Pub Date : 2024-06-07DOI: 10.1177/09540083241259449
Nanyang Ding, Chengzhong Wang
Bisphenol A-based phthalonitrile resin was synthesized by nucleophilic substitution reaction from bisphenol A and 4-nitrophthalonitrile, and then the obtained resin was cured with sulfaguanidine as a novel curing agent. The curing characteristics, kinetics, thermal stability and dynamic mechanical property were studied by standard thermal analysis techniques including DSC, TGA, and DMA. The peak temperature of exothermic peak ( Tp) and apparent activation energy ( Ea) of sulfaguanidine cured phthalonitrile resin were 263.20°C and 76.6 kJ·mol−1 respectively, much lower than those of traditional aromatic diamine cured resin. Moreover, the resin cured by sulfaguanidine showed excellent thermomechanical properties and thermal stability. The glass transition temperature ( Tg) was 284.8°C, the initial thermal decomposition temperature ( Td,5%) was 439.6°C, and the char yield at 800°C was 62.1% in nitrogen atmosphere. To sum up, organic guanidine cured phthalonitrile resin exhibits excellent curing characteristics (low Tp and Ea) and high thermal properties, which provides a promising approach to preparing phthalonitrile resin with high comprehensive performance.
以双酚 A 和 4-硝基邻苯二甲腈为原料，通过亲核取代反应合成了双酚 A 基邻苯二甲腈树脂，然后用磺胺脒作为新型固化剂对得到的树脂进行固化。采用标准热分析技术（包括 DSC、TGA 和 DMA）对固化特性、动力学、热稳定性和动态机械性能进行了研究。结果表明，磺胺脒固化邻苯二腈树脂的放热峰温度（Tp）和表观活化能（Ea）分别为 263.20°C 和 76.6 kJ-mol-1，远低于传统的芳香族二胺固化树脂。此外，磺胺胍固化的树脂还具有优异的热机械性能和热稳定性。玻璃化温度（Tg）为 284.8°C，初始热分解温度（Td,5%）为 439.6°C，在氮气环境下，800°C 时的炭化率为 62.1%。综上所述，有机胍固化酞腈树脂具有优异的固化特性（低 Tp 和 Ea）和高热稳定性，为制备综合性能高的酞腈树脂提供了一种可行的方法。
{"title":"Study on the curing characteristics and properties of phthalonitrile resin cured with organic guanidine","authors":"Nanyang Ding, Chengzhong Wang","doi":"10.1177/09540083241259449","DOIUrl":"https://doi.org/10.1177/09540083241259449","url":null,"abstract":"Bisphenol A-based phthalonitrile resin was synthesized by nucleophilic substitution reaction from bisphenol A and 4-nitrophthalonitrile, and then the obtained resin was cured with sulfaguanidine as a novel curing agent. The curing characteristics, kinetics, thermal stability and dynamic mechanical property were studied by standard thermal analysis techniques including DSC, TGA, and DMA. The peak temperature of exothermic peak ( Tp) and apparent activation energy ( Ea) of sulfaguanidine cured phthalonitrile resin were 263.20°C and 76.6 kJ·mol−1 respectively, much lower than those of traditional aromatic diamine cured resin. Moreover, the resin cured by sulfaguanidine showed excellent thermomechanical properties and thermal stability. The glass transition temperature ( Tg) was 284.8°C, the initial thermal decomposition temperature ( Td,5%) was 439.6°C, and the char yield at 800°C was 62.1% in nitrogen atmosphere. To sum up, organic guanidine cured phthalonitrile resin exhibits excellent curing characteristics (low Tp and Ea) and high thermal properties, which provides a promising approach to preparing phthalonitrile resin with high comprehensive performance.","PeriodicalId":504490,"journal":{"name":"High Performance Polymers","volume":" 42","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141373734","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Good mechanical properties, heat resistance and processability are the basic requirements of matrix resins for high performance heat resistant composites. The existing two types of silicon-containing arylacetylene resins, poly (silylene arylacetylene) (PSA) and poly (silane arylether arylacetylene) (PSEA), cannot balance these three requirements well. To achieve this goal, an attempt was made to synthesize a copolymerized resin containing both diethynylbenzene and diynyl arylether structures in the main chain, silicon-containing poly (diethynylbenzene-co-phenoxyphenoxybenzenediacetylene). By controlling the amount of 1,3-diethynylbenzene ( m-DEB) and 1,3-bis(4′-ethynylphenoxy)benzene ( pmp-BEPB), several random copolymerized resins with various ratios of m-DEB to pmp-BEPB were synthesized by the Grignard reactions. The results show that the introduction of m-DEB could effectively reduce the viscosity of the resin, and thermal stability of the cured resin is improved, but the mechanical strength of the cured resin is slightly reduced. The copolymerized resin has good overall performance when the amount of m-DEB and pmp-BEPB is equal. The processing window of the resin is 56∼169°C, the flexural strength and modulus of the cured resin are 32.9 MPa and 2.7 GPa, respectively, and the temperatures of 5% weight loss (Td5) of the cured resin is 589°C in nitrogen.
