{"title":"用于提高环氧树脂阻燃性和机械性能的丁缩醛-DOPO 衍生物","authors":"Zhengpeng Chen, Xin He, Zhengshuai Cao, Yunfan Li, Denglong Chen, Zhiwang Yang, Ziqiang Lei","doi":"10.1002/fam.3228","DOIUrl":null,"url":null,"abstract":"<p>With the wide application of epoxy resins in adhesives, electronic packaging materials, and aerospace fields, it is necessary to prepare high-performance flame-retardant epoxy resins to reduce the fire risk caused by their flammability. In this study, the rigid structure intermediate Schiff base (DMDA-SH) was synthesized by condensation reaction of syringaldehyde (SH) with O-Tolidine (DMDA). Then, DMDA-SH-DOPO, a novel P/N-structured biobased flame-retardant curing agent, was synthesized by addition reaction with 9,10-dihydro-9-oxaza-10-phosphame-10-oxide (DOPO) and was applied to the preparation of intrinsic flame-retardant epoxy resin. As expected, DMDA-SH-DOPO has good flame-retardant properties due to the synergistic action of N/P elements. Epoxy resin with only 2.5% DMDA-SH-DOPO (P = 0.16%) can pass the UL-94 V-0 test. Compared with DGEBA/DDM, DMDA-SH-DOPO-7.5's (P = 0.49%) peak heat release rate was reduced by 48.4% and the limiting oxygen index (LOI) reached 27%, making it a flame-retardant material. From the point of view of carbonaceous residue performance, the expansion height of carbon residue after DMDA-SH-DOPO-7.5 combustion is significantly increased, and the amount of carbon residue at 800°C is increased by 36.4%. In addition, appropriate DMDA-SH-DOPO can effectively improve the bending property of epoxy resin. This study provides a new idea for preparing renewable high-performance intrinsic flame-retardant epoxy resin.</p>","PeriodicalId":12186,"journal":{"name":"Fire and Materials","volume":"48 7","pages":"752-764"},"PeriodicalIF":2.0000,"publicationDate":"2024-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Syringaldehyde-DOPO derivative for enhancing flame retardancy and mechanical properties of epoxy resin\",\"authors\":\"Zhengpeng Chen, Xin He, Zhengshuai Cao, Yunfan Li, Denglong Chen, Zhiwang Yang, Ziqiang Lei\",\"doi\":\"10.1002/fam.3228\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>With the wide application of epoxy resins in adhesives, electronic packaging materials, and aerospace fields, it is necessary to prepare high-performance flame-retardant epoxy resins to reduce the fire risk caused by their flammability. In this study, the rigid structure intermediate Schiff base (DMDA-SH) was synthesized by condensation reaction of syringaldehyde (SH) with O-Tolidine (DMDA). Then, DMDA-SH-DOPO, a novel P/N-structured biobased flame-retardant curing agent, was synthesized by addition reaction with 9,10-dihydro-9-oxaza-10-phosphame-10-oxide (DOPO) and was applied to the preparation of intrinsic flame-retardant epoxy resin. As expected, DMDA-SH-DOPO has good flame-retardant properties due to the synergistic action of N/P elements. Epoxy resin with only 2.5% DMDA-SH-DOPO (P = 0.16%) can pass the UL-94 V-0 test. Compared with DGEBA/DDM, DMDA-SH-DOPO-7.5's (P = 0.49%) peak heat release rate was reduced by 48.4% and the limiting oxygen index (LOI) reached 27%, making it a flame-retardant material. From the point of view of carbonaceous residue performance, the expansion height of carbon residue after DMDA-SH-DOPO-7.5 combustion is significantly increased, and the amount of carbon residue at 800°C is increased by 36.4%. In addition, appropriate DMDA-SH-DOPO can effectively improve the bending property of epoxy resin. This study provides a new idea for preparing renewable high-performance intrinsic flame-retardant epoxy resin.</p>\",\"PeriodicalId\":12186,\"journal\":{\"name\":\"Fire and Materials\",\"volume\":\"48 7\",\"pages\":\"752-764\"},\"PeriodicalIF\":2.0000,\"publicationDate\":\"2024-07-14\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Fire and Materials\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/fam.3228\",\"RegionNum\":4,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"MATERIALS SCIENCE, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Fire and Materials","FirstCategoryId":"88","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/fam.3228","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"MATERIALS SCIENCE, MULTIDISCIPLINARY","Score":null,"Total":0}
Syringaldehyde-DOPO derivative for enhancing flame retardancy and mechanical properties of epoxy resin
With the wide application of epoxy resins in adhesives, electronic packaging materials, and aerospace fields, it is necessary to prepare high-performance flame-retardant epoxy resins to reduce the fire risk caused by their flammability. In this study, the rigid structure intermediate Schiff base (DMDA-SH) was synthesized by condensation reaction of syringaldehyde (SH) with O-Tolidine (DMDA). Then, DMDA-SH-DOPO, a novel P/N-structured biobased flame-retardant curing agent, was synthesized by addition reaction with 9,10-dihydro-9-oxaza-10-phosphame-10-oxide (DOPO) and was applied to the preparation of intrinsic flame-retardant epoxy resin. As expected, DMDA-SH-DOPO has good flame-retardant properties due to the synergistic action of N/P elements. Epoxy resin with only 2.5% DMDA-SH-DOPO (P = 0.16%) can pass the UL-94 V-0 test. Compared with DGEBA/DDM, DMDA-SH-DOPO-7.5's (P = 0.49%) peak heat release rate was reduced by 48.4% and the limiting oxygen index (LOI) reached 27%, making it a flame-retardant material. From the point of view of carbonaceous residue performance, the expansion height of carbon residue after DMDA-SH-DOPO-7.5 combustion is significantly increased, and the amount of carbon residue at 800°C is increased by 36.4%. In addition, appropriate DMDA-SH-DOPO can effectively improve the bending property of epoxy resin. This study provides a new idea for preparing renewable high-performance intrinsic flame-retardant epoxy resin.
期刊介绍:
Fire and Materials is an international journal for scientific and technological communications directed at the fire properties of materials and the products into which they are made. This covers all aspects of the polymer field and the end uses where polymers find application; the important developments in the fields of natural products - wood and cellulosics; non-polymeric materials - metals and ceramics; as well as the chemistry and industrial applications of fire retardant chemicals.
Contributions will be particularly welcomed on heat release; properties of combustion products - smoke opacity, toxicity and corrosivity; modelling and testing.