• Macromolecular Research
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• v.16 no.8
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• pp.734-740
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• 2008

A new crosslinked, poly(acrylic acid)-based, dehydrating agent was synthesized through solution polymerization. The Taguchi method, a robust experimental design, was adopted to optimize the synthetic conditions based on the moisture and water absorbing capacities of the dehydrating agent. The method applied for the experiment was a standard L27 ($3^8$) orthogonal array with eight parameters and three levels. By analyzing the variance of the test results, the most effective parameters to control the moisture absorbing capacity (MAC) and its rate were the kind of alkaline base (LiOH, NaOH, or KOH) used as a neutralizing agent of the acrylic acid monomer and the degree of neutralization: The maximum MAC of 40% was achieved at only 2 hat $32^{\circ}C$ and 50% RH when KOH was used as a base and the degree of neutralization was 90%, respectively. However, the water absorbing capacity (WAC) of the resulting dehydrating agent was very low at 158 g/g, indicating that WAC is unaffected by MAC and its rate in this system. The surface morphologies of the agents were examined using scanning electron microscopy (SEM).

• Journal of the Korean Chemical Society
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• v.53 no.3
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• pp.345-354
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• 2009

Sulfonated poly(ether sulfone)s (PESs) with a network structure were prepared by heat-induced crosslinking of the allyl-terminated telechelic sulfone polymers using a bisazide and their structure was analyzed by $^1H$ NMR. Having both uniform distribution of the hydrophilic conductive sites and controlled hydrophobic nature by minimized crosslinking, the crosslinked polymer (PES-60) membrane offered excellent proton conductivity at high temperature with a good thermal stability. In addition, selectivity of the crosslinked membrane (PES-60) was more than three times than that of Nafion$^{(R)}$.

• Textile Coloration and Finishing
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• v.24 no.4
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• pp.281-287
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• 2012

Poly(phenylene sulfide) films containing acetophenone as a photoinitiator were photocrosslinked under UV irradiation using a continuous UV irradiator. The gel fraction of the irradiated PPS in 1-Chloro naphthalene reached 94.7% with increasing UV energy and the photoinitiator concentration in the film upto $200J/cm^2$ and 12wt% respectively. Solid state $^1C$ NMR analysis suggested that the crosslinking occurred between the phenylene chains in PPS, indicating that the acetophenone may the phenylene hydrogens and subsequently adjacent polymer radicals could be recombined to form the crosslinked structure. The crosslinking improved the thermal behavior of PPS such as loss of $T_g$ and $T_c$, higher melting point and lower melting enthalphy as well as significantly higher peak pyrolysis temperature as much as $63.5^{\circ}C$. Surprisingly the tensile toughness of the most crosslinked PPS increased by 842%, resulting from the substantial enhancements in tensile modulus, strength and strain as much as 76%, 236% and 240% respectively. Also dynamic mechanical measurement indicated that the distance between crosslinks in the crosslinked PPS reached 85.3 g/mol corresponing to a crosslink density of 0.012 mol/g.

• Membrane Journal
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• v.23 no.6
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• pp.450-459
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• 2013

2,3,5,6-Tetramethyl-1,4-phenylenediamine (TMPD) based polyimide (PI) were crosslinked with 1,2-Diaminoethane (DAE) and 1,6-Diaminohexane (DAH) to enhance gas transport properties. Fourier transform infrared (FT-IR) studies show that imide groups were converted into amide groups during crosslinking process. Thermogravimetric analysis (TGA) results indicate that the degradation temperature of crosslinked PI membranes decreased after crosslinking. This is due to degradation of alkyl group in crosslinking agent. The d-space of crosslinked PI membranes decreased with increasing crosslinking time. The ideal permeability for $CH_4$, $N_2$, $O_2$, and $CO_2$ decreased after crosslinking and the ideal permeability of crosslinked PI membranes induced by DAH is larger than that by DAE. In contrast, the permselectivity of $CO_2/CH_4$, $CO_2/N_2$ and $O_2/N_2$ increased during crosslinking. For the gas pair of $CO_2/CH_4$, the maximum increment is about 39.5% after 6 minutes of DAE crosslinking. Also, that of $O_2/N_2$ gas pair is about 20.5% after 6 minutes of DAE crosslinking. According to these result, DAE is more suitable for enhanced permselectivity than DAH. On the contrary, DAE is not useful for $CO_2/N_2$ separation due to reduction in $CO_2/N_2$ permselectivity after 3 minutes DAE crosslinking.

• Polymer(Korea)
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• v.26 no.4
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• pp.523-534
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• 2002

A new hydroxypropylcellulose (HPC) capable of exhibiting reflection colours in the temperature ranges of about 60-$130^{\circ}C$ and acrylic acid esters of HPC (ESs) with degree of esterification (DE) ranging from 1 to 3 were synthesized. The crosslinked ES films with the optical pitch ($\lambda_m$) ranging throughout the visible region were also prepared by exposing thermotropic cholesteric phases of ESs with a DE of more than 2 to UV light at $50^{\circ}C$. The thermal and optical properties for both the uncrosslinked and crosslinked samples and the swelling behavior of the crosslinked films in acetone were investigated. The $\lambda_m$'s of ESs, as well as HPC itself, increased with temperature. However, the $\lambda_m$'s of ESs were larger than of HPC at the same temperature and decreased with increasing DE. The temperature dependence of $\lambda_m$of the crosslinked samples was much weaker than that of ESs. Moreover, in contrast with ESs that exhibit a decrease of the isotropization temperature with increase in the DE, the networks were found to decompose at about $210^{\circ}C$, giving no transition to an isotropic state. The crosslinked samples exhibited an anisotropic swelling, suggesting that the two-dimensional crosslinking preferentially performs between ES molecules.

