• Title/Summary/Keyword: Unreacted monomer

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A Study on the Polymerization of Energetic Poly(NEO) (에너지를 함유한 선 폴리머인 poly(NEO) 제조 공정 연구)

  • Cheun Young Gu;Kim Jin Seuk
    • Journal of the Korea Institute of Military Science and Technology
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    • v.7 no.2 s.17
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    • pp.109-117
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    • 2004
  • We synthesized energetic prepolymer(2-nitrato ethyl oxirane, NEO) for plastic-bonded explosive and measured its thermodynamic parameters. 2-Nitrato ethyl oxirane(NEO) as a monomer was synthesized from 4-butene-ol, the first-step was preparation of 1-nitrate-3-butene and second-step was synthesized 2-nitrate-ethyl oxirane from 1nitrate-3-butene and then polymerized by cationic ring opening polymerization. The unreacted monomer concentration was measured by GC. The thermodynamic parameters were obtained from the ceiling temperature(Tc) values of 1 mole monomer at each reaction temperature. We varied feed rate of monomer, concentration of initiator and monomer to control molecular weight and polydispersity of perpolymer(NEO). Number average molecular weight(Mn), polydispersity(PD), and glass transition temperature(Tg), viscosity of prepolymer(NEO) were 2000, 1.07, $-55^{\circ}C$ and 300 poise respectively.

Reaction Condition Dependency of Propagating Behavior in the Polymerization Reaction by Thermal Front

  • Huh, Do-Sung;Choe, Sang-Joon;Lee, Burm-Jong
    • Bulletin of the Korean Chemical Society
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    • v.23 no.2
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    • pp.325-329
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    • 2002
  • In this study, the dependency of the behavior of propagating front on the reaction condition in frontal polymerization reaction has been studied. We have used some multifunctional acrylates as a monomer and ammonium persulfate as an initiator for the polymerization reactions. In frontal polymerization, a method of producing polymeric materials via a thermal front that propagates through the unreacted monomer/initiator solution, the behavior of self propagating front shows various dynamic patterns depending on the reaction condition. We have obtained some spin modes of propagating front in the number of 'hot spots' or 'spin heads' by changing the reaction condition. The effect of the reactor tube diameter on the mode of propagating front has also been studied by using some reactor tubes with different size of tube diameter and it has been examined in some detail by adopting an experimental method of two-tubes system.

Preparation of Composite Membranes for Recovery of Unreacted Olefin Monomers (미반응 올레핀계 모노머 회수를 위한 복합막의 제조)

  • Kim, Hyun-Gi;Kim, Sang-Yong;Kim, Sung-Soo
    • Membrane Journal
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    • v.20 no.4
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    • pp.297-303
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    • 2010
  • Composite membranes were prepared for membrane/cold condensation process for recovery of unreacted olefin monomer from the polyolefin polymerization process by solution coating and plasma polymerization processes. Poly(dimethylsiloxane) (PDMS) solution was coated on polysulfone (PSF) support and increase of prepolymer content in solution made more dense membrane structure to result in the increase of separation factor while absolute flux decreased. Permeation of organic materials through the composite membranes follows the sorption and diffusion mechanism, which brought about the results that separation factor increased with critical temperature of the organic materials, and that flux increased with the increase of the molar volume. Crosslinking period affected the permeation characteristics. Other types of composite membranes were fabricated by plasma polymerization of siloxane materials on polypropylene (PP) and PSF supports. PP was tested as a support for composite membranes, which had not been used so far in solution coating process, and plasma polymerization made the composite membranes equivalent performances to those of membranes prepared by solution coating process.

Process Design for Recovery of Unreacted Styrene Monomer for Utility Saving (유틸리티 절감을 위한 미반응 스티렌 모노머 회수공정의 설계)

  • Bong, Jooyoung;Na, Sujin;Lee, Kwang soon
    • Korean Chemical Engineering Research
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    • v.55 no.1
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    • pp.54-59
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    • 2017
  • A study for process design to curtail the utility consumption during residual styrene monomer recovery in an ABS polymerization process was carried out. Among different techniques for residual monomer recovery, the steam stripping is dominantly employed in industries. The existing process, however, consumes a large amount of utility (steam and cooling water), and this study focused on the design of a new process that can substantially spare the utility consumption. A new process was configured to utilize the latent heat of the stripping steam, which is condensed with the monomer using cooling water after exiting the stripper. The condenser was modified to use vacuum state water as coolant and to generate vacuum state steam using the latent heat of the stripping steam. The steam is injected to the stripper as the stripping steam after upgrading using a compressor. Through this modification, consumption of steam and also cooling water could be significantly reduced at some expense of electricity for compressor operation.