{"title":"Synthesis and properties of silicon-containing poly(diethynylbenzen-co-phenoxyphenoxybenzenediacetylene)s","authors":"Shuyue Liu, Shuaikang Lv, Changjun Gong, Wanli Xv, Junkun Tang, F. Huang","doi":"10.1177/09540083241259504","DOIUrl":"https://doi.org/10.1177/09540083241259504","url":null,"abstract":"Good mechanical properties, heat resistance and processability are the basic requirements of matrix resins for high performance heat resistant composites. The existing two types of silicon-containing arylacetylene resins, poly (silylene arylacetylene) (PSA) and poly (silane arylether arylacetylene) (PSEA), cannot balance these three requirements well. To achieve this goal, an attempt was made to synthesize a copolymerized resin containing both diethynylbenzene and diynyl arylether structures in the main chain, silicon-containing poly (diethynylbenzene-co-phenoxyphenoxybenzenediacetylene). By controlling the amount of 1,3-diethynylbenzene ( m-DEB) and 1,3-bis(4′-ethynylphenoxy)benzene ( pmp-BEPB), several random copolymerized resins with various ratios of m-DEB to pmp-BEPB were synthesized by the Grignard reactions. The results show that the introduction of m-DEB could effectively reduce the viscosity of the resin, and thermal stability of the cured resin is improved, but the mechanical strength of the cured resin is slightly reduced. The copolymerized resin has good overall performance when the amount of m-DEB and pmp-BEPB is equal. The processing window of the resin is 56∼169°C, the flexural strength and modulus of the cured resin are 32.9 MPa and 2.7 GPa, respectively, and the temperatures of 5% weight loss (Td5) of the cured resin is 589°C in nitrogen.","PeriodicalId":504490,"journal":{"name":"High Performance Polymers","volume":" 5","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141371018","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-14DOI: 10.1177/09540083241254540
Wen Zhang, Zhilin Cao, Ling Chao, Zhengzhou Wang
The development of epoxy resin (EP) with simultaneous enhancements in flame retardancy, mechanical performance, and low dielectric properties represents a significant and complex challenge. In this study, halloysite nanotubes (HNTs) were modified with melamine amino tris-methylene phosphonate (MA) to produce MA-modified HNTs (HMA), which were then integrated into EP to form EP/HMA composites. The incorporation of 1 wt% HMA significantly enhanced the flame retardancy (limit oxygen index up to 29.7%, UL-94 V-0 rating), reduced peak heat release rate by 23.4%, decreased total heat release by 11.9%, reduced total smoke production by 18.4%, and improved mechanical properties (tensile strength by 17.0%, impact strength by 61.0%) compared to pure EP. Additionally, EP/HMA showed a low dielectric constant (3.16) and a dielectric loss (0.019) at 1 GHz. This research presents a versatile strategy for creating multifunctional EP composites with high potential for applications in microelectronics, electronic packaging, and other relevant fields.
