Graft copolymerization and characterization of 2‐hydroxyethyl methacrylate onto jute fiber by photoirradiation

UV radiation induced graft copolymerization of 2‐hydroxyethyl methacrylate onto natural lignocellulose (jute) fiber was carried out by two methods: simultaneous irradiation and grafting and preirradiation grafting. 1‐Hydroxycyclohexyl‐phenylketone was used as the photoinitiator in both methods. In the former method, the variation of the graft weight was measured for different values of radiation exposure time and the concentrations of both the monomer and photoinitiator. The latter method produced up to 76% graft weight compared to 45% obtained with the former method. The preirradiation method offers better control of the homopolymerization reaction compared to that afforded by the other method. The optimum value of the reaction parameters on the graft weight was evaluated. The mechanical properties of grafted samples were found to be drastically different from those of the as‐received ones and the effect was proportional to the percentage of graft weight. Differential scanning calorimetry studies showed that the percentage of graft add‐on of hydroxyethyl methacrylate with jute had a significant effect on the thermal properties. IR studies indicated the degree of grafting could be estimated by correlating the band intensities with the graft weight. The jute samples grafted with poly(hydroxyethyl methacrylate) at a level of 12% graft weight exhibited a maximum 20% increase in hydrophilicity. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2898–2910, 2006     

Surface graft copolymerization of 2‐hydroxyethyl methacrylate onto low‐density polyethylene film through corona discharge in air

The corona discharge technique was explored as a means of forming chemically active sites on a low‐density polyethylene (LDPE) film surface. The active species thus prepared at atmospheric pressure in air was exploited to subsequently induce copolymerization of 2‐hydroxyethyl methacrylate (HEMA) onto LDPE film in aqueous solution. The results showed that with the corona discharge voltage, reaction temperature, and inhibitor concentration in the reaction solution the grafting degree increased to a maximum and then decreased. As the corona discharge time, reaction time, and HEMA concentration in the reaction solution increased, the grafting degree increased. With reaction conditions of a 5 vol % HEMA concentration, 50°C copolymerization temperature, and a 2.0‐h reaction time, the degree of grafting of the LDPE film reached a high value of 158.0 μg/cm² after treatment for 72 s with a 15‐kV voltage at 50 Hz. Some characteristic peaks of the grafted LDPE came into view at 1719 cm^?1 on attenuated total reflectance IR spectra (C?O in ester groups) and at 531 eV on electron spectroscopy for chemical analysis (ESCA) spectra (O_1s). The C_1s core level ESCA spectrum of HEMA‐grafted LDPE showed two strong peaks at ～286.6 eV (? C ? O? from hydroxyl groups and ester groups) and ～289.1 eV (O?C ? O? from ester groups), and the C atom ratio in the ? C? O? groups and O?C? O groups was 2:1. The hydrophilicity of the grafted LDPE film was remarkably improved compared to that of the ungrafted LDPE film. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 2881–2887, 2001     

Surface modification of polymethyl methacrylate intraocular lenses with the mixture of acrylic acid and acrylamide via plasma‐induced graft copolymerization

An approach is presented for the graft copolymerization of acrylic acid (AAc) and acrylamide (AAm) mixture onto the surfaces of polymethyl methacrylate intraocular lenses (PMMA IOLs) treated with an Argon gas plasma, followed by the exposure to the oxygen atmosphere. In this case, peroxides formed by the plasma treatment are likely to be responsible for initiating the graft copolymerization. The amount of peroxides on the surface of PMMA IOLs was determined using 1,1‐diphenyl‐2‐picrylhydrazyl, and the maximum amount was found with the plasma treatment at 30 W for 20 s under 5 mTorr pressure. The surfaces of the grafted PMMA IOLs were characterized using Fourier transform infrared spectroscopy‐attenuated total reflectance (FTIR‐ATR), electron spectroscopy for chemical analysis, and contact angle meter. The FTIR‐ATR spectrum of PMMA‐g‐AAc‐AAm showed the characteristic band of PAAc at 1580 cm^?1 together with those of PAAm at 1670 and 1630 cm^?1, confirming that the copolymer of AAc and AAm was successfully grafted onto the surfaces of PMMA IOLs. The experimental data of O1s/C1s and N1s/C1s reasonably concurred with the calculated data, a strong indication that the pH value of the reaction medium at 3.77 could produce a graft with an equal molar ratio. Surface tension of the samples increased to 52 dyn/cm due to the graft of the hydrophilic monomers. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 2361–2366, 2002     

