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含1,4-萘基氯化聚芳醚酮酮无规共聚物的合成与性能 被引量:1
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作者 徐海云 程乐华 《材料科学与工程学报》 CAS CSCD 北大核心 2004年第1期86-90,共5页
以无水AlCl3为催化剂、ClCH2 CH2 Cl和NMP(N ,N 二甲基吡咯烷酮 )为复合溶剂 ,由二苯醚 (DPE) ,2 ,5 二氯对苯二甲酰氯 (DCTPC)和 4 ,4′ 二 (α 萘氧基 )二苯酮 (DNBP)通过亲电缩聚反应合成了一系列新型主链含1,4 亚萘基结构的氯化... 以无水AlCl3为催化剂、ClCH2 CH2 Cl和NMP(N ,N 二甲基吡咯烷酮 )为复合溶剂 ,由二苯醚 (DPE) ,2 ,5 二氯对苯二甲酰氯 (DCTPC)和 4 ,4′ 二 (α 萘氧基 )二苯酮 (DNBP)通过亲电缩聚反应合成了一系列新型主链含1,4 亚萘基结构的氯化聚芳醚酮酮无规共聚物。优化后的工艺条件为 :n(AlCl3)∶n(DCTPC)∶n(DNBP +DPE) =0 0 6∶0 0 1∶0 0 1,预聚合温度小于 - 10℃下反应 2h ,再逐渐升温至 2 5℃左右反应约 8h。研究了DNBP结构单元及含氯侧基对共聚物性能的影响 ,并用IR、DSC、TG、WAXD等方法对其进行了表征。结果表明 ,所得聚合物在 193~2 12℃的温度范围内均只出现一个玻璃化温度 (Tg)转变峰 ,且随着共聚物中DNBP结构单元含量的增加 ,其Tg 逐渐升高 ,而熔融温度 (Tm)和结晶度逐渐降低。同时由于芳环上氯取代基的影响 ,降低了共聚物的热分解温度(Td) ,但仍具有良好的耐热性并且明显提高了阻燃性能和溶解性能。当x(DNBP) <30 %时 ,共聚物仍为半结晶性 ,并选择n(DNBP)∶n(DPE)在 10∶90~ 30∶70范围内为理想的聚合物加工成型条件。共聚物的断裂伸长率随着DNBP结构单元的引入逐渐增加 ,而拉伸强度和拉伸模量却有所下降。该类共聚物的拉伸强度可达 78MPa以上 ,拉伸模量在 2 8GPa以上 。 展开更多
关键词 1 4-萘基氯化醚酮酮无规共聚物 合成工艺 耐热性 力学性能 耐高温材料
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二芳氧基稀土氯化物(ArO)_2YCl(THF)_2·MePh的合成、表征及晶体结构(ArO=2,6-二叔丁基-4-甲基酚基) 被引量:1
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作者 喻龙宝 姚英明 沈琪 《中国稀土学报》 CAS CSCD 北大核心 2002年第5期398-401,共4页
无水YCl3 与二倍量的ArONa(ArO =2 ,6 二叔丁基 4 甲基酚基 )在四氢呋喃 (THF)中反应 ,经甲苯溶液重结晶 ,高产率地合成了二芳氧基稀土氯化物 (ArO) 2 YCl(THF) 2 ·MePh。产物经元素分析和核磁共振表征 ,并测定了其晶体结构。配... 无水YCl3 与二倍量的ArONa(ArO =2 ,6 二叔丁基 4 甲基酚基 )在四氢呋喃 (THF)中反应 ,经甲苯溶液重结晶 ,高产率地合成了二芳氧基稀土氯化物 (ArO) 2 YCl(THF) 2 ·MePh。产物经元素分析和核磁共振表征 ,并测定了其晶体结构。配合物属正方晶系 ,I4( 1) /acd空间群 ,晶胞参数为a =1.8913( 1)nm ,b =1.8913( 1)nm ,c =5 .2 2 39( 1)nm ,V =18.6 86 ( 1)nm3 ,Z =16 ,Dc=1.137mg·m- 3 ,μ =1.342mm- 1 (MoKα) ,F( 0 0 0 ) =6 848,R =0 .0 46 9,Rw=0 .112 2。中心金属钇原子与二个芳氧基中的氧原子、一个氯原子和两个THF分子中的氧原子配位 ,形成一个五配位的扭曲的三角双锥几何构型。Y O(Ar)和Y Cl的键长分别为 0 .2 10 1( 3)和 0 .2 5 17( 6 )nm。 展开更多
关键词 氧基稀土氯化物(ArO)2YCl(THF)2·MePh 合成 表征 晶体结构 稀土配合物
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含2,6-萘基的氯化聚芳醚酮酮的合成与性能
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作者 徐海云 田冬 +1 位作者 徐俊 崔明 《安庆师范学院学报(自然科学版)》 2003年第1期41-44,50,共5页
通过4,4′-二(β-萘氧基)二苯酮(DNOPK)、二苯醚(DPE)与对苯二甲酰氯(TPC)、2,5-二氯对苯二甲酰氯(DCTPC)的低温溶液亲电共缩聚反应合成出一系列不同组分的高分子量含2,6-萘基结构的氯化聚芳醚酮酮无规共聚物。研究了含氯侧基对共聚物... 通过4,4′-二(β-萘氧基)二苯酮(DNOPK)、二苯醚(DPE)与对苯二甲酰氯(TPC)、2,5-二氯对苯二甲酰氯(DCTPC)的低温溶液亲电共缩聚反应合成出一系列不同组分的高分子量含2,6-萘基结构的氯化聚芳醚酮酮无规共聚物。研究了含氯侧基对共聚物性能的影响,并对其进行了IR、DSC、TG、WAXD等分析表征。结果表明:所得共聚物具有优良的耐热性和力学性能,随着DCTPC单体含量的增加,其玻璃化温度(Tg)变化不大,而熔融温度(Tm)和结晶度逐渐降低,当其含量超过40mol%时,Tm消失,聚合物呈现非晶态结构,聚合物的热分解温度(失重5%)Td及力学性能均呈下降趋势,但溶解性能得到明显改善。 展开更多
关键词 氯化醚酮酮 4 4’-二(β-萘氧基)二苯酮 2 5-二氯侧基 2 6-萘基 合成 亲电共缩聚反应
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浅谈比色法测定氯化苦残留量的几个问题 被引量:4
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作者 尚瑛达 曹素芳 《粮油仓储科技通讯》 1999年第6期48-50,共3页