COMPARISON OF MONOMER RELEASE FROM PIT AND FISSURE SEALANT FOLLOWING VARIOUS SURFACE TREATMENT (치면열구전색제의 광중합 후 표면 처리 방법에 따른 미반응 모노머 용리 비교)

  • Lee, Sang-Woo;Lee, Ju-Hyun;Seo, Hyun-Woo;Park, Ho-Won
    • Journal of the korean academy of Pediatric Dentistry
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    • v.33 no.1
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    • pp.70-76
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    • 2006
  • The aim of this study was comparison of effectiveness of surface treatment methods in reducing the oxygen-inhibited layer of a commercially available freshly polymerized, light cured dental sealant($concise^{TM}$, 3M, St Paul, USA). Surface treatment groups were consisted of no treatment(negative control group) and 3 experimental groups according to surface treatment of light-cured sealant. Experimental group I was 10 seconds' exposure to distilled water syringe, group II was 10 seconds' manual application using a cotton pellet wetted with 75% alcohol and group III was 10 seconds' prophylaxis with pumice/water slurry using rubber cup on a slow-speed handpiece. All specimens were immersed in 5ml distilled water and stored at 37c water bath for 10 minutes. All eluates were analyzed by HLPC for identification and quantitive analysis of monomers. The results of this study can be summarized as follows. 1. None of the chromatograms of the tested sealant displayed peaks with the same retention time as that of the standard solution, except for TEGDMA. 2. All surface treatment group had a statistically significant decrease of monomer release in comparison with no treatment group. 3. Removal effects of unreacted monomer in group III was statistically significant in comparison with group I and group II. These results revealed that mechanical method using pumice and rubber cup is the most effective in removing residual monomer and may be valuable to be used effectively in clinic.

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A STUDY ON THE DEGREE OF POLYMERIZATION OF AUTOPOLYMERIZED RESIN FOR REMOVABLE ORTHODONTIC APPLIANCE ACCORDING TO CURING TIME AND CURING METHOD (중합시간과 중합방법에 따른 자가중합형 상교정용 레진의 중합률의 비교에 관한 연구)

  • Yoo, Jong-Wook;Jang, Ki-Taeg;Kim, Chong-Chul
    • Journal of the korean academy of Pediatric Dentistry
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    • v.26 no.2
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    • pp.296-309
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    • 1999
  • Autopolymerized resin facilitates a more rapid and easier means for the construction of removable orthodontic appliances than heat cured resin. But many reports reveal that more unreacted monomer is found in autopolymerized resin. It is very important to achieve maximum degree of polymerization because if polymerization is inadequate, high level of unreacted monomer has been shown to adversely affect mechanical and physical properties, and also the question of allergy or toxicity to methylmethacrylate must be considered. The purpose of this study was to compare the degree of polymerization according to curing method and curing time. Five groups were desinged ; Group 1 was polymerizied at room temperature($28^{\circ}C$) ; Group 2 in $28^{\circ}C$ water ; Group 3 in $28^{\circ}C$ water under 30psi pressure ; Group 4 in $43^{\circ}C$ water ; Group 5 in $43^{\circ}C$ water under 30psi pressure for 10 minutes, 1 hour 12 hours, 1 day and 3 days. The degree of polymerization was measured by means of Fourier Transform Infrared spectroscopy. The results were as follows: 1. The degree of polymerization increased constantly in accordance with curing time in all groups and after curing for 10 minutes, Group 1 showed significantly higher degree of polymerization after 12 hours and Group 2, Group 3, Group 4, Group 5 after 1 hour(p<0.05). 2. The degree of polymerization decreased in the order of Group 5, Group 4, Group 3, Group 2, Group 1 except when the curing time was 1 hour and 12 hours(p<0.05). 3. The degree of polymerization of Group 4, Group 5 cured at $43^{\circ}C$ showed significantly higher degree of polymerization than Group 2, Group 3 at $28^{\circ}C$ except when the curing time was 1 day(p<0.05). 4. Among Group 2, Group 3 and Group 4, Group 5, the pressure had no effect on polymerization except when the curing time was 12 hours(p<0.05). 5. Between Group 1 and Group 2, the method of storage had no effect on polymerization except when the curing time was 1 hour(p<0.05).