• Korean Journal of Food Science and Technology
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• v.28 no.3
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• pp.580-586
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• 1996

Gelatinization behavior and morphology of epichlorohydrin-crosslinked potato starches (XPs) were investigated. Native potato starch showed a very steep single stage swlling pattern, but crosslinked starches showed various patterns with the degree of crosslinking. Swelling power, solubility and light transmittance were reduced drastically as the degree of crosslinking increased. Brabender initial pasting temperature and peak temperature of crosslinked starches increased because the crosslinking reinforces the intermolecular net work of the starches. Although the swelling of the potato starch granule was inhibited by crosslinking as compared to that of the native one, Brabender peak viscosities (6.5% w/v, db) were on the order of 2,500 units for the native potato starch, 3,700 for the XP with 2.300 anhydroglucose units per crosslinking (AGU/CL) and 3,400 for the XP with 2,100 AGU/CL, due to the decreased breakdown of the swollen granule resulting from the resistance to heat and shear. The XP with 1,900 AGU/CL, however, did not show the peak viscosity and the viscosity was on the order of 500 units because of the excessive unhibition of the swelling. Unlike the native potato starch, 6.5%(m/v, db) pastes of the crosslinked potato starches could form gels, which could be predicted from the Brabender setback and consistency index. When the degree of crosslinking is low, random contraction and radial swelling of the granule was possible. As the degree of crosslinking increased, morphological change became similar to the single dimensional tangential swelling observed from the lenticular wheat starch. These morphological change during heating in excess water explained the gelatinization behaviors of crosslinked starches tested.

• Membrane Journal
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• v.17 no.4
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• pp.311-317
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• 2007

Proton conducting crosslinked membranes have been prepared by polymer blending, which consist of poly(vinyl alcohol-co-ethylene) (PVA-co-PE) and poly(styrene sulfonic acid-co-maleic acid) (PSSA-co-PMA) at 50 : 50 wt ratio. Two kinds of PSSA-co-PMA copolymer with 3 : 1 and 1 : 1 the molar ratio of PSSA to PMA wereused as a proton conducting source. The ethylene content of PVA-co-PE was also changed as 0, 27 and 44 mol%. The membranes were thermally crosslinked via the esterification reaction between -OH of PVA and -COOH of PMA, as demonstrated by FT-IR spectroscopy (PVA-co-PE)/(PSSA-co-PMA) membranes with 3 : 1 the molar ratio of PSSA to PMA showed higher ion exchange capacity (IEC), lower water uptake and higher proton conductivity than those with 1 : 1 molar ratio. As the PE concentration increased, the IEC values, water uptake and proton conductivities decreased continuously. These properties were elucidated in terms of competitive effect between the concentration of sulfonic acid, hydrophilicity and the crosslinked structure of membranes.

• Polymer(Korea)
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• v.36 no.2
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• pp.208-215
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• 2012

To study the effect of surface crosslinked layer on the crosslinked poly(sodium acrylate) (cPSA) absorbent, we synthesized several surface crosslinked cPSAs with 5, 10 and 20 g of ethylene glycol dimethacrylate (EGDMA) by an inverse emulsion polymerization method to delay the absorption of excess water in concrete. We measured the compressive and flexural strength of mortars having 0.5, 1.0 and 1.5 wt% cPSA-EGDMA. We observed the increase of compressive and flexural strength of the cPSA-EGDMA added cement mortars except for the 0.5 wt% cPSA-EGDMA (20 g) added cement mortar. 1.0 wt% cPSA-EGDMA (5 g) added cement mortar showed about 16% and 10% increased compressive and flexural strength than those of plain cement mortar. To study the effect of porosity on compressive and flexural strength, we used FE-SEM and porosimeter. FE-SEM analysis showed swollen cPSMAEGDMA (5 g) filled between calcium silicate hydrate (C-S-H) crystals. We observed the decreased porosity of the cPSA-EGDMA added cement mortars than that of plain cement mortar. 1.0 wt% cPSA-EGDMA (5 g) cement mortar showed the lowest porosity of 16.5%.

• Polymer(Korea)
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• v.35 no.4
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• pp.363-369
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• 2011

To study the effect of incorporation of a surface crosslinking layer on a crosslinked poly (sodium acrylate) (cPSA) absorbent with ethylene glycol dimethacrylate CEGDMA), we synthesized several surface crosslinked cPSAs with EGDMA by an inverse emulsion polymerization method to delay the absorption of excess water in concrete, Liquid paraffin was used as a continuous phase. cPSA was synthesized with acrylic acid (AA) neutralized with aqueous 8 M sodium hydroxide solution as a monomer, N,N-methylene bisacrylamide (MBA) as crosslinking agent and ammonium persulfate (APS) and sodium metabisulfite (SMBS) as a redox initiator system by inverse emulsion polymerization. FTIR spectroscopy was used to characterize $Ca^{2+}$ ion interaction with cPSA and cPSA-EGDMAs. The swelling ratios of synthesized absorbents were evaluated from the absorption in deionized water, cement saturated aqueous solution and aqueous solution of calcium hydroxide (pH 12). Equilibrium swelling times for cPSA and surface crosslinked cPSA with EGDMA were 2 and 3 hrs, respectively. We also observed an increase in setting time of the cement and an increase in the compressive strength of mortar by addition of the synthesized cPSA-EGDMA.

• Proceedings of the Membrane Society of Korea Conference
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• 2003.05a
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• pp.53-56
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• 2003