• 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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• 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.

• 한국응용과학기술학회지
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• 제19권1호
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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%.

• 한국응용과학기술학회지
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• 제22권2호
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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.

• 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.

• Transactions on Electrical and Electronic Materials
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• 제14권1호
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• pp.1-8
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• 2013

The present approach shows the use of nano-silica/nano-alumina in polyurethane (PU) matrix, which lead to significant improvements in the mechanical and thermal properties of the nano-composite. It is observed that with incorporation of 1% of nano-alumina into the PU matrix, there is an improvement in the tensile strength of around 50%, and for nano-silica the improvement is around 41%, at the same concentration. The morphological data shows that above 3% of the nano particles there are agglomerations in the nanocomposite. Again with the absorption of moisture, there is a decrease in the thermal and mechanical properties of the PU resin, but in this research work it is observed that with the incorporation of the nano particles, in the presence of absorbed moisture there is an improvement in mechanical and thermal properties of the composite, over that of the PU matrix.

• 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.

• Corrosion Science and Technology
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• 제4권1호
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• pp.15-18
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• 2005

Hydroxyapatite(HAp) was synthesized using the waste sludge from semiconductor process and used as an anticorrosive pigment. The water absorption of coating pigmented with anticorrosive pigment and the corrosion at interface between coating and substrate were monitored using AC impedance techniques. The anticorrosive performance of HAp was compared with those of red lead(RL) and zinc potassium chromate(ZPC), which have been known as representative anticorrosive pigments. The amount of absorbed water in ZPC- and HAp- pigmented coatings was much higher compared to that in RL-pigmented and unpigmented film. However, it seems that the water absorbed into HAp- or ZPC-pigmented film is beneficial to anticorrosive function. The anticorrosive performance of HAp is superior or at least comparable to those of ZPC and RL. The excellent anticorrosive properties of HAp can be explained by its passivating ability, caused by the reaction of the soluble component of HAp with Fe to form iron phosphate in the presence of water.

• 한국응용과학기술학회지
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• 제23권2호
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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.

• 한국응용과학기술학회지
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• 제24권3호
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• pp.287-295
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• 2007

Three phosphorus functional groups were introduced in one structural unit of polymer backbone to enhance the flame retardancy of PU coatings. In the first step, we synthesized tetramethylene bis(orthophosphate) (TBOP) that contained two phosphorus functional groups in one structural unit. In the next step, we synthesized modified polyesters (ATBTP-10C, -20C, -30C) that contained triphosphorus group using TBOP, 1,4-butanediol, trimethylolpropane, adipic acid, and another functional monomer, phenylphosphonic acid (PPA). The amount of PPA in ATBTPs was adjusted from 10 wt% to 30 wt%. The structure and characteristics of ATBTPs were examined using FT-IR, NMR, GPC, and TGA analysis. From the thermo-behavior test of diphosphorus modified polyester (ATBT) and ATBTPs, the afterglow of ATBT, ATBTP-10C, ATBTP-20C, and ATBTP-30C were 24.7, 27.1, 29.0, and 31.7%, respectively. It was found from this result that the afterglow increased with the amount of PPA component.