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THE EFFECT OF OXYGEN INHIBITION ON INTERFACIAL BONDING BETWEEN COMPOSITE RESIN LAYERS (복합레진 적층계면에서 oxygen inhibition의 영향에 관한 연구)

  • Choi, Su-Mi;Park, Jae-Hong;Choi, Sung-Chul;Kim, Kwang-Chul;Choi, Young-Chul
    • Journal of the korean academy of Pediatric Dentistry
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    • v.37 no.3
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    • pp.298-307
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    • 2010
  • The purpose of this study was to assess the effect on oxygen inhibition layer(OIL) for the interfacial bonding between resin composite layers, including shear bond strength, fracture modes and degree of conversion. The first layer of specimen was filled with Z-250(shade A3) and was cured for 40s. The second layer of specimen was filled with same composite(shade A1) and was cured for 40s. The first layer of specimens for each group were prepared by methods as followings. Control(curing in atmospheric air), Group1(curing against Mylar strip), Group2(scrubbed with a acetone-soaked cotton), Group3(using Tescera light cup), Group4(using Tescera heat cup), Group5(stored in disti1led water for 30days at $37^{\circ}C$), Group6 (using bonding agent). The results were as follows: 1. There was no statistically significant different shear bond strength between control and group 1(p>0.05). 2. Group 2 showed significantly lower shear bond strength than control and group 1(p<0.05). 3. The observation of the fracture surface leads to the evidence that a major difference occurs in the case of control, group1 and group 3 samples which break mainly cohesively while the other groups break in majority adhesively. 4. The results of FTIR showed that the degree of conversion was the highest in group 2 and the lowest in control group(p<0.05). It can be concluded that an OIL is not necessary for bonding with composite resin. But if a reduced critical amount of the unreacted monomer is present, it was detrimental to bonding additional layers of composite. Further study, such as the quantitative analysis of the unreacted monomer are required.

Copolymerization of 2-Hydroxyethyl Methacrylate with Functional Silane Monomers (2-히드록시에틸 메타크릴레이트와 기능성 사이레인 단량체와의 공중합에 관한 연구)

  • Sung, Yong-Kiel;Lee, Chang-Gyu;Jung, Il-Nam
    • Journal of Biomedical Engineering Research
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    • v.8 no.1
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    • pp.29-40
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    • 1987
  • 2-Hydroxyethyl methacrylate(HEMA) was copolymerized with allyltrimethylsilane- (ATMS) and allylt.imethoxysilane(ATMOS) at 70。C in N, N'dimethylformamide- (DMV) using $\alpha$ , $\alpha$'-azobisisobutyronitrile(AIBN). The compositions of unreacted monomers were determined by gas chromatographic analysis. The monomer reactivity ratios were determined by Fireman-Ross, Helen-Tiidus and intersection methods. The average values are as follows : $$r_1(HEMA) : 6.62 $\pm$ 0.07, r_2(ATMS) : 0.07 $\pm$ 0.01 for HEMA-ATMS system.$$ $$r_l(HEMA) : 4.09 $\pm$ 0.14, r_2(ATMOS) : 0.06 $\pm$ 0.01 for HEMA-ATMOS toys tem.$$ The lower rl(HEMA) In the HEMA-ATMOS system as compared to HEMA ATMS system may be contributed to higher relative reactivity of ATMOS toward the poly(HEMA) radical. The compositions of synthesized copolymers were determined from silicon con tents estimated gravimetrically. The thermal stabilities of the copolymers were investigated by thermogravimetry(TG). The enthalpic changes associated with the endothermic transition were evaluated by differential scanning calorimetry(DSC). The swelling properties of the copolymers in water were also investigated.