UV‐radiation‐induced preirradiation graft copolymerization of methacrylic acid and acrylic acid onto jute fibre

UV‐radiation‐induced graft copolymerization of methacrylic acid and acrylic acid onto jute fibre was carried out using a preirradiation method with 1‐hydroxycyclohexyl‐phenylketone as a photoinitiator. 2‐methyl‐2‐propene 1‐sulfonic acid, sodium salt was incorporated into the grafting solution in suppressing the homopolymer/gel formation and facilitating graft copolymerization. In comparison, results showed that the type of monomer significantly influence on grafting. The results of the characterisation showed that the graft weight and the type of monomer have significant influence on the mechanical and water absorption properties in the case of grafted samples. Copyright © 2004 Society of Chemical Industry     

等规聚丙烯-丙烯酸接枝共聚

详细研究了等规聚丙烯细粒子在丙烯酸水溶液中,以过氧化苯甲酰为引发剂的液－固相接枝共聚反应和十氢化萘乙醇溶液对等规聚丙烯的膨化预处理作用,检测了等规聚丙烯－聚丙烯酸的某些性质,发现随接枝率提高,其吸湿性和碱性染料染色性均提高,熔点略有降低,但熔体流动性下降,按本研究获得的最佳膨化预处理条件和最佳接枝共聚反应条件,接枝产物等规聚丙烯－聚丙烯酸的接枝率可超过13％。     

用低温等离子体诱导PET织物接枝丙烯酸

运用氧气等离子体表面改性技术对PET织物进行处理后接枝丙烯酸,探讨了处理时放电功率、单体浓度、反应温度、处理时间等对接枝率的影响,并对接枝率与织物的吸湿性进行了研究。     

羟乙基纤维素与丙烯酸-2-羟基丙酯的反应规律

以硝酸铈铵/乙二胺四乙酸(CAN/EDTA)为引发剂,研究了羟乙基纤维素(HEC)与丙烯酸-2-羟基丙酯(HPA)的接枝共聚反应,讨论了单体浓度、引发剂浓度、反应温度、反应时间等因素对接枝率的影响,试验结果表明:在引发剂CAN和EDTA为22mmol/L,单体HPA为0.31mol/L,反应温度为40℃,反应时间为4h时,接枝率和接枝效率值最佳,并用红外光谱对接枝共聚物结构进行了鉴定。     

Graft copolymerization of acrylic acid onto guar gum

The graft copolymerization of acrylic acid (AA) onto guar gum (GOH) was carried out by a peroxydiphosphate (PDP)–silver(I) system. Grafting ratio, efficiency, add‐on, and conversion increase upon increasing the concentration of PDP and acrylic acid, whereas they decrease upon increasing the concentration of guar gum. Upon increasing the concentration of silver and hydrogen ions up to 2.0 × 10⁻³ and 4.87 × 10⁻² mol dm⁻³, respectively, the grafting ratio and efficiency increase but decrease upon further increasing the concentration. The increase in temperature from 30 to 45°C increases the grafting ratio but the conversion efficiency decreases. The optimum time period for graft copolymerization was found to be 2 h. The graft copolymers were characterized by infrared spectroscopy and thermogravimetric analysis. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 39–44, 2000     

Graft polymerization of acrylic acid onto polyphenylene sulfide nonwoven initiated by low temperature plasma

Graft copolymerization of acrylic acid (AA) onto polyphenylene sulfide (PPS) nonwoven initiated by low temperature plasma was studied. The effects of various conditions on graft reaction and the grafting rate were investigated. SEM images showed that PPS nonwoven was grafted, and the graft copolymerization only occurred on the surface of PPS. It may be due to the chain transference going with the graft copolymerization. It was found that with the increasing of plasma power, treatment time, space between electrodes, monomer concentration, and temperature of graft polymerization, the grafting rate increased at first, went to the top, and then decreased. The PPS nonwoven surface graft reaction could be optimized by the following processing conditions: 120 s of plasma treatment time, 50 W of plasma power, 1.5 cm of space between electrodes, 30% (w/w) of monomer concentration, and 50°C of temperature of graft polymerization. Measurement of XPS showed that the peak of C1s of graft polyacrylic acid was existed, and the peak area increased with the increase of the grafting rate. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5884–5889, 2006     

