• 공업화학
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• 제32권4호
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• pp.449-455
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• 2021

복합재료는 단일물질이 갖는 각각의 특성을 복합화 함으로써 우수한 물성을 갖도록 구성한 물질로 금속 및 고분자의 성능을 뛰어넘는 재료로써 각광받고 있다. 다만, 생산시간이 길고, 단가가 비싼 단점이 있어 이를 극복하기 위해 많은 연구가 진행되고 있다. 본 연구에서는 복합재료의 대량생산 시 시간을 단축할 수 있는 에폭시 수지 경화제를 개발하였고, 난연성을 부여하여 이의 적용성을 확대하고자 하였다. 기본 물질로 사용한 에폭시 수지는 bisphenol F 및 resorcinol 구조의 에폭시 2종을 사용하였으며, 난연성을 부여하기 위하여 9,10-dihydro-9-oxa-10-phosphaphenantrene-10-oxide(DOPO)를 이용하여 변성하였다. 첨가제로는 triethylphosphate (TEP) 및 bis[(5-ethyl-2-methyl-1,3,2-dioxaphosphorinan-5-yl)methyl] methyl phosphonate P,P'-dioxide (FR-001)을 사용하여 7종의 조성물을 배합하였고, 열적 특성(겔화시간, 유리전이온도), 난연 성능을 평가하여 high pressure resin transfer molding (HP-RTM) 공법에 적용 가능한 에폭시 기지재를 개발하였다.

• 공업화학
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• 제24권1호
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• pp.77-81
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• 2013

본 연구에서는 인-할로겐계 난연제가 첨가된 경질 폴리우레탄 폼(PUF)을 합성하여 인-할로겐계 난연제의 종류와 함유량, 노화 가속화 전 후의 열적, 물리적, 난연 특성 등의 변화와 이들의 상관관계를 조사하였다. 난연제로는 Tri(2-chloroethyl) phosphate [TCEP]와 Tris(2-chloropropyl) phosphate [TCPP]를 0, 3, 5, 10, 15, 20, 30%씩 변화시키며 첨가하였다. 난연제의 첨가량이 증가함에 따라 PUF의 reduced compressive strength와 유리전이 온도가 감소하였다. 노화 가속화 후에는 초기 미 반응된 물질의 추가 반응으로 인하여 reduced compressive strength와 유리전이 온도가 증가하였다. SEM과 열전도도 측정을 통하여 TCPP가 TCEP보다 cell의 크기와 분포를 균일하게 하여 TCPP가 첨가된 PUF가 TCEP가 첨가된 PUF 보다 열전도도가 감소 한다는 것을 알 수 있었다. Vacuum oven을 통한 노화가속화 전후의 PUF 난연성을 비교한 결과 노화 후 PUF의 발화 시간은 감소하고 연소 거리가 증가하여 난연성이 현저히 감소함을 확인하였다.

• 한국응용과학기술학회지
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• 제20권4호
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• pp.275-282
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• 2003

Aqueous polyurethane dispersion was synthesized using phosphorus compound which received significant attention for the replacement of halogenated flame retardants. In this study, polyols which have phosphorus moity in their structural unit were synthesized by two-step polycondensation reaction using dimethyl phenylphosphonate, ethylene glycols. adipic acid, and 1,4-butanediol. In the next step, polyurethane dispersion was prepared using these polyols, isophorone diisocyanate with dimethyl propionic acid. The particle size of polyurethane latex was reduced from 347 nm to 240 nm with increasing DMPA content. It was observed that the LOI values of prepared coatings increased from 27% to 35% with increasing phosphorus content.

• 한국응용과학기술학회지
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• 제23권1호
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• pp.26-36
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• 2006

The aim of this study is to synthesis basic resins for the preparation of PU flame-retardant coatings that contain phosphorus and chlorine. After synthesizing intermediates of tetramethylene bis(orthophophate) (TMBO) and neohexanediol trichlorobenzoate (TBA-adduct), the condensation polymerization was performed with the intermediates, 1,4-butanediol, and adipic acid to obtain four-component copolymers. In the condensation polymerization, the content of phosphorus was fixed to be 2%, and the content of trichlorobenzoic acid (TBA) that provides chlorine component was varied to be 10, 20, and 30wt%, and we designated the prepared modified polyesters containing chlorine and phosphorus as TTBA-10C, TTBA-20C and TTBA-30C. Average molecular weight and polydispersity index of the prepared TTBAs decreased with increasing TBA content because of the increase in the number of hydroxyl groups that retards reaction. We found that the thermal stability of the prepared TTBAs increased with chlorine content at high temperatures.

• 한국염색가공학회지
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• 제24권1호
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• pp.33-38
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• 2012

In this study, to increase flame retardation of poly(ethylene terephthalate) (PET) in burning, bisphenol A bis(diphenyl phosphate) (BDP), a well known flame retardant containing phosphorous, was reacted on end groups of PET by radical pathway. End-capping mechanism of PET with BDP was suggested and confirmed by spectroscopic and thermal analysis. From 400 MHz $^{31}P$ solid state FT-NMR spectrum of end-capped PET (PET-BDP), phosphorus spectra peak in BDP was found at ca. -20 ppm. Furthermore, P-C bond stretching vibration peaks were found ca. $600cm^{-1}$ in FT-IR spectrums of PET-BDP. These results showed that BDP can be chemically added on end groups of PET by our method. Thermal characteristics of pure PET (pPET) and PET-BDP were measured and evaluated by TGA analysis. There was not significant changes in thermal characteristics of PET-BDP compared to that of pPET.

