{"title":"枝晶钛催化剂的合成及乙烯聚合反应。","authors":"Tianyu Lan, Liduo Chen, Na Zhang, Jun Wang","doi":"10.1080/15685551.2020.1868666","DOIUrl":null,"url":null,"abstract":"<p><p>The 1.0 G dendrimer (C<sub>22</sub>H<sub>48</sub>N<sub>10</sub>O<sub>4</sub>),3,5-di-tert-butylsalicylaldehyde and TiCl<sub>4</sub> · 2THF were used as the synthetic materials, and the dendritic salicylaldehyde imide ligand with substituent hindrance and its titanium catalyst were synthesized by the condensation reaction of schiff base. The structure of the synthesized products was characterized by infrared spectroscopy, nuclear magnetic resonance hydrogen spectroscopy, ultraviolet spectroscopy, electrospray mass spectrometry, and inductively coupled plasma mass spectrometry, The actual structure is consistent with the theoretical design structure. Activated methylaluminoxane (MAO) was used as a catalyst precursor for ethylene polymerization in the process of ethylene catalytic. The effects of ethylene polymerization were studied in terms of the Al/Ti molar ratio, reaction time, reaction temperature, polymerization pressure, and ligand structure of the catalyst. The results show at the reaction temperature of 25°C, the reaction time was 30 min, and the ethylene pressure was 1.0 MPa and Al/Ti was 1,000, the catalytic activity can reach 78.56 kg PE/(mol Ti.h). Furthermore, high-temperature GPC-IR, DSC, and torque rheometer were used to characterized the microstructure, thermal properties, and viscoelastic state of polyethylene samples obtained. The results showed that the product was ultra-high-molecular-weight polyethylene.</p>","PeriodicalId":11170,"journal":{"name":"Designed Monomers and Polymers","volume":"24 1","pages":"13-21"},"PeriodicalIF":1.8000,"publicationDate":"2021-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1080/15685551.2020.1868666","citationCount":"0","resultStr":"{\"title\":\"Synthesis and ethylene polymerization reaction of dendritic titanium catalysts.\",\"authors\":\"Tianyu Lan, Liduo Chen, Na Zhang, Jun Wang\",\"doi\":\"10.1080/15685551.2020.1868666\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>The 1.0 G dendrimer (C<sub>22</sub>H<sub>48</sub>N<sub>10</sub>O<sub>4</sub>),3,5-di-tert-butylsalicylaldehyde and TiCl<sub>4</sub> · 2THF were used as the synthetic materials, and the dendritic salicylaldehyde imide ligand with substituent hindrance and its titanium catalyst were synthesized by the condensation reaction of schiff base. The structure of the synthesized products was characterized by infrared spectroscopy, nuclear magnetic resonance hydrogen spectroscopy, ultraviolet spectroscopy, electrospray mass spectrometry, and inductively coupled plasma mass spectrometry, The actual structure is consistent with the theoretical design structure. Activated methylaluminoxane (MAO) was used as a catalyst precursor for ethylene polymerization in the process of ethylene catalytic. The effects of ethylene polymerization were studied in terms of the Al/Ti molar ratio, reaction time, reaction temperature, polymerization pressure, and ligand structure of the catalyst. The results show at the reaction temperature of 25°C, the reaction time was 30 min, and the ethylene pressure was 1.0 MPa and Al/Ti was 1,000, the catalytic activity can reach 78.56 kg PE/(mol Ti.h). Furthermore, high-temperature GPC-IR, DSC, and torque rheometer were used to characterized the microstructure, thermal properties, and viscoelastic state of polyethylene samples obtained. The results showed that the product was ultra-high-molecular-weight polyethylene.</p>\",\"PeriodicalId\":11170,\"journal\":{\"name\":\"Designed Monomers and Polymers\",\"volume\":\"24 1\",\"pages\":\"13-21\"},\"PeriodicalIF\":1.8000,\"publicationDate\":\"2021-01-18\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.1080/15685551.2020.1868666\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Designed Monomers and Polymers\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://doi.org/10.1080/15685551.2020.1868666\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"POLYMER SCIENCE\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Designed Monomers and Polymers","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1080/15685551.2020.1868666","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"POLYMER SCIENCE","Score":null,"Total":0}