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MONOMER RELEASE FROM PIT AND FISSURE SEALANT FOLLOWING BY SURFACE TREATMENT AND CURING TIME (치면열구전색제의 표면처리와 중합시간 증가에 따른 미반응 모노머 용리 평가)

  • Seo, Hyun-Woo
    • Journal of the korean academy of Pediatric Dentistry
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    • v.34 no.1
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    • pp.122-129
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    • 2007
  • The purpose of this study was to evaluate the effects of a various light curing time on the residual monomers released from light-cured dental sealant, and to examine the effectiveness of surface treatment in reducing the oxygen-inhibited layer of light-cured dental sealant($Helioseal^{(R)}$ F, Vivadent, Liechtenstein). Specimens were cured with a halogen light curing unit(XL 3000, 3M, USA) for 20, 40, 60s. Surface treatment of a light-cured dental sealant included no treatment(control group), a 10-seconds exposure to distilled water(Group I), 10-seconds manual application using a cotton pellet wetted with 75% alcohol(Group II), and 10-seconds application of a water/pumice slurry using a rubber cup on a slow-speed handpiece The specimens were eluted in distilled water for 10 minutes. All elutes were analyzed by HPLC for identification and quantitive analysis of monomers. The results of this study can be summarized as follows. 1. None of the chromatograms of the tested sealant displayed peaks with the same retention time as that of the standard solution, except for TEGDMA. 2. The release of TEGDMA decreased with increasing curing time in conventional halogen light. 3. All surface treatment group had a decrease of monomer release in comparison with no treatment group. 4. Treatment that Group III eliminated the greatest amount of any type of residual monomers. 5. The elution of unreacted monomers from curing with halogen curing unit for 60s and Group III was less than other groups.

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DEGREE OF CONVERSION OF BIS-ACRYLIC BASED PROVISIONAL CROWN AND FIXED PARTIAL DENTURE MATERIALS

  • Kim, Sung-Hun;Watts, David C.
    • The Journal of Korean Academy of Prosthodontics
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    • v.46 no.6
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    • pp.639-643
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    • 2008
  • STATEMENT OF PROBLEM: The degree of conversion may influence the ultimate mechanical and physical properties of provisional crown and fixed partial denture materials. The high levels of the unreacted residual monomer may cause deleterious effect on the properties. PURPOSE: The purpose of this study was to measure the degree of conversion of bis-acrylic based provisional crown and fixed partial denture materials by using an infrared spectroscopic method. MATERIAL AND METHODS: Chemically activated three bis-acrylic based provisional crown and fixed partial denture materials, LuxaTemp [DMG, Hamburg, Germany], fast set TemPhase [Kerr, Orange, CA, USA] and Protemp 3 Garant [3M-ESPE, St Paul, MN, USA], were investigated by Fourier transform infrared spectrometry (FTIR). The FTIR spectra of the materials tested were immediately obtained after mixing. The specimens were stored under dry conditions and at $23^{\circ}C$ for 24 hours, and then the spectra of the materials were also obtained. The degree of conversion (%) was calculated from the spectrum of the absorbance between the aliphatic double bond at 1637 $cm^{-1}$ and the aromatic double bond at 1608 $cm^{-1}$ using the baseline method. The data were statistically analyzed using one-way ANOVA and the multiple comparison Scheffe test at the significance level of 0.05. RESULTS: The mean value and standard deviation of the degree of conversion were 52.5 % ${\pm}$ 1.1 %, 50.3 % ${\pm}$ 0.8 %, and 42.3 % ${\pm}$ 4.9 % for LuxaTemp, Protemp 3 Garant and fast set TemPhase, respectively. There was no significant difference between LuxaTemp and Protemp 3 Garant, whereas there was a statistically difference between Protemp 3 Garant and fast set TemPhase, and LuxaTemp and fast set TemPhase (P < .05). CONCLUSION: The degree of conversion of fast set TemPhase was significantly lower than those of the others. The degree of conversion may be correlated with the rate of polymerization.