• Korean Chemical Engineering Research
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• v.54 no.1
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• pp.57-63
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• 2016

Thermally induced phase separation (TIPS) and nonsolvent induced phase separation (NIPS) were simultaneously induced for the preparation of flat PVDF membranes. N-methyl-2-pyrrolidone (NMP) was used as a solvent and dibutyl-phthlate (DBP) was used as a diluent for PVDF. When PVDF was melt blended with NMP and DBP, crystallization temperature was lowered for TIPS and unstable region was expanded for NIPS. Ratio of solvent to diluent changed the phase separation mechanism to obtain the various membrane structures. Contact mode of dope solution with nonsolvent determined the dominant phase separation behavior. Since heat transfer rate was greater than mass transfer rate, surface structure was formed by NIPS and inner structure was by TIPS. Quenching temperature of dope solution also affected the phase separation mechanism and phase separation rate to result in the variation of structure.

• Journal of the Korean Applied Science and Technology
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• v.28 no.4
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• pp.386-392
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• 2011

We are crystallized to the linear low density polyethylene(LLDPE) particles by a thermally induced phase separation(TIPS). TIPS process based on the phase separation mechanism was performed for the LLDPE system which undergoes liquid-solid phase separation. The linear low density polyethylene particle formation occurred by the nucleation and growth mechanism in the metastable region. Although the growth rates depended on the experimental conditions such as the polymer concentration and temperature, the particles were larger when the polymer concentration was higher or temperature was higher. The particles were observed by SEM. The LLDPE particle size distribution became broader when the polymer concentration was higher.

• Journal of the Korean Applied Science and Technology
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• v.28 no.3
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• pp.306-312
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• 2011

In this study, we are crystallized to the low density polyethylene (LDPE) micro-particles in $n$-dodecanol solution by thermally induced phase separation(TIPS) method. The Low density polyethylene micro-particles is used in a wide variety of polymer coatings and industrial application. The utility of that for a particular application depends on a number of factors such as the particle size and distribution, and chemical composition of the materials. However, there are still needs for new methods of preparation which will provide the structure with unique sizes. The widely used processes for micro-size particles are crystallization method and thermally induced phase separation. TIPS process based on the phase separation mechanism was performed for the LDPE system which undergoes liquid-solid phase separation. Effects of various operating parameters were examined on the structure variation of the particles. Professionality, take-up speed and crystallization rate depended on temperature and concentration of polymer in solution.

• Proceedings of the Membrane Society of Korea Conference
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• 1992.10a
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• pp.41-42
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• 1992

고내열 및 고내화학적 특성을 갖는 미세다공성 고분자막의 개발을 위한 기초연구가 수행되었다. 본 연구에서는 고분자막 제조기법의 첨단기술로 등장한 열유도상 분리공정(Thermally Induced Phase Separation, 이하 TIPS)이 도입되었다. TIPS 공정은 고분자를 고분자의 용융점을 상회하는 온도에서 매우 미세하게 분산시킬 수 있는 희석제를 고분자와 함께 melt-blending하여 균일한 single phase의 용액을 만들고 이를 적당한 막의 형태로 성형한 후, 가해진 열을 제거하여 냉각시킴에 따라 polymer-rich phase 와 polymer-poor phase 로 구성되는 two phase system으로 상분리를 일으키는 방법이다. 이때 polymer-poor phase를 차지하는 희석제를 제거함에 따라 고분자 matrix 내에는 void volume이 형성되고, 그 결과 고분자 matrix 전체적으로 다공성이 부여되어 고분자막으로서의 기본적인 기능을 갖추게 된다.

• Membrane Journal
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• v.28 no.6
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• pp.395-405
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• 2018

Poly(ethylene-co-vinylalcohol) EVOH hollow fiber membranes were successfully fabricated via a thermally induced phase separation (TIPS) method. It was observed that all membranes fabricated under different spinning conditions had interconnected and bicontinuous structures through liquid-liquid phase separation. Glycerol and poly(ethylene glycol) 200 were used as diluents for the TIPS method. Glycerol was used as a mixing component in quenching bath to control pores on the outer surface of the hollow fiber membrane. Hot quenching bath with a mixing component to generate large pores on the outer surface of the hollow fiber membrane. The effects of polymer concentration, diluent and quenching bath on the morphologies, water permeabilities, and mechanical properties of the EVOH hollow fiber membranes were systematically investigated. The relationship between water permeability, mechanical properties and spinning conditions was discussed in detail.

