, the swelling capability of the hydrogel was measured in solutions with pH ranged from 1 to 13. The synthesized hydrogel exhibited a pH-dependent character. Water absorbency of the product in aqueous chloride salt solutions has the Na⁺ > Ca²⁺ > Mg²⁺ > Al³⁺ order in the investigated concentration.     

Preparation and slow‐release property of a poly(acrylic acid)/attapulgite/sodium humate superabsorbent composite

A novel poly(acrylic acid)/attapulgite (APT)/sodium humate (SH) superabsorbent composite was synthesized through the graft copolymerization reaction of acrylic acid on APT micropowder and SH with N,N′‐methylene bisacrylamide as a crosslinker and ammonium persulfate as an initiator in an aqueous solution. Various effects on the water absorbency, including the amounts of the crosslinker, initiator, APT, and SH, were investigated. The superabsorbent composite was characterized with Fourier transform infrared spectroscopy and scanning electron microscopy. The superabsorbent composite synthesized under optimal synthesis conditions with an APT concentration of 20% and an SH concentration of 20% exhibited absorption of 583 g of H₂O/g of sample and 63 g of H₂O/g of sample in distilled water and in a 0.9 wt % NaCl solution, respectively. The slow‐release property of SH from the superabsorbent composite into water was measured, and a test of the water retention of the superabsorbent composite in soil was also carried out experimentally with and without the superabsorbent composite. The results showed that the superabsorbent composite had not only good water retention but also an additional slow‐release property of SH. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 37–45, 2007