开发同时具有阻燃性、机械性能和低介电性能的环氧树脂（EP）是一项重大而复杂的挑战。在这项研究中，用三聚氰胺氨基三亚甲基膦酸盐（MA）改性哈洛石纳米管（HNTs），生成 MA 改性 HNTs（HMA），然后将其融入 EP 中，形成 EP/HMA 复合材料。与纯 EP 相比，加入 1 wt% 的 HMA 可显著提高阻燃性（极限氧指数高达 29.7%，UL-94 V-0 级），降低 23.4% 的峰值热释放率，降低 11.9% 的总热释放率，降低 18.4% 的总产烟量，并改善机械性能（拉伸强度提高 17.0%，冲击强度提高 61.0%）。此外，EP/HMA 的介电常数较低（3.16），在 1 GHz 时的介电损耗为 0.019。这项研究为制造多功能 EP 复合材料提供了一种多功能策略，在微电子、电子封装和其他相关领域具有很高的应用潜力。
{"title":"Design synthesis of melamine amino tris-methylene phosphonate modified halloysite nanotubes for epoxy resin with simultaneously improved flame retardancy, dielectric properties and mechanical performance","authors":"Wen Zhang, Zhilin Cao, Ling Chao, Zhengzhou Wang","doi":"10.1177/09540083241254540","DOIUrl":"https://doi.org/10.1177/09540083241254540","url":null,"abstract":"The development of epoxy resin (EP) with simultaneous enhancements in flame retardancy, mechanical performance, and low dielectric properties represents a significant and complex challenge. In this study, halloysite nanotubes (HNTs) were modified with melamine amino tris-methylene phosphonate (MA) to produce MA-modified HNTs (HMA), which were then integrated into EP to form EP/HMA composites. The incorporation of 1 wt% HMA significantly enhanced the flame retardancy (limit oxygen index up to 29.7%, UL-94 V-0 rating), reduced peak heat release rate by 23.4%, decreased total heat release by 11.9%, reduced total smoke production by 18.4%, and improved mechanical properties (tensile strength by 17.0%, impact strength by 61.0%) compared to pure EP. Additionally, EP/HMA showed a low dielectric constant (3.16) and a dielectric loss (0.019) at 1 GHz. This research presents a versatile strategy for creating multifunctional EP composites with high potential for applications in microelectronics, electronic packaging, and other relevant fields.","PeriodicalId":504490,"journal":{"name":"High Performance Polymers","volume":"36 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140979787","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-09DOI: 10.1177/09540083241227589
Bin Ren, Chenchen Wang, Rui Ma, Ying Huang, Xiuyun Li
A reactive flame retardant containing biphenyl structure (DEU-2DOPO) was prepared from the bio-based raw material eugenol. The incorporation of DEU-2DOPO into the epoxy resin serves to enhance the ring-opening reaction of the epoxy. Furthermore, the inclusion of DEU-2DOPO has been found to have a positive impact on the glass transition temperature and residual carbon rate of the epoxy resin. This additive also significantly improves the mechanical properties of the epoxy resin, leading to a 49.3% increase in tensile strength, an 81.9% increase in breaking elongation, and a 15.8% increase in flexural strength. Notably, when DEU-2DOPO is introduced at a concentration of 5 wt%, it not only achieves a V-0 rating in the UL-94 test but also exhibits an impressive ultimate oxygen index of 34.5%. Additionally, the cone calorimetric testing revealed that the presence of DEU-2DOPO results in lower combustion metrics compared to pure epoxy, as evidenced by a reduction of 15.1% in total heat release (THR) and 10.8% in total smoke release (TSR). An analysis of the flame retardant mechanism elucidates that DEU-2DOPO promotes the formation of a stable and dense residual carbon, thereby impeding gas and heat exchange. Furthermore, the decomposition of DEU-2DOPO generates PO· and PO2· radicals, which effectively neutralize reactive radicals.