麦秸秆纤维素与丙烯酸接枝共聚制备耐盐性吸水树脂的研究

应用小麦秸秆与丙烯酸接枝共聚制备了耐盐性吸水树脂,进行了结构表征,研究了单体配比、丙烯酸中和度、引发剂和交联剂用量以及反应温度对吸盐水倍率的影响。研究发现,接枝共聚的适宜条件为:丙烯酸单体与麦秸秆质量比为8∶1,丙烯酸中和度为70%,引发剂过硫酸钾-硫代硫酸钠的用量为单体的3.5%,交联剂N,N-亚甲基双丙烯酰胺用量为单体质量的0.24%,反应温度为70℃。在此条件下制备的树脂吸盐水倍率最高,吸盐水(CNaC l=0.9%)可达68 g/g,可应用于医疗卫生等方面。     

Kinetic behaviour of styrene–2‐hydroxyethyl methacrylate copolymerisation in microemulsion

The copolymerisation of styrene and 2‐hydroxyethyl methacrylate (2‐HEMA) in a three‐component oil‐in‐water microemulsion containing sodium dodecylsulfate as emulsifier was investigated as a function of temperature and concentration of potassium persulfate or hydrogen peroxide/ascorbic acid as initiator. Stable and transparent poly(styrene–2‐HEMA) latexes were produced. The latexes were characterised for particle size and number of particles by dynamic light scattering and transmission electron microscopy. The isolated products were characterised by ¹H NMR as well as by thermal analysis. The overall size of particles was observed to be in the range 22–38 nm. Attempts are made to examine the suitability of the existing mathematical models for homopolymerisation to account for the copolymerisation of styrene and 2‐HEMA. © 2002 Society of Chemical Industry     

Plasma‐induced graft polymerization of acrylic acid onto poly(ethylene terephthalate) films

The graft polymerization of acrylic acid was carried out onto poly(ethylene terephthalate) films that had been pretreated with argon plasma and subsequently exposed to oxygen to create peroxides. The influence of synthesis conditions, such as plasma treatment time, plasma power, monomer concentration, temperature, and the presence of Mohr's salt, on the degree of grafting was investigated. The observed initial increase in grafting with monomer concentration accelerated at about 20% monomer. The grafting reached a maximum at 40% monomer and subsequently decreased with further increases in monomer concentration. The reaction temperature had a pronounced effect on the degree of grafting. The initial rate of grafting increased with increasing temperature, but the degree of grafting showed a maximum at 50°C. The activation energy of the grafting obtained from an Arrhenius plot was 29.1 kJ/mol. The addition of Mohr's salt to the reaction medium not only led to a homopolymer‐free grafting reaction but also diminished the degree of grafting. The degree of grafting increased with increasing plasma power and plasma treatment time. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 2993–3001, 2001     

Graft copolymerization of mixtures of acrylic acid and acrylamide onto polypropylene film

Liquid phase ultraviolet irradiation in the presence of benzophenone as a photosensitizer and barium hydroxide as a pH controller were used to graft the mixtures of acrylic acid and acrylamide to a polypropylene surface. The surface of the grafted polypropylene samples were characterized by Fourier transform infrared spectroscopy‐attenuated total reflectance, electron spectroscopy for chemical analysis, scanning electron microscopy, and a contact angle meter. The pH value of the reaction medium that produced the graft with equal molar ratio was found to be ∼ 3.77. The optimal reaction condition was found at a monomer feed of 25%, a reaction time of 30 min, and a benzophenone concentration of 1%. Surface tension of the samples increased to a value of 40 dyn cm⁻¹ due to the graft of the hydrophilic monomers. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 251–256, 1999     

Graft copolymerization of acrylic acid onto polystyrene using the solid phase grafting technique

Graft copolymerization of acrylic acid (AAc) onto polystyrene (PS) by the solid phase graft copolymerization technique was studied. Benzoyl peroxide (BPO) was used as the free radical initiator. Acrylic acid was introduced into the reactor as an aqueous solution. Optimum reaction conditions to obtain maximum grafting were evaluated. The variables studied were temperature, initiator concentration, monomer concentration, acrylic acid-to-water ratio, and reaction time. The graft copolymer was characterized by infrared (IR) spectroscopy, and the graft level was quantified by the IR absorbance ratio technique and titration. © 1998 John Wiley & Sons, Inc. J. Appl. Polym. Sci. 70: 1001–1007, 1998     

羧甲基甲壳素接枝甲基丙烯酸甲酯的制备及成膜性

通过高速搅拌,未使用乳化剂,制备了羧甲基甲壳素和甲基丙烯酸甲酯的接枝共聚物,避免了产物中引入乳化剂杂质。利用红外光谱对接枝共聚物进行了表征。考察了不同接枝率的产物在12种常见溶剂中的溶解性,结果表明,不同接枝率的接枝共聚物都有良好的水溶性,可以形成无色透明的膜,扩大了其实际应用价值。     

