• Journal of the Korean Applied Science and Technology
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• v.19 no.1
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• pp.25-32
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• 2002

Two PU flame-retardant coatings, 2,3-DBPO/N-l00 (DBPON) and 2,3-DBPO/IL (DBPOI), were prepared by curing 2,3-dibromo modified polyester (2,3-DBPO) with isocyanate curing agent Desmodur N-l00 (or Desmodur IL) at room temperature. The physical properties and flame-retardancy of the two coatings were tested and compared. As a result, the pot-life, yellowness index, lightness index difference, $60^{\circ}$ specular gloss, cross-hatch adhesion, viscosity, and accelerated weathering resistance of DBPON were better than those of DBPOI; the fineness of grind of the two coatings were the same; and the drying time, hardness, and abrasion resistance of DBPOI were better than those of DBPON. The flame retardancy of the flame-retardant coatings increased with the content of the flame retarding component, 2,3-dibromopropanoic acid (2,3-DBP); and the LOI values of the two coatings were in a range of $27{\sim}29%$ when the content of 2,3-DBP was 30wt%.

• Journal of the Korean Applied Science and Technology
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• v.23 no.1
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• pp.77-84
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• 2006

Modified polyesters (TTBA-10C, -20C, -30C) that contain phosphorus and chlorine were synthesized by the condensation polymerization of tetramethylene bis(orthophosphate), neohexanediol trichlorobenzoate, 1,4-butanediol and adipic acid, in which tetramethylene bis(orthophosphate) and neohexanediol trichlorobenzoate were prepared previously in our laboratory. In this study, two-component flame-retardant polyurethane coatings (TTBA-10C/HDI-trimer=TTHD-10C, TTBA-20C/ HDI-trimer= TTHD-20C, TTBA-30C/HDI-trimer= TTHD-30C) were obtained by curing at room temperature with the synthesized TTBAs and hexamethylene diisocyanate (HDI)-trimer as a curing agent. The obtained TTHDs were made into coating samples and used as test samples for various physical properties. The physical properties of the flame-retardant coatings containing chlorine and phosphorus groups were generally inferior to those containing only phosphorus group. Flame retardancy was tested by vertical and horizontal combustion method, and $45_{\circ}$ Meckel burner method. Since the retardancy of flame-retardant coatings containing chlorine and phosphorus groups was better than that containing only phosphorus group, it could be concluded that the retardancy by the synergism effect of chlorine and phosphorus groups exhibited.

• Journal of the Korean Society of Safety
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• v.26 no.4
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• pp.47-58
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• 2011

Halogen free intumescent flame retardants(IFRS), such as the mixture of melamine phosphate(MP) and char forming agents(pentaerythritol(PER), di-pentaerythritol(DiPER), tris(2-hydroxyethyl) isocyanurate(THEIC)), were prepared and characterized. Polypropylene(PP)/$IFR_S$ composites were also prepared in the presence of ethylene diamine phosphate(EDAP) as a synergist and used into flame retardant PP powder coatings. Thermoplastic PP powder coatings at 20 wt% flame retardant loading were manufactured by extruded and then mechanical cryogenic crushed to bring them in fine powder form. These intumescent flame retardant powder coatings($IFRPC_S$) were applied on mild steel surface for the purpose of protection and decorative. It is a process in which a $IFRPC_S$ particles coming in contact with the preheated mild steel surface melt and form a thin coating layer. The obtained MP flame retardant was analyzed by utilizing FTIR, solid-state $^{31}P$ NMR, ICP, EA and PSA. The mechanical properties as tensile strength, melt flow index(MFI) and the thermal property as TGA/DTA and the fire safety characteristics as limiting oxygen index(LOI), UL94 test, SEM were used to investigate the effect of $IFRPC_S$. The experimental results show that the presence of $IFR_S$ considerably enhanced the fire retardant performances as evidenced by the increase of LOI values 17.3 vol% and 32.6 vol% for original PP and $IFRPC_S$-3(PP/MP-DiPER/EDAP), respectively, and a reduction in total flaming combustion time(under 15 sec) in UL94 test of $IFRPC_S$. The prepared $IFRPC_S$-3 have good comprehensive properties with fire retardancy 3.2 mm UL94 V-0 level, LOI value 32.6%, tensile strength $247.3kg/cm^2$, surface roughness Ra $0.78{\mu}m$, showing a better application prospect. Through $IFRPC_S$-2(PP/MP-PER/EDAP) and $IFRPC_S$-3 a better flame retardancy than that of the $IFRPC_S$-1(PP/MP/EDAP) was investigated which was responsible for the formed more dense and compact char layer, improved synergy effect of MP and PER/DiPER.

• Journal of the Korean Applied Science and Technology
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• v.25 no.2
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• pp.151-159
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• 2008

The flame-retardant coatings were prepared by blending the synthesized triphosphorus modified polyester in the previous paper and hexamethylene diisocyanate-trimer and curing it at room temperature. The characterization of the films of the prepared coatings was performed. It was confirmed that no deterioration of physical properties of PU coatings was observed with the increasing phenylphosphonic acid (PPA) contents. Flame retardancy was tested by a $45^{\circ}$ Meckel burner method and LOI method. With the $45^{\circ}$ Meckel burner method, CATBTP-20C and CATBTP-30C that contain 20 wt% and 30 wt% of PPA, flame retarding component, respectively, showed the first grade flame retardancy with $2.8{\sim}3.9\;cm$ of char length ; and, with LOI method, they exhibited a good flame retardancy as a range of $30{\sim}32%$ of combustion values.

