Zhongliang Guo, Yuqin Zhu, Yu Mi, Zhiyong Zhang, Huiying Wen, Lubin Liu, Miaojun Xu and Bin Li
{"title":"基于dopo的含磷热液晶共聚酯阻燃原位增强PBT","authors":"Zhongliang Guo, Yuqin Zhu, Yu Mi, Zhiyong Zhang, Huiying Wen, Lubin Liu, Miaojun Xu and Bin Li","doi":"10.1039/D5NJ02773J","DOIUrl":null,"url":null,"abstract":"<p >In this study, a phosphorus-containing thermotropic liquid crystal copolyester (p-TLCP) was synthesized <em>via</em> melt polycondensation using 2-(6-oxid-6<em>H</em>-dibenzo[<em>c</em>,<em>e</em>][1,2]oxaphosphorin-6-yl)-1,4-benzenediol (DOPO-HQ), terephthalic acid (TPA), <em>p</em>-hydroxybenzoic acid (<em>p</em>-HBA), and dimethyl terephthalate (DMT) as raw materials with a molar ratio of 3 : 3 : 2 : 2. The flame-retardant p-TLCP was subsequently incorporated into polybutylene terephthalate (PBT) to fabricate composites. The thermal properties, flame retardancy, and mechanical performance of the PBT/p-TLCP composites were systematically investigated through limiting oxygen index (LOI), vertical burning (UL-94), and cone calorimetry tests, dynamic thermomechanical analysis (DMA), tensile/impact testing, scanning electron microscopy (SEM), coupled with laser Raman spectroscopy (LRS) and thermogravimetric-Fourier transform infrared (TG-FTIR) spectroscopy. Results revealed that the flame retardancy and mechanical properties of the composites were markedly improved with increasing p-TLCP content. When the p-TLCP addition was 10.0 wt%, the LOI value of the composite increased from 22.0% (pure PBT) to 27.0%, achieving a UL-94 V-0 rating; at a p-TLCP loading of 12.5 wt%, the peak heat release rate (PHRR) and the total heat release (THR) decreased by 22.4% and 35.8% relative to pure PBT, respectively, while the storage modulus and tensile strength were elevated by 22.8% and 19.4%, with impact strength reaching 30.5% enhancement, demonstrating optimal comprehensive performance.</p>","PeriodicalId":95,"journal":{"name":"New Journal of Chemistry","volume":" 38","pages":" 16750-16763"},"PeriodicalIF":2.5000,"publicationDate":"2025-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Flame-retardant in situ reinforced PBT via a DOPO-based phosphorus-containing thermoliquid crystal copolyester\",\"authors\":\"Zhongliang Guo, Yuqin Zhu, Yu Mi, Zhiyong Zhang, Huiying Wen, Lubin Liu, Miaojun Xu and Bin Li\",\"doi\":\"10.1039/D5NJ02773J\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >In this study, a phosphorus-containing thermotropic liquid crystal copolyester (p-TLCP) was synthesized <em>via</em> melt polycondensation using 2-(6-oxid-6<em>H</em>-dibenzo[<em>c</em>,<em>e</em>][1,2]oxaphosphorin-6-yl)-1,4-benzenediol (DOPO-HQ), terephthalic acid (TPA), <em>p</em>-hydroxybenzoic acid (<em>p</em>-HBA), and dimethyl terephthalate (DMT) as raw materials with a molar ratio of 3 : 3 : 2 : 2. The flame-retardant p-TLCP was subsequently incorporated into polybutylene terephthalate (PBT) to fabricate composites. The thermal properties, flame retardancy, and mechanical performance of the PBT/p-TLCP composites were systematically investigated through limiting oxygen index (LOI), vertical burning (UL-94), and cone calorimetry tests, dynamic thermomechanical analysis (DMA), tensile/impact testing, scanning electron microscopy (SEM), coupled with laser Raman spectroscopy (LRS) and thermogravimetric-Fourier transform infrared (TG-FTIR) spectroscopy. Results revealed that the flame retardancy and mechanical properties of the composites were markedly improved with increasing p-TLCP content. When the p-TLCP addition was 10.0 wt%, the LOI value of the composite increased from 22.0% (pure PBT) to 27.0%, achieving a UL-94 V-0 rating; at a p-TLCP loading of 12.5 wt%, the peak heat release rate (PHRR) and the total heat release (THR) decreased by 22.4% and 35.8% relative to pure PBT, respectively, while the storage modulus and tensile strength were elevated by 22.8% and 19.4%, with impact strength reaching 30.5% enhancement, demonstrating optimal comprehensive performance.</p>\",\"PeriodicalId\":95,\"journal\":{\"name\":\"New Journal of Chemistry\",\"volume\":\" 38\",\"pages\":\" 16750-16763\"},\"PeriodicalIF\":2.5000,\"publicationDate\":\"2025-08-29\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"New Journal of Chemistry\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.rsc.org/en/content/articlelanding/2025/nj/d5nj02773j\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"New Journal of Chemistry","FirstCategoryId":"92","ListUrlMain":"https://pubs.rsc.org/en/content/articlelanding/2025/nj/d5nj02773j","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
Flame-retardant in situ reinforced PBT via a DOPO-based phosphorus-containing thermoliquid crystal copolyester
In this study, a phosphorus-containing thermotropic liquid crystal copolyester (p-TLCP) was synthesized via melt polycondensation using 2-(6-oxid-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)-1,4-benzenediol (DOPO-HQ), terephthalic acid (TPA), p-hydroxybenzoic acid (p-HBA), and dimethyl terephthalate (DMT) as raw materials with a molar ratio of 3 : 3 : 2 : 2. The flame-retardant p-TLCP was subsequently incorporated into polybutylene terephthalate (PBT) to fabricate composites. The thermal properties, flame retardancy, and mechanical performance of the PBT/p-TLCP composites were systematically investigated through limiting oxygen index (LOI), vertical burning (UL-94), and cone calorimetry tests, dynamic thermomechanical analysis (DMA), tensile/impact testing, scanning electron microscopy (SEM), coupled with laser Raman spectroscopy (LRS) and thermogravimetric-Fourier transform infrared (TG-FTIR) spectroscopy. Results revealed that the flame retardancy and mechanical properties of the composites were markedly improved with increasing p-TLCP content. When the p-TLCP addition was 10.0 wt%, the LOI value of the composite increased from 22.0% (pure PBT) to 27.0%, achieving a UL-94 V-0 rating; at a p-TLCP loading of 12.5 wt%, the peak heat release rate (PHRR) and the total heat release (THR) decreased by 22.4% and 35.8% relative to pure PBT, respectively, while the storage modulus and tensile strength were elevated by 22.8% and 19.4%, with impact strength reaching 30.5% enhancement, demonstrating optimal comprehensive performance.