For the purpose of the pre-industry production of poly(L-lactide) (PLLA) and full understanding of the supercritical polymerization system, large scale polymerization of L-iactide initiated by 1-dodecano/stannous 2-ethyl-hexanoate (DoOH/Sn(Oct)$_2$) was carried out in supercritical chlorodifluoromethane under various reaction conditions (time, temperature and pressure)and reactants (monomer and supercritical solvent) concentrations. A 3 L sized-reactor system was used throughout this study. The monomer conversion increased to 72% on increasing reaction time to 5 h. The molecular weight of PLLA product also increased to 68000 g/moi over the same period. An increase in monomer concentration resulted in a higher molecular weight, up to 144000 g/mol and 97% of monomer conversion. Raising the reaction pressure from 130 to 240 bar also resulted in an increased monomer conversion and molecular weight. To increase heat resistivity of PLLA, methanol treatment and heat-vacuum methods were evaluated. Both of them successfully improved the heat resistivity property of PLLA.
We have described primary studies on conductivity and molecular weight of polyaniline separately in the electric and magnetic fields when it is used in a field effect experimental configuration. We report further studies on doped in-situ deposited polyaniline. First we have chemically synthesized polyaniline by ammonium peroxodisulfate in acidic aques and organic solutions at different times. Then we measured mass and conductivity and obtained the best time of polymerizations. In continue, we repeated these reactions separately under different electric and magnetic fields in constant time and measured mass and conductivity. The polyaniline is characterized by gel permeation chromatography (GPC), UV-Visible spectroscopy and electrical conductivity. High molecular weight polyanilines are synthesized under electric field, $M_w$ = 520000-680000 g/mol, with $M_w/M_n$ = 2-2.5. The UV-Visible spectra of polyanilines oxidized by ammonium peroxodisulfate and protonated with dodecylbenzenesulfonic acid (PANi-DBSA), in N-methylpyrolidone (NMP), show a smeared polaron peak shifted into the visible. Electrical conductivity of polyanilines has been studied by four-probe method. The conductivity of the films of emeraldine protonated by DBSA cast from NMP are higher than 500 and 25 S/cm under 10 KV/m of potential) electric field and 0.1 T magnetic field, respectively. It shows an enhanced resistance to ageing too. By the next steps, we carried chemical polymerization at the best electric and magnetic fields at different times. Finally, resulted in finding the best time and amount of the fields. The longer polymerization time and the higher magnetic field can lead to degradation of polyaniline films and decrease conductivity and molecular mass.
Purpose of this research is estimating polymerization depth of different source of light. XL 3000 for halo-gen light, Apollo 95E for plasma arc light and Easy cure for LED light source were used in this study. Different shade (B1 & A3) resin composites (Esthet-X, Dentsply, U.S.A.) were used to measure depth of cure. 1, 2, and 3 mm thick samples were light cured for three seconds, six seconds or 10 seconds with Apollo 95E and they were light cured with XL-3000 and Easy cure for 10 seconds, 20 seconds, or 40 seconds. Vicker's hardness test carried out after store samples for 24 hours in distilled water. Results were as following. 1. Curing time increases from al1 source of lights, oui$.$ing depth increased(p<0.05). 2. Depth (that except 1mm group and 2mm group which lighten to halogen source of light) deepens in all groups, Vickers hardness decreased(p<0.05). 3. Vicker's hardness of A3 shade composite was lower in all depths more than B1 shade composites in group that do polymerization for 10 seconds and 20 seconds using halogen source of light(p<0.05), but group that do polymerization lot 40 seconds did not show difference(p>0.05). 4. Groups that do polymerization using Plasma arc and LED source of light did not show Vicker's hardness difference according to color at surface and 1mm depth(p>0.05), but showed difference according to color at 2mm and 3mm depth(p<0.05). The results showed that Apollo 95E need more polymerization times than manufacturer's recommendation (3 seconds), and Easy cure need polymerization time of XL-3000 at least.