• Proceedings of the Membrane Society of Korea Conference
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• 2004.05a
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• pp.74-77
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• 2004

Porous membranes were prepared via thermally induced phase separation (TIPS) of (ethylene-co-vinyl alcohol) (EVOH)/glycerol mixtures. The liquid-liquid (L-L) phase boundaries are shifted to higher temperature when the ethylene contents in EVOH increase. Moreover, the kinetic study proved that the growth of droplets formed by the general liquid-liquid (L-L) phase separation obeyed a power-law scaling relationship in the later stage of spinodal decomposition (SD). A new phase separation mechanism was presented, in which the L-L phase separation could be resulted from the crystallization. The hollow fiber membranes were prepared. The membranes showed asymmetric structures with skin layer near the outer surface, the larger pores just below the skin layer and the smaller pores near the inner surface. The effect of ethylene content (EC) in EVOH, cooling water bath temperature and take-up speed on membrane performance was investigated.

• Membrane Journal
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• v.27 no.4
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• pp.350-357
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• 2017

In this study, we used TIPS (thermally induced phase separation) for the application of water treatment membrane, and observed the change in morphology of separation membrane due to the change of solidification temperature and heat capacity. For manufactured membrane, PVDF and silica with excellent mechanical properties and chemical resistance were used, and DOP (dioctyl phthalate), DBP (dibutyl phthalate) were used as the diluent. Using the SEM (scanning electron microscope), the morphology of each different coagulation solutions of heat capacity change was observed. As the heat capacity increased, the crystallization rate of PVDF was decreased and showed large pore. In contrast, It also confirmed that the smaller heat capacity, the faster the crystallization rate and make smaller pores.

• Membrane Journal
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• v.24 no.2
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• pp.158-166
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• 2014

In this research, microporous and bicontinuous poly vinylidene fluoride(PVDF) hollow fiber membranes were prepared via hybrid process of the thermally induced phase separation (TIPS) and stretching method. The mechanism of the membrane preparation is based on liquid-liquid phase separation. The final membranes have characteristic structures which have both bicontinuous and fibrillar morphology by applying the stretching method. They showed quite different structure when compared with the spherulitic or nodular structure from S/L TIPS and bicontinuous structure from L/L TIPS. At first, PVDF hollow fiber precursors were prepared via TIPS method using various kind of diluent mixtures. We used gamma-butyrolacton, dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP) as diluents. We could make hollow fiber membranes which had porous outer surface or dense outer surface by controling the parameters such as cooling conditions, PVDF concentration and the ratio of diluent mixtures. Finally, these hollow fiber were stretched at room temperature and diluents were extracted by ethanol. Effects of the stretching ratio on the membrane morphology were investigated using scanning electron microscope (SEM), and its effects on water flux, porosity, pore size, roughness and tensile strength were examined.

• Membrane Journal
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• v.27 no.2
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• pp.189-198
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• 2017

In this study, we used thermally induced phase separation (TIPS) to produce water treatment membrane and poly(vinylidene fluoride) (PVDF), silica with excellent mechanical properties and chemical resistance to evaluate characterization of the membrane. The diluents used for the characterization were dioctyl phthalate (DOP) and dibutyl phthalate (DBP). We observed the crystallization temperature, cloud point and SEM images to see the manufacture conditions according to the ratio of PVDF and silica. The crystallization temperature and cloud point increased with the contents of silica. Through the phase diagram drawn from these results, the conditions for the preparation of the membrane confirmed.

• Korean Membrane Journal
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• v.9 no.1
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• pp.27-33
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• 2007

PVDF membrane formation via TIPS was performed for PVDF/DBP and PVDF/DMP systems. PVDF/DBP system showed solid-liquid phase separation behavior, while PVDF/DMP system has liquid-liquid phase separation characteristic as well as solid-liquid phase separation characteristic. PVDF contents and cooling conditions had great influence on structure, and the effects of each parameter were examined. Spherulitic structure was obtained due to the dominant PVDF crystallization. Diluent rejected to the outside of spherulite occupied the surface of the PVDF spherulites to result in the microporous spherulite formation and micro-void between spherulites. PVDF/DMP system had competitive solid-liquid and liquid-liquid phase separation depending on the cooling path.