H. Hu, W. Wang, Liqin Jiang, Liang Liu, Y. Zhang, Y. Yang, Jinming Wang
{"title":"基于变温FTIR光谱和热重质谱的树脂固化机理研究","authors":"H. Hu, W. Wang, Liqin Jiang, Liang Liu, Y. Zhang, Y. Yang, Jinming Wang","doi":"10.1177/09673911221102114","DOIUrl":null,"url":null,"abstract":"To solve the problem that the curing mechanism evolution of phenolic resin catalyzed by Ba(OH)2 remained unclear, the p-p methylene index, o-p methylene index, o-o methylene index, hydroxymethyl index, and ether index were introduced to quantitatively investigate the chemical structure of resin in the curing temperature range of 90–230°C. The chemical structures were investigated by variable temperature FT-IR. The gas products released with the increase of curing temperature were characterized by Thermogravimetry-Mass Spectrometry. The curing mechanism from 90°C to 230°C was concluded finally. The results show that the main reaction is the formation of the p-p methylene group in the range of 90–120°C. It is difficult to form the o-p methylene bridge at this stage. In the range of 120–160°C, the main reaction is the formation of the p-p methylene group. From 160°C to 190°C, the main reactions are the breaking of the ether bond, the formation of the carbonyl group and the propyl bridge. Above 190°C, the main reactions are polycondensation reaction among phenolic hydroxyl groups, and the formation reaction of carbonyl groups. The ether bond breaks completely above 230°C. This work provides a new method to investigate the curing mechanism. It is a benefit for the rational design of the curing process of phenolic resin-based composites.","PeriodicalId":20417,"journal":{"name":"Polymers and Polymer Composites","volume":null,"pages":null},"PeriodicalIF":0.0000,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"4","resultStr":"{\"title\":\"Curing mechanism of resole phenolic resin based on variable temperature FTIR spectra and thermogravimetry-mass spectrometry\",\"authors\":\"H. Hu, W. Wang, Liqin Jiang, Liang Liu, Y. Zhang, Y. Yang, Jinming Wang\",\"doi\":\"10.1177/09673911221102114\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"To solve the problem that the curing mechanism evolution of phenolic resin catalyzed by Ba(OH)2 remained unclear, the p-p methylene index, o-p methylene index, o-o methylene index, hydroxymethyl index, and ether index were introduced to quantitatively investigate the chemical structure of resin in the curing temperature range of 90–230°C. The chemical structures were investigated by variable temperature FT-IR. The gas products released with the increase of curing temperature were characterized by Thermogravimetry-Mass Spectrometry. The curing mechanism from 90°C to 230°C was concluded finally. The results show that the main reaction is the formation of the p-p methylene group in the range of 90–120°C. It is difficult to form the o-p methylene bridge at this stage. In the range of 120–160°C, the main reaction is the formation of the p-p methylene group. From 160°C to 190°C, the main reactions are the breaking of the ether bond, the formation of the carbonyl group and the propyl bridge. Above 190°C, the main reactions are polycondensation reaction among phenolic hydroxyl groups, and the formation reaction of carbonyl groups. The ether bond breaks completely above 230°C. This work provides a new method to investigate the curing mechanism. It is a benefit for the rational design of the curing process of phenolic resin-based composites.\",\"PeriodicalId\":20417,\"journal\":{\"name\":\"Polymers and Polymer Composites\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2022-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"4\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Polymers and Polymer Composites\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.1177/09673911221102114\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Polymers and Polymer Composites","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1177/09673911221102114","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
Curing mechanism of resole phenolic resin based on variable temperature FTIR spectra and thermogravimetry-mass spectrometry
To solve the problem that the curing mechanism evolution of phenolic resin catalyzed by Ba(OH)2 remained unclear, the p-p methylene index, o-p methylene index, o-o methylene index, hydroxymethyl index, and ether index were introduced to quantitatively investigate the chemical structure of resin in the curing temperature range of 90–230°C. The chemical structures were investigated by variable temperature FT-IR. The gas products released with the increase of curing temperature were characterized by Thermogravimetry-Mass Spectrometry. The curing mechanism from 90°C to 230°C was concluded finally. The results show that the main reaction is the formation of the p-p methylene group in the range of 90–120°C. It is difficult to form the o-p methylene bridge at this stage. In the range of 120–160°C, the main reaction is the formation of the p-p methylene group. From 160°C to 190°C, the main reactions are the breaking of the ether bond, the formation of the carbonyl group and the propyl bridge. Above 190°C, the main reactions are polycondensation reaction among phenolic hydroxyl groups, and the formation reaction of carbonyl groups. The ether bond breaks completely above 230°C. This work provides a new method to investigate the curing mechanism. It is a benefit for the rational design of the curing process of phenolic resin-based composites.