• Polymer(Korea)
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• v.26 no.2
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• pp.193-199
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• 2002

The dichloro-polyester polyol (DCBAO) which was synthesized in our earlier work was cured at room temperature with two different type of curing agents including Desmodur N-3300 and Desmodur L-75 to get a polyurethane flame-retardant coatings (DCBAO/N-3300=DEBAN and DCBAO/L-75=DCBAL). We could not observe any deterioration of physical properties of the flame-retardant PU coatings (UCBAN and DCBAL) in comparison with the conventional PU coatings. Thermal resistance of DCBAL-type flame-retardant coatings, which was measured by yellowness index difference, was inferior to that of DCBAL-type PU coatings. We believe that this phenomena is attributed to the poor thermal resistance of Desmodur L-75 isocyanate. It was observed that the LOI values were 25∼26% for the PU coatings containing 20∼30 wt% of 2,4-dichlorobenzoic acid.

• Polymer(Korea)
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• v.25 no.3
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• pp.391-398
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• 2001

Two-component polyurethane (PU) flame-retardant coatings were prepared by blending tribromo modified polyesters ($TBAO_s$) and isocyanate.$TBAO_s$ were synthesized by condensation polymerization of tribromoacetic acid, a flame-retardant component, with 1,4-butanediol, adipic acid, and trimethylolpropane. The content of tribromoacetic acid was varied by 10, 20, and 30 wt% for the reaction. Various physical properties of these new flame-retardant coatings were comparable to nonflame-retardant coatings. Coatings with 20 wt% tribromoacetic acid did not burn during the vertical burning test.

• Journal of the Korean Applied Science and Technology
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• v.20 no.2
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• pp.110-117
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• 2003

Pyrophosphoric modified polyesters (TATBs) were synthesized by polycondensation of adipic acid, trimethylolpropane, 1,4-butanediol, and tetramethylene bis(orthophosphate). Two-component PU flame-retardant coatings (TATBCs) were prepared by blending TATBs with HDI-Biuret. Most of the physical properties of the flame-retardant coatings were comparable to those of non-flame-retardant coatings. Coatings containing 10 and 15wt% 1,4-butanediol, TATBC-10C and TATBC-15C were not flammable in the vertical flame-retardancy test.

• Journal of the Korean Applied Science and Technology
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• v.22 no.1
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• pp.1-8
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• 2005

Chlorine-containing modified polyester polyols were synthesized by two-step condensation reactions. Intermediate was synthesized by the esterification of monochloroacetic acid with trimethylolpropane in the first step. Polycondensation of the intermediate (MCAOs), 1,4-butanediol, and trimethylolpropane with adipic acid was carried out. Two-component polyurethane (PU) coatings were prepared by blending MCAOs and IPDI-isocyanurate. There new flame-retardant coatings showed various properties comparable to other non-flame-retardant coatings. They were superior to flammable coatings from the experimental results showing rapid and 10 to 13 hours of pot-life. Coatings with 30wt% monochloroacetic acid was not flammable by the vertical flame retardancy test.

• Journal of the Korean Applied Science and Technology
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• v.23 no.4
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• pp.328-339
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• 2006

The PU flame-retardant coatings (TTBAH, ATBAH-10C, -20C, and -30C) were prepared using the synthesized ATBAs and HDI-trimer as curing agent at room temperature. The physical properties of PU flame-retardant coatings with chlorine and phosphorus were inferior to those with phosphorus only and the properties were getting worse with increasing chlorine content. Flame retardancy was tested with three methods. With the vertical method, complete combustion time of ATBAHs were $259^{\sim}347$ seconds, which means that the prepared coatings are good flame-retardant. With the $45^{\circ}$ Meckel burner method, char lengths of the three prepared coatings were less than 2.9 cm, which indicates that the prepared coatings are first grade. With the limiting oxygen index (LOI) method, the LOI values of the three prepared coatings were in the range of $30^{\sim}35%$, which proves good flame retardancy of the prepared coatings. from the result of flame retardancy tests of the specimens that contain the same amounts of flame retarding compounds. it was found that the coatings containing both phosphorus and chlorine show higher flame retardancy than the coatings containing only phosphorus. This indicates that there exists, some synergy effect between coexisting phosphorus and chlorine.