Most of cervical abrasion and erosion lesions show gingival margin where the cavosurface angle is on cementum or dentin. Composite resin restoration of cervical lesion shrink toward enamel margin due to polymerization contraction. This shrinkage has clinical problem such as microleakage and secondary caries. Several methods to diminish contraction stress of composite resin restoration, such as modifying cavity form and building up restorations in several increments have been attempted. The purpose of this study was to compare polymerization contraction stress of composite resin in Class V cavity subjected to cavity forms and placement methods. In this study, finite element model of 5 types of Class V cavity was developed on computer tomogram of maxillary central incisor. The types are : 1) Box cavity 2) Box cavity with incisal bevel 3) V shape cavity 4) V shape cavity with incisal bevel 5) Saucer shape cavity. The placement methods are 1) Incisal first oblique incremental curing 2) Bulk curing. An FEM based program for light activated polymerization is not available. For simulation of curing dynamics, time dependent transient thermal conduction analysis was conducted on each cavity and each placement method. For simulation of polymerization shrinkage, thermal stress analysis was performed with each cavity and each placement method. The time-temperature dependent volume shrinkage rate, elastic modulus, and Poisson's ratio were determined in thermal conduction data. The results were as follows : 1. With all five Class V cavifies, the highest Von Mises stress at the composite-tooth interface occurred at gingival margin. 2. With box cavity, V shape cavity and saucer cavity, Von Mises stress at gingival margin of V shape cavity was lower than the others. And that of box cavity was lower than that of saucer cavity. 3. Preparing bevel at incisal cavosurface margin decreased the rate of stress development in early polymerization stage. 4. Preparing bevel at incisal cavosurface margin of V shape cavity increased the Von Mises stress at gingival margin, but decreased at incisal margin. 5. At incisal margin, stress development by bulk curing method was rapid at early stage. Stress development by first increment of incremental curing method was also rapid but lower than that by bulk curing method, however after second increment curing final stress was the same for two placement methods. 6. At gingival margin, stress development by incremental curing method was suddenly rapid at early stage of second increment curing, but final stress was the same for two placement methods.
Many studies have been carried out on the graft finishing in order to improve the quality of silk fiber. Various vinyl monomers, for instance, styrene, methylmethacrylate, 2-hydroxyeth-ylmethacrylate and methacrylamide, have been used practically up to date. Among these monomers, methacrylamide has been applied as the most favourable monomer onto silk fibers in recent years. The polymerization mechanism about styrene- and methylmethacrylate-grafted silk fiber has been studied by many researchers. They proposed that free radicals were formed and vinyl monomers were polymerized in silk fibroin by graft polymerization mechanism, while active sites were varied by the types of monomer and initiator as well as by the reaction condition. In general. there is another Opinion that monomers are polymerized and impregnated in the internal side of the fiber by homopolymerization, which has not been proved experimentally yet More than 10 years have been passed since methacrylamide was applied on the silk fiber, and at the present time most finishings are being achieved by methacrylamide. However, no attention has been paid to the polymerization mechanism of the methacrylamide-treated silk fiber yeL In this paper, the treatments of methacrylamide on silk fibers were studied in aqueous solution using potassium persulfate as an initiator. The polymerization mechanism of the methacrylamide-treated silk fibers was investigated and analyzed on the basis of the results of infrared spectroscopy, amino acid analysis and scanning electron microscopy. From the results of these instrumental analyses, it can be suggested that polymerization mechanism about the methacrylamide-treated silk fibers is not performed by graft polymerization which has been accepted generally in styrene and methylmethacrylate-grafted silk fibers. The different mechanism is supposed to be due to the difference in monomer types, initiator types and treatment conditions.
Ion-exchange polymeric stationary phases presenting amino acid and amino groups were prepared by the surface grafting of glycidyl methacrylate onto a silica gel surface and subsequent amination. Three kinds of amino acids-L-arginine (Arg), D-lysine (Lys), and D-histine (His)-were used in this study. An ion-exchange polymeric stationary phase presenting ethylene diamine (EDA) was also prepared by surface graft polymerization. Separation of the model proteins bovine serum albumin (BSA), chick egg albumin (CEA), and hemoglobin (Hb) was performed using the amino acid- and amine-derived columns. In separating the CEA/BSA mixture, the resolution time of BSA was longer than that of CEA when using the EDA column, whereas the resolution time of BSA was shorter than that of CEA when using the Arg, Lys, and His columns. In the separation of the Hb/BSA mixture, the resolution time of BSA was longer than that of Hb in the EDA column, whereas the resolution time of BSA was shorter than that of Hb in the amino acid columns (D-Lys, L-Arg, and D-His).