{"title":"Bio-based flame retardants containing biphenyl structure for simultaneously enhancing mechanical properties and fire safety of epoxy resins","authors":"Bin Ren, Chenchen Wang, Rui Ma, Ying Huang, Xiuyun Li","doi":"10.1177/09540083241227589","DOIUrl":"https://doi.org/10.1177/09540083241227589","url":null,"abstract":"A reactive flame retardant containing biphenyl structure (DEU-2DOPO) was prepared from the bio-based raw material eugenol. The incorporation of DEU-2DOPO into the epoxy resin serves to enhance the ring-opening reaction of the epoxy. Furthermore, the inclusion of DEU-2DOPO has been found to have a positive impact on the glass transition temperature and residual carbon rate of the epoxy resin. This additive also significantly improves the mechanical properties of the epoxy resin, leading to a 49.3% increase in tensile strength, an 81.9% increase in breaking elongation, and a 15.8% increase in flexural strength. Notably, when DEU-2DOPO is introduced at a concentration of 5 wt%, it not only achieves a V-0 rating in the UL-94 test but also exhibits an impressive ultimate oxygen index of 34.5%. Additionally, the cone calorimetric testing revealed that the presence of DEU-2DOPO results in lower combustion metrics compared to pure epoxy, as evidenced by a reduction of 15.1% in total heat release (THR) and 10.8% in total smoke release (TSR). An analysis of the flame retardant mechanism elucidates that DEU-2DOPO promotes the formation of a stable and dense residual carbon, thereby impeding gas and heat exchange. Furthermore, the decomposition of DEU-2DOPO generates PO· and PO2· radicals, which effectively neutralize reactive radicals.","PeriodicalId":504490,"journal":{"name":"High Performance Polymers","volume":" 21","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139789411","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-09DOI: 10.1177/09540083241227589
Bin Ren, Chenchen Wang, Rui Ma, Ying Huang, Xiuyun Li
A reactive flame retardant containing biphenyl structure (DEU-2DOPO) was prepared from the bio-based raw material eugenol. The incorporation of DEU-2DOPO into the epoxy resin serves to enhance the ring-opening reaction of the epoxy. Furthermore, the inclusion of DEU-2DOPO has been found to have a positive impact on the glass transition temperature and residual carbon rate of the epoxy resin. This additive also significantly improves the mechanical properties of the epoxy resin, leading to a 49.3% increase in tensile strength, an 81.9% increase in breaking elongation, and a 15.8% increase in flexural strength. Notably, when DEU-2DOPO is introduced at a concentration of 5 wt%, it not only achieves a V-0 rating in the UL-94 test but also exhibits an impressive ultimate oxygen index of 34.5%. Additionally, the cone calorimetric testing revealed that the presence of DEU-2DOPO results in lower combustion metrics compared to pure epoxy, as evidenced by a reduction of 15.1% in total heat release (THR) and 10.8% in total smoke release (TSR). An analysis of the flame retardant mechanism elucidates that DEU-2DOPO promotes the formation of a stable and dense residual carbon, thereby impeding gas and heat exchange. Furthermore, the decomposition of DEU-2DOPO generates PO· and PO2· radicals, which effectively neutralize reactive radicals.
{"title":"Bio-based flame retardants containing biphenyl structure for simultaneously enhancing mechanical properties and fire safety of epoxy resins","authors":"Bin Ren, Chenchen Wang, Rui Ma, Ying Huang, Xiuyun Li","doi":"10.1177/09540083241227589","DOIUrl":"https://doi.org/10.1177/09540083241227589","url":null,"abstract":"A reactive flame retardant containing biphenyl structure (DEU-2DOPO) was prepared from the bio-based raw material eugenol. The incorporation of DEU-2DOPO into the epoxy resin serves to enhance the ring-opening reaction of the epoxy. Furthermore, the inclusion of DEU-2DOPO has been found to have a positive impact on the glass transition temperature and residual carbon rate of the epoxy resin. This additive also significantly improves the mechanical properties of the epoxy resin, leading to a 49.3% increase in tensile strength, an 81.9% increase in breaking elongation, and a 15.8% increase in flexural strength. Notably, when DEU-2DOPO is introduced at a concentration of 5 wt%, it not only achieves a V-0 rating in the UL-94 test but also exhibits an impressive ultimate oxygen index of 34.5%. Additionally, the cone calorimetric testing revealed that the presence of DEU-2DOPO results in lower combustion metrics compared to pure epoxy, as evidenced by a reduction of 15.1% in total heat release (THR) and 10.8% in total smoke release (TSR). An analysis of the flame retardant mechanism elucidates that DEU-2DOPO promotes the formation of a stable and dense residual carbon, thereby impeding gas and heat exchange. Furthermore, the decomposition of DEU-2DOPO generates PO· and PO2· radicals, which effectively neutralize reactive radicals.","PeriodicalId":504490,"journal":{"name":"High Performance Polymers","volume":"81 10-11","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139849489","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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