• 한국응용과학기술학회지
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• 제25권2호
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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.

• 폴리머
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• 제27권3호
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• pp.169-175
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• 2003

무독성의 반응형 난연 도료를 제조할 목적으로 모체수지 1개의 구조단위 속에 2개의 인산기를 보유한 파이로포스포릭 락톤 변성 폴리에스터 (PATT)를 합성하고, PATT에 이소시아네이트인 toluene diisocyanate-isocyanurate를 상온경화시켜 2성분계 폴리우레탄 난연 도료(PIPUC)를 제조하였다. PIPUC로서 도막제작 후 비난연 도료와의 도막물성을 비교한 결과 난연 성분 도입에 따른 난연 도료의 물성이 저하되지 않음을 알았다. 난연성 시험 중 45$^{\circ}$ Meckel burner 법에서는 탄화길이가 3.1~4.4 cm를, LOI법에서는 LOI 27~30%를 각각 나타냄으로써 양호한 난연 효과를 보여주었고, SEM에 의한 표면 도막을 관찰한 결과 도막의 결함이나 상분리 현상이 생기지 않음을 관찰하였다.

• 한국응용과학기술학회지
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• 제22권3호
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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.

• 한국응용과학기술학회지
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• 제24권1호
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• pp.31-46
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• 2007

This study was focused on the maximization of flame-retardancy of polyesters by a synergism of simultaneously introduced chlorine and phosphorus into polymer chains of modified polyesters. To prepare modified polyesters, reaction intermediates, TD-adduct (prepared from trimethylolpropane/2,4-dichlorobenzoic acid (2,4-DCBA)) and TMBO (prepared from tetramethylene bis(orthophosphate)), were prepared first, then condensation polymerization of the prepared intermediates, adipic acid, and 1,4-butanediol were carried out. In the condensation polymerization, the content of phosphorus was fixed to be 2%, and the content of 2,4-DCBA that provides chlorine component was varied to be 10, 20, and 30wt%, and we designated the prepared modified polyesters containing chlorine and phosphorus as ABTT-10C, -20C, -30C. Two-component PU flame-retardant coatings (ABTTC, ABTTC-10C, ABTTC-20C, ABTTC-30C) were prepared by the curing of synthesized ABTTs with a curing agent of allophanate/trimer at room temperature. To examine the film properties of the prepared PU 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-DCBA, respectively, were proved to be good, whereas the film properties of ABTTC-30C, which contains 30wt% 2,4-DCBA, was proved to be a little bit poor. Two kinds of flame retardancy tests, $^{\circ}45Meckel$ burner method and LOI method were performed. With the $^{\circ}45Meckel$ burner method, three flame-retardant coatings except ABTTC showed less than 3.4cm 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 30%, 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.

• 폴리머
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• 제30권3호
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• pp.238-246
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• 2006

본 연구에서는 인과 염소를 공유한 폴리우레탄(PU) 난연도료를 제조하여 인과 염소기의 시너지 효과에 의해 난연성을 더욱 향상시키는데 그 연구목적을 두었다. 합성은 tetramethylene bis (orthophosphate) 중간생성물(TMBO)과 neohexanediol trichlorobenfoate 중간생성물(TBA-adduct)인 이들 2종류 중간생성물과 1,4-butanediol 및 adipic acid의 4종류 단량체를 축합중합을 수행하여 4원공중합물(TTBA)을 얻은 다음, 합성된 TTBA류와 hexamethylene diisocyanate(HDI)-trimer인 경화제를 상온경화시켜 2성분계 PU 난연도료(TTBA-10C/ HDI-trimer=TTHD-10C, TTBA-20C/HDI-trimer=TTHD-20C, TTBA-30C/HDI-trimer=TTHD-30C)를 제조하였다. 제조된 TTHD류의 난연도료로서 도막시편을 제작하여 도막물성 측정용 시료로 사용하였다. 도막물성 측정 결과, 전반적으로 인 단독 함유보다 인과 염소를 공유한 쪽의 도막물성이 저하되는 경향을 나타내었다. 또한 난연성 시험으로서 수직법과 수평법의 연소성 시험법 및 $45^{\circ}$ Meckel burner법을 선정하여 난연성을 알아본 결과, 인 단독 함유보다 인과 염소를 공유한 TTHD류 쪽의 난연성이 더 좋게 나타난 것으로 보아 인과 염소에 의한 난연 시너지 효과가 일부 일어남을 인지할 수 있었다.

• 한국응용과학기술학회지
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• 제21권1호
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• pp.62-68
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• 2004

PU flame-retardant coatings (APHD) containing phosphorous were prepared by blending of hexamethylene diisocyanate-trimer, white pigment, dispersing agent, flowing agent, and previously prepared benzoic acid modified polyester (APTB) that contains phosphorous. Physical properties of the prepared APHD were examined. With the introduction of BZA (contained in APTB), 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, and in a $45^{\circ}$ Meckel burner method, shows 1.3${\sim}$4.0$cm^2$ of char length, 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.

• 한국응용과학기술학회지
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• 제23권3호
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• pp.252-263
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• 2006

It is attempted to develop flame retardant polyurethane coatings, which have received significant attention in recent years. It is the purpose of this study to synthesize new reactive polyurethane coatings containing halogen. Lactone based modified polyester polyols, using trichlorobenzoic acid as chlorine moiety (TBAOs) were synthesized. These polyesters were cured with isophorone diisocyanate (IPDI)-isocyanurate at room temperature (TBAPUs). Physical properties of these flame retardant coatings were similar with those of non-flame retardant coatings. The flammability of coatings was strongly dependent on the chlorine contents. We found that the increasing chlorine contents showed better flame retarding properties and that, however, they also resulted in more smog generation during combustion. The detailed results of flammability test using various methods indicated $24{\sim}26%$ in LOI and $3.7{\sim}5.3\;cm$ char length in $45^{\circ}$ Meckel burner method.

• 한국응용과학기술학회지
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• 제17권3호
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• pp.203-211
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• 2000

Pyrophosphoric lactone modified polyester(PATT) that contains two phosphorous functional groups in one unit base resin structure was synthesized to prepare a non-toxic reactive flame retardant coatings. Then the PATT was cured at room temperature with isocyanate, Desmodur IL, to get a two-component polyurethane flame retardant coatings(PIPUC). Comparing the physical properties of the films of PIPUC with the film of non-flame retardant coatings, there was no degradation observed in physical properties by the introduction of a flame-retarding component into the resin. We found that the char lengths measured by $45^{\circ}$Meckel burner method were $3.1{\sim}4.4cm$ and LOI values recorded $27{\sim}30%$. These results indicate that the coatings prepared in this study is good flame retardant one. The surface structure of coatings investigated with SEM does not show any defects and phase separation.

• 한국응용과학기술학회지
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• 제23권4호
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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.

• 한국응용과학기술학회지
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• 제23권1호
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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.