• Journal of the Korean Applied Science and Technology
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• v.25 no.3
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• pp.332-340
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• 2008

Two component polyurethane (PU) flame retardant coatings were prepared by blending trichloro modified polyesters (TCMPs) and isophorone diisocyanate isocyanurate. TCMPs were synthesized by polycondensation of trichlorobenzoic acid (TCBA), a flame retardant component, with adipic acid, 1,4 butanediol, and trimethylolpropane. The content of TCBA was varied in 10, 20, and 30 wt% for the reaction. Theses new flame retardant coatings showed various properties comparable to other non flame retardant coatings. Moreover, we carried out the combustion test and the flammability test for our flame retardant coatings. The results of vertical burning test for the coatings containing more than 20 wt% of TCBA were determined as no burn. The results of flammability test for the coatings with 20 wt% and 30 wt% of TCBA contents indicated the limiting oxygen index (LOI) values of 26% and 29% respectively, which implied relatively good flame retardancy.

• 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.3
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• pp.270-280
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• 2005

To maximize a synergy effect in flame-retardancy of flame-retardant coatings, phosphorus and chlorine were introduced in polymer chains. Two-components PU flame-retardant modified polyesters (ABTTC-10C, -20C, -30C) were prepared by curing, at room temperature, of isocyanate (allophanate-trimer) and prepared modified polyesters which contain phosphorus and chlorine. To examine the film properties of the prepared flame-retardant coatings, film specimens were prepared with the prepared coatings. The film properties of ABTTC, ABTTC-10C and ABTTC-20C, which contain 0, 10 and 20wt%, 2,4-dichlorobenzoic acid (2,4-DCBA), respectively, were proved to be good, whereas the film properties of ABTTC-30C, which contains 30wt% 2,4-DCBA, were proved to be a little bit poor. Two kinds of flame retardancy tests, $45^{\circ}$Meckel burner method and LOI method, were performed. With the $45^{\circ}$Meckel burner method, three flame-retardant coatings except ABTTC showed less than 3.4 cm of char length, and showed less than 2 seconds of afterflaming and afterglow. From this result, the prepared flame-retardant coatings were proved to have the 1st grade flame retardancy. With the LOI method, the LOI values of the coatings containing more than 10wt% 2,4-DCBA were higher than 30wt%, which means that the coatings possess good flame-retardancy. From these results, it was found that synergistic effect in flame-retardancy was taken place by the introduced phosphorus and chlorine.

• Journal of the Korean Applied Science and Technology
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• v.23 no.3
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• pp.264-271
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• 2006

PU type flame-retardant coatings (TBAO/L-75, TBAOL ; TBAO/N-100, TBAON) were prepared by blending bromine-containing modified polyester (TBAO) which was synthesized in our earlier work. with two kinds of isocyanate curing agents, Desmodur L-75 and Desmodur N-100. Physical properties of the prepared flame-retardant coatings were tested. TBAOL shows better hardness than TBAON, while TBAON shows better viscosity, accelerated weathering resistance, yellowness index and lightness index difference than TBAOL. There were no remarkable differences in fineness of grind, $60^{\circ}$ specular gloss, cross-hatch adhesion, and abrasion resistance of TBAOL and TBAON. There was no discernable difference in flame-retardancy between the two flame-retardant coatings, TBAOL and TBAON. When the content of tribromo acetic acid, which is flame-retarding component, was 30wt% the LOI value was in a range of $29{\sim}30%$, which indicates that the two coatings are good flame-retardant coatings.

• Journal of the Korean Applied Science and Technology
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• v.24 no.2
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• pp.124-139
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• 2007

In order to obtain the maximum flame retardancy with the minimal deterioration of physical properties of PU flame-retardant coatings, chlorine and phosphorous 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 kind of intermediates to obtain copolymer. The modified polyesters containing chlorine and phosphorous (ATBA-10C, -20C, and -30C) were synthesized by adjusting the contents of chlorine compound (dichloroacetic acid, 10, 20, 30 wt%) with fixed the content of phosphorous compound (2 wt%). The PU flame-retardant coatings (TTBAH -10C, -20C, and -30C) were prepared using the synthesized ATBAs and HDI-trimer as curing agent at room temperature. The physical properties of PU flame-retardant coatings with chlorine and phosphorous were inferior to those with phosphorous only and the properties were getting worse with increasing chlorine content. Flame retardancy was tested with three methods. With the vertical method, Complete combustion time of ATBAHs were $259^{\sim}347$ seconds, which means that the prepared coatings are good flame-retardant. With the $45^{\circ}$ Meckel burner method, char lengths of the three prepared coatings were less than 2.9 cm, which indicates that the prepared coatings are 1st grade flame retardancy. With the limiting oxygen index (LOI) method, the LOI values of the three prepared coatings were in the range of $30^{\sim}35%$, which proves good flame retardancy of the prepared coatings. From the results of flame retardancy tests of the specimens that contain the same amounts of flame retarding compounds, it was found that the coatings containing both phosphorous and chlorine show higher flame retardancy than the coatings containing phosphorous alone. This indicates that some synergy effect of flame retardancy exists between phosphorous and chlorine.