引用次数: 0
摘要
以1.0 G树状大分子(C22H48N10O4)、3,5-二叔丁基水杨醛和TiCl4·2THF为合成材料,通过席夫碱缩合反应合成具有取代基位阻的树突状水杨醛亚胺配体及其钛催化剂。通过红外光谱、核磁共振氢谱、紫外光谱、电喷雾质谱、电感耦合等离子体质谱等手段对合成产物的结构进行了表征,实际结构与理论设计结构一致。考察了Al/Ti摩尔比、反应时间、反应温度、聚合压力、催化剂配体结构等因素对乙烯聚合的影响。结果表明,在反应温度为25℃,反应时间为30 min,乙烯压力为1.0 MPa, Al/Ti为1000的条件下,催化活性可达78.56 kg PE/(mol Ti.h)。利用高温GPC-IR、DSC和扭矩流变仪对所得聚乙烯样品的微观结构、热性能和粘弹性状态进行表征。结果表明,该产物为超高分子量聚乙烯。
Synthesis and ethylene polymerization reaction of dendritic titanium catalysts.
The 1.0 G dendrimer (C22H48N10O4),3,5-di-tert-butylsalicylaldehyde and TiCl4 · 2THF were used as the synthetic materials, and the dendritic salicylaldehyde imide ligand with substituent hindrance and its titanium catalyst were synthesized by the condensation reaction of schiff base. The structure of the synthesized products was characterized by infrared spectroscopy, nuclear magnetic resonance hydrogen spectroscopy, ultraviolet spectroscopy, electrospray mass spectrometry, and inductively coupled plasma mass spectrometry, The actual structure is consistent with the theoretical design structure. Activated methylaluminoxane (MAO) was used as a catalyst precursor for ethylene polymerization in the process of ethylene catalytic. The effects of ethylene polymerization were studied in terms of the Al/Ti molar ratio, reaction time, reaction temperature, polymerization pressure, and ligand structure of the catalyst. The results show at the reaction temperature of 25°C, the reaction time was 30 min, and the ethylene pressure was 1.0 MPa and Al/Ti was 1,000, the catalytic activity can reach 78.56 kg PE/(mol Ti.h). Furthermore, high-temperature GPC-IR, DSC, and torque rheometer were used to characterized the microstructure, thermal properties, and viscoelastic state of polyethylene samples obtained. The results showed that the product was ultra-high-molecular-weight polyethylene.
期刊介绍:
Designed Monomers and Polymers ( DMP) publishes prompt peer-reviewed papers and short topical reviews on all areas of macromolecular design and applications. Emphasis is placed on the preparations of new monomers, including characterization and applications. Experiments should be presented in sufficient detail (including specific observations, precautionary notes, use of new materials, techniques, and their possible problems) that they could be reproduced by any researcher wishing to repeat the work.
The journal also includes macromolecular design of polymeric materials (such as polymeric biomaterials, biomedical polymers, etc.) with medical applications.
DMP provides an interface between organic and polymer chemistries and aims to bridge the gap between monomer synthesis and the design of new polymers. Submssions are invited in the areas including, but not limited to:
-macromolecular science, initiators, macroinitiators for macromolecular design
-kinetics, mechanism and modelling aspects of polymerization
-new methods of synthesis of known monomers
-new monomers (must show evidence for polymerization, e.g. polycondensation, sequential combination, oxidative coupling, radiation, plasma polymerization)
-functional prepolymers of various architectures such as hyperbranched polymers, telechelic polymers, macromonomers, or dendrimers
-new polymeric materials with biomedical applications