• Macromolecular Research
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• 제16권4호
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• pp.293-302
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• 2008

In our previous publication, the problem of particle deformation and coagulation at the nucleation stage in the presence of cross-linker was intensely studied by seeded batch dispersion polymerization of methyl methacrylate (MMA). In the present work, highly cross-linked, monodisperse PMMA particles were prepared under various reaction conditions by seeded semi-continuous process. Monodisperse, $6.5{\mu}m$-diameter PMMA particles containing up to 8 wt% of DVB or EGDMA were successfully made by seeded semi-continuous process and multi-semi-continuous addition process, respectively. Therefore, this study shows that seeded semi-continuous process is more effective and efficient to prepare highly cross-linked, monodisperse particles than non-seeded and seeded batch processes.

• Macromolecular Research
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• 제15권3호
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• pp.244-255
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• 2007

Nucleation is the most sensitive stage in the preparation of highly cross-linked, monodisperse microspheres by dispersion polymerization, since the addition of a small amount of cross-linker results in particle deformation and coagulation. To overcome these problems, $5\;{\mu}m$ poly(methyl methacrylate) seed particles prepared by dispersion polymerization were used in the preparation of mono disperse, cross-linked PMMA particles containing up to 7 wt% divinylbenzene by seeded batch dispersion polymerization. Spherical particles with a narrow size distribution containing up to 8 wt% of EGDMA were prepared by seeded multi-batch dispersion polymerization processes. These particles were identified by scanning electron microscopy and DSC.

• 한국응용과학기술학회지
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• 제21권4호
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• pp.370-379
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• 2004

Highly crosslinked micron-size monodispersed PMMA/PDVB and PS/PDVB particles were prepared using seeded multi-stage emulsion polymerization. PMMA and PS seed particles were synthesized by seeded multi-stage emulsion polymerization and soap-free emulsion polymerization. Then PMMA/PDVB and PS/PDVB particles were obtained using semi-batch type emulsion polymerized using divinyl benzene as a cross-linkable monomer in the presence of seed particles. PMMA particles with size of ca. 730 nm and polydispersity of 1.03 were successfully prepared in this experiment. PS particles with size of ca. 1.5 ${\mu}m$ and polydispersity of 1.01 were prepared in this experiment. Highly crosslinked PS/PDVB particles with size of ca. 1.3 ${\mu}m$ and polydispersity of 1.00 were obtained.

• Elastomers and Composites
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• 제46권1호
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• pp.60-69
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• 2011

[ $2.1\;{\mu}m$ ]입자경의 단분산 PBA seed를 이용한 2단계 분산중합을 seeded batch process 와 seeded semi-continuous process를 이용하여 다양한 형태의 PBA/PMMA composite 미립자를 제조하였다. Batch process의 경우 PBA/PMMA composite 입자의 모폴로지는 중합 분산매인 methanol/water 비와 중합 2단계에서의 PBA seed/MMA단량체의 비에 따라 크게 영향을 받으며, methanol/water 중합분산매중 물의 량이 증가함에 따라, 그리고 중합 2단계에서 MMA단량체량이 증가함에 따라 PBA와 PMMA간의 상분리현상이 심화되어 구형의 입자로부터 egg, snowman, confetti, peanut와 같은 비구형의 PBA/PMMA composite 입자들이 제조되었다. Semi-continuous process의 경우 단량체 부가시간을 조절함으로서 PBA/PMMA composite 입자의 모폴로지가 변함을 발견하였고 특히, 단량체의 결핍된 조건하에서 구형의 PBA(코어)/PMMA(쉘) composite 라텍스가 제조되었다.

• 폴리머
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• 제30권1호
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• pp.50-55
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• 2006

분산중합으로 제조된 폴리스티렌(PS) 시드 고분자 미립자에 가교단량체인 HDDA(1,6-hexanedioldiacrylate)를 one-step으로 흡수시키고 이를 중합하여 단분산 가교고분자 미립자를 제조할 시 1) 시드 고분자의 분자량, 2) 흡수된 가교단량체와 시드의 중량비, 3) 중합반응속도 등의 변화에 따른 가교고분자 입자의 표면 모폴로지 변화 등을 관찰하였다. 이번 연구를 통해 PS/HDDA계에서는 시드 고분자의 분자량 및 가교단량체 흡수비에 관계없이 가교고분자 입자표면에 분화구 형태의 모폴로지가 관찰되었으며, 이와 같은 표면 모폴로지는 중합반응속도를 조절함으로써 조절이 가능함을 알 수 있었다.