氯化苦是我国最早使用的储粮熏蒸剂,世界上50年代最为盛行。但是,由于氯化苦的强烈刺激性气味和高毒、高残留及强腐蚀性等缺陷,给保粮工作带来了诸多不便和危害,所以后来渐渐被磷化氢熏蒸剂所取代。但是,由于长期、频繁使用磷化氢熏蒸,... 氯化苦是我国最早使用的储粮熏蒸剂,世界上50年代最为盛行。但是,由于氯化苦的强烈刺激性气味和高毒、高残留及强腐蚀性等缺陷,给保粮工作带来了诸多不便和危害,所以后来渐渐被磷化氢熏蒸剂所取代。但是,由于长期、频繁使用磷化氢熏蒸,使储粮害虫普遍产生了对磷化氢的抗性和耐药性,影响了熏蒸剂效果。所以目前不少地区又开始使用氯化苦,与磷化氢进行交叉或混合熏蒸。 展开更多
关键词 氯化芳 储粮熏蒸剂 残留量 比色法 测定
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Iron(Ⅲ) phthalocyanine chloride-catalyzed oxidation–aromatization of α,β-unsaturated ketones with hydrazine hydrate: Synthesis of 3,5-disubstituted 1H-pyrazoles 被引量:4
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作者 赵军龙 邱骏 +2 位作者 苟小锋 花成文 陈邦 《Chinese Journal of Catalysis》 SCIE EI CAS CSCD 北大核心 2016年第4期571-578,共8页
We have developed an iron(III) phthalocyanine chloride‐catalyzed oxidation–aromatization ofα,β‐unsaturated ketones with hydrazine hydrate. Various 3,5‐disubstituted 1H‐pyrazoles were obtained in good to excel... We have developed an iron(III) phthalocyanine chloride‐catalyzed oxidation–aromatization ofα,β‐unsaturated ketones with hydrazine hydrate. Various 3,5‐disubstituted 1H‐pyrazoles were obtained in good to excellent yields. This method offers several advantages, including room‐tem‐perature conditions, short reaction time, high yields, simple work‐up procedure, and use of air as an oxidant. The catalyst can be recovered and reused five times without loss of activity. 展开更多
关键词 Iron(III) phthalocyanine chloride AROMATIZATION Pyrazole Michael addition Recyclable catalyst Green chemistry
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Blanc Reaction of Aromatic Compounds Catalyzed by Ionic Liquids 被引量:3
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作者 方岩雄 邓运泉 +4 位作者 任清刚 黄敬平 张赛丹 黄宝华 张焜 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2008年第3期357-360,共4页
Ionic liquids have been used as catalysts for Blanc reaction of toluene. The effects of reaction temperature, reaction time and dosage of the ionic liquid catalyst have been investigated, and the catalytic performance... Ionic liquids have been used as catalysts for Blanc reaction of toluene. The effects of reaction temperature, reaction time and dosage of the ionic liquid catalyst have been investigated, and the catalytic performance of different ionic liquid catalysts for toluene chloromethylation was also studied. The reaction was found to proceed under mild conditions with excellent conversion (up to 90%) in the absence of Lewis acids. The ionic liquids could be recycled and reused without loss of their catalytic activities. 展开更多
关键词 CHLOROMETHYLATION Blanc reaction ionic liquid aromatic compound TOLUENE phase transfer
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Removal of Trace Olefins from Aromatics by Catalytic Alkylation Using 1-Alkyl-3-methylimidazolium Bromochloroaluminate Catalyst
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作者 Sun Yu Shi Li(State Key Laboratory of Chemical Engineering,East China University of Science and Technology,Shanghai 200237) 《China Petroleum Processing & Petrochemical Technology》 SCIE CAS 2011年第2期14-18,共5页