New 2‐hydroxyethyl methacrylate resins with good swelling characteristics

2‐Hydroxyethyl methacrylate copolymers with styrene and series of the cross‐linkers (divinylbenzene and mono‐, di‐ and triethylene glycol dimethacrylates) with low cross‐linking degree (2–5 mol %) were obtained by suspension polymerization. Loading capacity of the resins, their glass transition temperature, and swelling characteristics in 20 solvents were analyzed depending on monomers composition. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 1487–1493, 2006     

Plasma induced graft polymerization of acrylic acid onto polypropylene monofilament

Plasma induced graft polymerization of acrylic acid onto polypropylene (PP) monofilament was carried to introduce carboxyl functionality on its surface. The monofilament was treated with oxygen plasma to create hydroperoxide groups and subsequent graft polymerization was initiated on this exposed monofilament. It was observed that in the absence of an added inhibitor, the grafting did not proceed because of the extensive homopolymerization which left behind hardly any monomer for the grafting reaction. The addition of ferrous sulfate to the grafting medium led to the homopolymer free grafting reaction. The addition of organics, such as methanol, butanone, and acetone led to complete inhibition of the homopolymerization at 60% content. However, the addition of butanone led to much lower degree of grafting than methanol and acetone. The contact angle of the monofilament showed drastic reduction by plasma treatment and by the subsequent grafting of acrylic acid. The grafting in ferrous sulfate medium showed higher contact angles as compared to the grafting in organic medium. The surface morphology was significantly influenced by the nature of the additive in the grafting medium. © 2007 Wiley Periodicals, Inc. JAppl Polym Sci, 2008     

Surface modification of polytetrafluoroethylene films by plasma pretreatment and graft copolymerization to improve their adhesion to bismaleimide

BACKGROUND: Polytetrafluoroethylene (PTFE) is utilized in many engineering applications, but its poor wettability and adhesion properties with other materials have limited its use. The study reported was aimed at achieving surface modification of PTFE films by radiofrequency NH₃ and N₂ plasma treatment, followed by graft copolymerization, in order to improve the interfacial adhesion of PTFE and bismaleimide. RESULTS: X‐ray photoelectron spectroscopy results showed that a short‐time plasma treatment had a distinct defluorination effect and led to nitrogen functional group formation. The nitrogen chemical bonding form was different for NH₃ and N₂ plasma treatments. Under the same experimental conditions, the NH₃ plasma exhibited a better etching effect than did the N₂ plasma. Contact angle measurement showed an improvement in both surface energy and wettabliity by short‐time plasma treatment. The concentration of the surface‐grafted bismaleimide on PTFE increased after the plasma pretreatment. The lap shear strength between PTFE and bismaleimide increased significantly after surface modification. CONCLUSION: This study found that plasma treatment caused changes in surface chemistry, thus leading to an increase of the wettability of PTFE surfaces. Hence, the adhesion properties of PTFE with bismaleimide were significantly improved. Copyright © 2008 Society of Chemical Industry     

氯丁橡胶/苯乙烯/甲基丙烯酸甲酯/丙烯酸接枝共聚物的合成

以苯乙烯(St)、甲基丙烯酸甲酯(MMA)、丙烯酸(AA)为接枝单体,以过氧化二苯甲酰(BPO)为引发剂,在氯丁橡胶(CR)上进行接枝共聚,制备出CR／St／MMA／AA四元接枝共聚物。用红外光谱(IR)和差热分析(DSC)对接枝共聚物进行了表征,探讨了提取剂和提取时间对四元接枝共聚物的接枝率测定的影响,并讨论了St／MMA质量比、AA用量对接枝率和单体转化率的影响。结果表明,选用丙酮作提取剂。提取时间为48h,能达到最佳的萃取效果;BPO质量分数为CR的1．3％～1.6％。CR／St/MMA／AA四元接枝共聚物的质量比为100／30／30／15时,其接枝率和单体转化率最佳;与CR相比,四元接枝共聚物的结晶性降低,极性增强。     

Surface graft copolymerization of acrylic acid onto corona-treated poly(ethylene terephthalate) fabric

Acrylic acid (AA) was grafted onto the surface of poly(ethylene terephthalate) (PET) fabric after having short-time corona-discharge treatment (CDT) in an atmosphere in the presence of the initiator. The effect of N,N-dimethylformamide (DMF) pretreatment time, CDT time, graft copolymerization time and temperature, concentration of AA, and the content of initiator on graft yield of PET fabric was discussed. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 1161–1164, 1999