• 접착 및 계면
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• 제10권4호
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• pp.174-181
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• 2009

고 고형분 점착제의 점도 개선을 위해 seed 중합을 이용하여 수용성 저점도 점착제를 중합하였다. Seed 바인더 중합 중 최적 중합 조건을 산출하고, 점착제 중합 시 seed 바인더와 acrylic acid의 함량을 변화시켜 점도변화와 피착면에 대한 점착박리강도를 측정하여 다음과 같은 결과를 얻었다. 점착제 중합에서 seed 바인더의 함량이 7 wt%/monomer일 때 60%의 고형분에서 2,100 cps의 낮은 점도를 나타내고 평활한 점착제 필름을 제조할 수 있었다. Acrylic acid함량 변화에 따른 기계적 물성 측정에서는 4 wt%/monomer의 acrylic acid를 사용 했을 때 우수한 점착박리강도와 유지력을 나타내었다.

• 공업화학
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• 제10권6호
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• pp.889-894
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• 1999

유화중합법으로 마이크론 크기의 고분자 라텍스 입자 제조시, 라텍스 입자의 응집, 2세대 입자의 생성 등의 문제 때문에 원하는 형태, 크기, 구조를 지니는 입자를 제조하기가 매우 어려운 것으로 알려져 있지만 구조적, 기능적 고분자 미립자를 합성할 수 있는 장점이 있다. 따라서, 본 연구에서는 마이크론 크기의 라텍스 입자를 제조하는데 있어서, 미립자 성분으로 n-butyl acrylate(BA)를 선정하고, 개시제의 농도, 유화제의 양, 반응 온도, 가교제의 양 및 교반기의 속도 등의 반응 변수 조건에 따른 seed 유화 중합을 실시하여 각 반응 변수들이 입자의 크기 및 분산도에 미치는 영향에 대하여 조사하였다. 실험 결과를 바탕으로 반응 변수의 최적 조건들을 규명하여 연속적 seed 유화중합법으로 $0.14{\sim}3.67{\mu}m$의 평균 입자경을 갖는 poly(n-butyl acrylate)(PBA) 라텍스 입자를 제조할 수 있었다.

• Macromolecular Research
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• 제17권4호
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• pp.250-258
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• 2009

One-step seeded polymerization was used to prepare $7{\sim}10{\mu}m$ of crosslinked monodisperse spheres with four crosslinking agents using $4.68{\mu}m$ poly(methyl methacrylate)(PMMA) seed particles in aqueous-alcoholic media in the absence of the swelling process. The crosslinking agents used were ethylene glycol dimethacrylate(EGDMA), allyl methacrylate(AMA), 1,6-hexanediol diacrylate(HDDA) and trimethylolpropane trimethacrylate(TMPTMA). The effects of the type and concentration of the crosslinking agents on the swelling, pore size, thermal property of the networks and morphology of the particles were studied. The chemical structures and concentrations of the crosslinking agents affected both the swelling ratio and the porosity of the networks. In addition, the chemistry of the reactive vinyl group and chain length of the crosslinking agents affected the stability of the monodisperse particles of the ultimate morphology.

• 한국응용과학기술학회지
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• 제19권2호
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• pp.131-136
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• 2002

As model waterborne acrylic coatings, mono-dispersed poly(butyl acrylate-methyl methacrylate) copolymer latexes of random copolymer and core/shell type graft copolymer were prepared by seeded multi-staged emulsion polymerization with particle size of $180{\sim}200$ nm using semi-batch type process. Sodium lauryl sulfate and potassium persulfate were used as an emulsifier and an initiator, respectively. The effect of particle texture including core/shell phase ratio, glass transition temperature and crosslinking density, and film forming temperature on the film formation and final properties of film was investigated using SEM, AFM, and UV in this study. The film formation behavior of model latex was traced simultaneously by the weight loss measurement and by the change of tensile properties and UV transmittance during the entire course of film formation. It was found that the increased glass transition temperature and higher crosslinking degree of latex resulted in the delay of the onset of coalescence of particles by interdiffusion during film forming process. This can be explained qualitatively in terms of diffusion rate of polymer chains. However, the change of weight loss during film formation was insensitive to discern each film forming stages-I, II and III.

• 한국응용과학기술학회지
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• 제21권1호
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• pp.69-75
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• 2004

In this study, various model composite latexes were synthesized using n-butyl acrylate and methyl methacrylate as comonomers by seeded multi-staged emulsion polymerization. Monodispersed model composite latex particles with size of 190 nm and polydispersity index of 1.05, which have various morphology including random copolymer particle, soft-core/hard-shell particle, hard-core/soft shell particle, and gradient-type copolymer particle, homopolymers particles were prepared. The designed morphology of model composite particles were confirmed.