The purpose of this study is to evaluate the polymerization ability of three different light sources by microhardness test. Stainless steel molds of 1, 2, 3, 4 and 5 mm in thickness of 7 mm in diameter were prepared. The hybrid composite Z100 was packed into the hole of the mold and curing light was activated for designated time. Three different light sources, conventional halogen, light emitting diode, and plasma arc, were used for curing of composite. Two different curing times applied ; one is to follow the manufacturers recommendation and the other is to extend the curing time of LED and plasma arc for balancing the light energy with halogen. Immediately after curing, the Vickers hardness was measured at the bottom of specimen. The results were as follows. 1 The composite cured with LED showed equal to higher microhardnesss than halogen. 2. The composite was cured with plasma arc by manufacturers recommendation showed lowest micro-hardness at all thickness. However, when curing time was extended, microhardness was higher than the others. In conclusion, this study suggested that plasma arc needs properly extended curing time.
The distinguishing characteristic of the glow discharge is that chemical reaction induced by partially ionized gases are limited only to the substrate surface. Most studies have been done on the plasma etching and polymerization. The graft polymerization in vapour phase by cold plasma has been rarely investigated. In this study the system of tub3ar reaction chamber with capacitively coupled electrode of alternative current of 60 Hz was employed for the graft polymerization. The graft polymerization of Acylic Acid(AA) onto the poly (ethylene terephthalate) (PET) was carried out by treatment of PET film and fabric by cold plasma (glow discharge of argon gas), followed by the supply of AA vapour. The graft yield was about 1 wt%. The surface property was determined by contact angle, the surface tension was evaluated by zisman’s plot and equation of surface tension mesurement. The results were as follows: 1. In order to obtain lower contact angle, it was effective to avoid the vicinity of electrodes for a setting position of substrate. 2. Contact angle affected on the monomer pressure and its duration of exposure to the acid vapour. 3. Polymer radical formation was influenced by the changes of the value of current density and plasma treatment time. 4. Total surface tension of plasma grafted PET film increased. With an increase in the carboxylic acid content, the dispersion force decreased, while, the polar force and hydrogen bonding force increased. 5. The contact angle decreased from $75^\circ$ to around $30^\circ$ by plasma grafting. There was no ageing effect on the contact angle after 4 months.
Byun, Gill Jae;Ha, Jong-Rok;Kim, Byung-Sun;Joe, Chee Ryong;Ok, Ju Seon
Composites Research
/
v.25
no.6
/
pp.198-204
/
2012
The objective of this study is to improve the mechanical properties in abaca fabric/epoxy composites produced using a VARTM process. The mechanical properties were improved by increasing the surface roughness of the fabric through plasma polymerization and improving the interfacial adhesion between the epoxy and the fabric through changing its hydrophilic properties to the hydrophobic properties. Plasma polymerization at atmospheric pressure and room temperature was used, and the optimal polymerization time to improve the mechanical properties was investigated. NaOH treatment on the fabric was also carried out for the comparison. The composite fabricated using the fabric polymerized for 10 seconds shows the highest tensile strength compared to that of none-polymerized or NaOH treated. Plasma polymerization for more than 20 seconds exhibits decrease in the tensile strength. As a result, the plasma polymerization for more than 20 seconds may have caused some damages on the surface of the fabrics. Also, the hydrophilic abaca represents a tendency of presenting the hydrophobic properties in absorption and sedimentation tests.
Oh, Dae Geun;Lee, Kyung Hoon;Kim, Wan Tae;Min, Byung Hoon;Chung, Dae-won;Lee, Jong Doo;Kim, Jeong Ho
Applied Chemistry for Engineering
/
v.19
no.4
/
pp.370-375
/
2008
Optimum synthesis conditions were investigated for the non-aqueous dispersion (NAD) polymerization of environmentally-friendly acrylic resin. The optimum amount of stabilizer was observed to be 20 wt% to prevent flocculation of the synthesized polymer particles. The optimum ratio of aliphatic solvents to aromatic solvents turned out to be 80 to 20 in order to obtain a stabilized NAD resins. The viscosity of NAD resins was affected not only by the reaction time but also by the amount of initiator and the impeller rpm. Also, the particle size and the size distribution were influenced by the amount of stabilizers and initiators. Since the stability of NAD resin was devastated by the increase in particle size when all the monomers were fed at the beginning of polymerization, the monomers need to be put into the reactor step by step throughout the entire polymerization process.
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