Removal of trace olefins from aromatic liquids had been investigated in the presence of various ionic liquids like 1-ethyl-3-methylimidazoliurn bromochloroaluminate (EMIMBr-AlCl3), 1-butyl-3-methylimidazolium bromoc... Removal of trace olefins from aromatic liquids had been investigated in the presence of various ionic liquids like 1-ethyl-3-methylimidazoliurn bromochloroaluminate (EMIMBr-AlCl3), 1-butyl-3-methylimidazolium bromochloroaluminate (BMIMBr-AlCl3), l-hexyl-3-methylimidazolium bromochloroaluminate (HMIMBr-AlCl3), and 1-octyl-3-methylimidazolium bromochloroaluminate (OMIMBr-A1C13). It was found that the longer the alkyl chain of ionic liquid cations was, the higher the olefins conversion would be. OMIMBr-AlCl3 (with 0.67 molar fraction of AlCl3) had an obvious performance on olefins removal. The influences of various reaction parameters such as the dosage of catalyst, the reaction temperature, and the reaction time on the reaction catalyzed by OMIMBr-AlCl3 were investigated. Under optimum reaction conditions, a higher than 99% conversion of olefins was achieved. The preliminary results revealed that the process could save time, consume less energy, separate products easier, and cause less pollution to the environment. 展开更多
关键词 ionic liquids olefins removal 1-alkyl-3-methylimidazolium bromochloroaluminate AROMATIC
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Metal Chlorides Supported Solid Catalysts for F-C Acylations of Arenes
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作者 李阳 刘云龙 +1 位作者 穆曼曼 陈立功 《Transactions of Tianjin University》 EI CAS 2015年第5期400-405,共6页
A series of metal chlorides supported solid catalysts were prepared by simple wet impregnation method. Their catalytic performances for Friedel-Crafts acylation of toluene with benzoyl chloride were evaluated and the ... A series of metal chlorides supported solid catalysts were prepared by simple wet impregnation method. Their catalytic performances for Friedel-Crafts acylation of toluene with benzoyl chloride were evaluated and the excellent results were obtained over FeC13/SiO2. These catalysts were characterized by BET, NH3-TPD and FT-IR of pyridine adsorption to clarify the structure-activity relationship. It was found that FeC13/SiO2 has larger pore size and pore volume than other catalysts, which increased the accessibility of the catalyst. In addition, FeC13/SiO2 ex- hibited higher molar ratio of Lewis acid sites and Brtpnsted acid sites, which might be another reason for the in- crease of toluene conversion. Furthermore, the reaction parameters, including temperature, time and molar ratio, were optimized. Under the optimized conditions, 91.2% conversion and 82.0% selectivity were obtained. Mean- while, the generality of the catalyst was demonstrated by the acylations of alkyl substituted aromatics. Finally, the catalyst was reused for four runs with slight loss in catalytic activity, which attributed to the drain of the active component. 展开更多