• 한국염색가공학회지
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• 제24권1호
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• pp.39-44
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• 2012

To improve flame retardation of poly(ethylene terephthalate) (PET) against burning, resorcinol bis(diphenyl phosphate) (RDP), phosphorous containing flame retardant, was incorporated into PET backbone by radical reaction pathway. Radical endcapping of PET with RDP was confirmed by spectroscopic and thermal analysis. From 400 MHz $^{31}P$ solid state FT-NMR spectrum of PET with RDP (PET-RDP), phosphorus spectra peak in RDP was found at ca. -10 ppm. Furthermore, P-C bond stretching vibration peaks were found ca. $530cm^{-1}$ in FT-IR spectrums of PET-RDP. These results indicated that RDP can be chemically bound at the ends of PET by radical addition method. Thermal characteristics of pure PET (pPET) and PET-RDP were measured and evaluated by TGA thermal analysis. There was not significant changes in thermal characteristics of PET-RDP compared to that of pPET.

• 한국염색가공학회지
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• 제33권2호
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• pp.64-71
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• 2021

Large amount of formaldehyde could be released inevitably during the flame-retardant (FR) treatments or from the finished fabrics using Provatex reagent and Proban polymers which have been used as durable FRs for cotton. A water-soluble cyclophosphazene derivative was synthesized as an ecofriendly phosphorus-based FR for cotton fibers. Dichloro tetrakis{N-[3-(Dimethylamino)propyl]methacrylamido} cyclcophosphazene (DCTDCP) was synthesized through the substiutution reaction of Hexachloro cyclophosphazene and N-[3-(Dimethylamino)propyl] methacrylamide at a mole ratio of 1 : 4, which can be cured dually by both alkaline treatment and UV irradiation. More crosslinked networks were produced through the addition of Triacryloyl hexahydrotriazine and Acrylamide as a UV-curable crosslinker and a comonomer respectively. Both flame retardancy and washing durability of the FR cotton were improved synergistically. The durability improvement may be caused by the covalent bond formation of the FR with cellulose and the high degree of polymerization of DCTDCP, which can be verified by the pyrolysis and combustion behaviors analyzed by LOI, TGA, and microcalorimeter.

• 한국건축시공학회지
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• 제21권2호
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• pp.113-119
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• 2021

고분자는 고유의 경량성 및 강성으로 인해 건축 자재에 두루 적용되는 소재이다. 그러나 건축 산업에서 빈번히 발생하는 화재 사고에서 대형 화재로의 확산을 일으키는 가장 큰 원인 중 하나가 가연 특성을 지니는 고분자라고 할 수 있다. 따라서 이를 해결하기 위한 방안으로 고분자 소재에 난연제를 첨가하여 난연 특성을 부여하는 연구가 활발히 진행되고 있는 추세이다. 이 중에서도 유기 인계 난연제는 고분자와의 혼화성이 우수하며, 독성이 낮은 장점을 가지고 있어 많은 주목을 받고 있다. 이에 따라 본 연구에서는 건축자재용으로 사용되는 친환경 고분자인 폴리락타이드의 난연성능을 확보하기 위하여 알콕시아민 기반의 유기 인계 난연제 구조를 설계 및 합성하여 이의 효과를 확인하는 것을 목적으로 둔다.

• 한국응용과학기술학회지
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• 제21권1호
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• pp.51-61
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• 2004

Reaction intermediates PCP/BZA (PBI) and tetramethylene bis(orthophosphate) (TBOP) wer synthesized from polycaprolactone (PCP) and benzoic acid (BZA) and from pyrophosphoric acid and 1,4-butanediol, respectively. Benzoic acid modified polyesters containing phosphorus (APTB-5, -10, -15) were synthesized by polycondensation of the prepared PBI (containing 5, 10, 15wt% of benzoic acid), TBOP, adipic acid, and 1,4-butanediol. The structure and characteristics of APTBs were examined using FT-IR, NMR, GPC, and TGA analysis. The increase of the amount of BZA in the synthesis of APTBs resulted in decrease in average molecular weight and kinematic viscosity. From the TGA analysis of APTBs, it was found that the afterglow decreased with the amount of BZA content at the high temperatures.

• 한국응용과학기술학회지
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• 제24권2호
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• pp.182-189
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• 2007

Used polyurethane was chemically degraded by treatments with flame retardants such as tris(3-chloropropyl) phosphate (TCPP), triethyl phosphate (TEP), and trimethyl phosphate (TMP). The structure of degraded products (DEP) was analyzed by FT-IR and P-NMR and it turned out to be phosphorus containing oligourethanes. Rigid polyurethane foam was produced by using the degraded products (DEP) as flame retardants. The flammability of recycled rigid polyurethane was investigated. The recycled polyurethane shows a reduced flammability over virgin polyurethane. In order to evaluate flame retardant properties of the recycled polyurethane foams with various amounts of DEP, the combustion parameters of the foam was measured by a cone calorimeter. Scanning electron micrograph of recycled PU shows the same uniform cell morphology as virgin PU.