• Journal of the Korean Applied Science and Technology
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• v.22 no.2
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• pp.123-135
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• 2005

Reaction intermediates PCP/BZA (PBI) and tetramethylene bis(orthophosphate)(TBOP) were synthesized from polycaprolactone (PCP) and benzoic acid (BZA) and from pyrophosphoric acid and 1,4-butanediol, respectively. Benzoic acid modified polyesters containing phosphorus (APTB-S, -10, -15) were synthesized by polycondensation of the prepared PBI (containing 5, 10, 15wt% of benzoic acid), TBOP, adipic acid, and 1,4-butanediol. Network structured PU flame-retardant coatings (APHD) were prepared by curing the synthesized benzoic acid modified polyesters containing phosphorus (APT B - 5 , -10, -15) with hexamethylene diisocyanate (HDI)-timer. From the TGA analysis of APTBs, it was found that the afterglow decreased with the amount of BZA content at the high temperatures. With the introduction of BZA, the film viscosity and film hardness of APHD decreased. With the introduction of caprolactone group, the flexibility, impact resistance, accelerated weathering resistance of APTBs increased. Flame retardancy of the coatings was tested. In a vertical burning method, APHD shows 210$^{\sim}$313 seconds, which indicates that the coatings are good flame-retardant coatings. Moreover, the amount of afterglow and flame retardancy of the coatings are decreased with increasing BZA content.

• Polymer(Korea)
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• v.30 no.3
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• pp.238-246
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• 2006

The aim of this study is to enhance the flame retardancy by the synergism effect of chlorine and phosphorus groups. The flame-retardant polyurethane coatings containing chlorine and phosphorus compounds were synthesized. After synthesizing the intermediate products of tetramethylene bis (orthophosphate) (TMBO) and neohexanediol trichlorobenzoate (TBA-adduct), the condensation polymerization was performed with four different monomers of two intermediates, 1,4-butanediol, and adipic acid to obtain four-component copolymer(TTBA). The two-component flame-retardant polyurethane coatings (TTBA-10C/HDI-trimer=TTHD-10C, TTBA-20C/HDI-trimer=TTHD-20C, TTBA-30C/HDI trimer=TTHD-30C) were obtained by curing reaction at room temperature with the synthesized TTBAs and hexamethylene diisocyanate (HDI)-trimer as a curing agent. The obtained TTHDs were made into coating samples and used as test samples for various physical properties. The physical properties of the flame-retardant coatings containing chlorine and phosphorus groups were generally inferior to those containing only phosphorus group. Flame retardancy was tested by vortical and horizontal combustion method, and $45^{\circ}$ Meckel burner method. Since the retardancy of flame-retardant coatings containing chlorine and phosphorus groups was better than that containing only phosphorus group, it could be concluded that the retardancy by the synergism effect of chlorine and phosphorus groups exhibited.

• Journal of the Korean Applied Science and Technology
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• v.23 no.2
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• pp.99-109
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• 2006

In order to obtain the maximum flame retardancy as well as the minimum deterioration of physical properties of PU flame-retardant coatings, chlorine and phosphorus functional groups were introduced into the pre-polymer of modified polyesters. In the first step, the tetramethylene bis(orthophosphate) (TBOP) and neohexanediol dichloroacetate (DCA-adduct) intermediates were synthesized. In the second step, 1,4-butanediol and adipic acid monomers were polymerized with the two kinds of intermediates to obtain copolymers. The modified polyesters containing chlorine and phosphorus (ATBA-10C, -20C, and -30C) were synthesized by adjusting that the content of phosphorus compound was fixed as 2wt% and the contents of chlorine compound (dichloroacetic acid) were varied as 10, 20, and 30wt%. Average molecular weight and polydispersity index of the preparation of ATBAs were decreased with increasing DCA content because of the increase in hydroxyl group that retards reaction.

• Journal of the Korean Applied Science and Technology
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• v.21 no.1
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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.

• Journal of the Korean Applied Science and Technology
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• v.23 no.1
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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.

• Journal of the Korean Applied Science and Technology
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• v.24 no.4
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• pp.319-331
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• 2007

The aim of this study is to enhance the flame retardancy by the synergism effect of phosphorus and bromine groups. The flame-retardant polyurethane coatings containing phosphorus and bromine compounds were synthesized. After synthesizing the intermediate products of tetramethylene bis(orthophosphate) (TBOP) and trimethylolpropane/2,3-dibromopropionic acid (2,3-DBP) [2,3-DBP-adduct], the condensation polymerization was performed with four different monomers of two intermediate products, 1,4-butanediol, and adipic acid to obtain four-components copolymer. In the condensation polymerization, the content of phosphorus was fixed to be 2wt%, and the content of 2,3-DBP that provides bromine component was varied to be 10, 20, and 30wt%, and we designated the prepared modified polyesters containing phosphorus and bromine as DTBA-10C, -20C, -30C. Average molecular weight and polydispersity index of the preparation of DTBAs were decreased with increasing 2,3-DBP content because of increase of hydroxyl group that retards reaction. We found that the thermal stability of the prepared DTBAs increased with bromine content at high temperature.