关键词 ACYLATION heterogeneous catalyst silica gel ferric chloride
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Removal of Trace Olefins from Aromatics Catalyzed by[bmim]Br-AlCl_3 Ionic Liquid
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作者 Jiang Zhenghong Hou Minghui +1 位作者 Weng Huixin Shi Li (State Key Lab of Chemical Engineering,East China University of Science & Technology,Shanghai 200237) 《China Petroleum Processing & Petrochemical Technology》 SCIE CAS 2010年第2期41-44,共4页
1-Butyl-3-methylimidazolium bromochloroaluminate ([bmim]Br-AlCl3) ionic liquid was used as an acid catalyst for removal of trace olefins from the aromatic hydrocarbons. The influence of various reaction parameters s... 1-Butyl-3-methylimidazolium bromochloroaluminate ([bmim]Br-AlCl3) ionic liquid was used as an acid catalyst for removal of trace olefins from the aromatic hydrocarbons. The influence of various reaction parameters such as reaction time, temperature, dosage and acid strength of catalyst was investigated. The experimental results demonstrated that the ionic liquid exhibited excellent activity under mild reaction conditions, with the conversion of olefins reaching 98.84% and the bromine index of the aromatics varying from 1129 to 13. On the basis of the results obtained, thereof, a possible reaction mechanism was proposed. 展开更多
关键词 ionic liquid bromine index olefins removal AROMATICS catalyst
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Redox-triggered hydroarylation of o-(hydroxyalkyl)arylalkynes with arylsulfonyl chlorides using visible light catalysis
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作者 Renjie Song Jiadong Xia +1 位作者 Jiangxi Yu Jinheng Li 《Science China Chemistry》 SCIE EI CAS CSCD 2016年第2期184-189,共6页
A new radical-mediated method for the synthesis of 1-(2-(1,2-diarylvinyl)phenyl)ethan-1-ones by the redox hydroarylation of o-(hydroxyalkyl)arylalkynes with arylsulfonyl chlorides is described. This visible light cata... A new radical-mediated method for the synthesis of 1-(2-(1,2-diarylvinyl)phenyl)ethan-1-ones by the redox hydroarylation of o-(hydroxyalkyl)arylalkynes with arylsulfonyl chlorides is described. This visible light catalysis method proceeds via a sequence of the radical addition of aryl group across the C?C triple bond, protonation and redox reaction, and represents a new redox transformation reaction directed by a neighboring hydroxyl group. 展开更多
关键词 HYDROARYLATION redox visible light catalysis ALKYNES arylsulfonyl chlorides
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