化学试剂
化學試劑
화학시제
CHEMICAL REAGENTS
2009年
11期
879-882
,共4页
曾锦萍%黄海平%梅光泉%于澍燕
曾錦萍%黃海平%梅光泉%于澍燕
증금평%황해평%매광천%우주연
4,4'-联苯-3,3'-二(2,4-戊二酮)%合成%表征%热分析
4,4'-聯苯-3,3'-二(2,4-戊二酮)%閤成%錶徵%熱分析
4,4'-련분-3,3'-이(2,4-무이동)%합성%표정%열분석
3,3'-( biphenyl-4,4'-diyl) dipentane-2,4-dione%synthesis%characterization%thermal analysis
以4,4'-二(氯甲基)联苯和2,3-丁二酮-亚磷酸三甲酯(1:1)加合物为原料合成了标题化合物,采用核磁共振谱、质谱、红外光谱和紫外可见光谱对化合物进行结构表征.在静态空气气氛中用热重-差示扫描量热分析法(TG-DSC)对其进行了热分析研究:168~436 ℃之间质量损失76.67%,最后的固体残留物为联苯骨架不完全燃烧的残留物.在272 ℃有一个放热峰,在210、302 ℃分别出现强吸热峰.结果表明该固态化合物在168 ℃以下很稳定.
以4,4'-二(氯甲基)聯苯和2,3-丁二酮-亞燐痠三甲酯(1:1)加閤物為原料閤成瞭標題化閤物,採用覈磁共振譜、質譜、紅外光譜和紫外可見光譜對化閤物進行結構錶徵.在靜態空氣氣氛中用熱重-差示掃描量熱分析法(TG-DSC)對其進行瞭熱分析研究:168~436 ℃之間質量損失76.67%,最後的固體殘留物為聯苯骨架不完全燃燒的殘留物.在272 ℃有一箇放熱峰,在210、302 ℃分彆齣現彊吸熱峰.結果錶明該固態化閤物在168 ℃以下很穩定.
이4,4'-이(록갑기)련분화2,3-정이동-아린산삼갑지(1:1)가합물위원료합성료표제화합물,채용핵자공진보、질보、홍외광보화자외가견광보대화합물진행결구표정.재정태공기기분중용열중-차시소묘량열분석법(TG-DSC)대기진행료열분석연구:168~436 ℃지간질량손실76.67%,최후적고체잔류물위련분골가불완전연소적잔류물.재272 ℃유일개방열봉,재210、302 ℃분별출현강흡열봉.결과표명해고태화합물재168 ℃이하흔은정.
In this paper, 3, 3'-(biphenyl-4, 4'-diyl) dipentane-2,4-dione was synthesized using4,4'-bis(chloromethyl)biphenyl and 2,2,2-trimethoxy-4,5-dimethyl-1,3,2-dioxaphospholene as starting materials. Its molecule structure was characterized by ~1HNMR,MS, IR and UV-Vis spectra. The thermal properties of 3, 3'-( biphenyl-4, 4'-diyl) dipentane-2, 4-dione were studied based on the TG-DTG and DSC-DDSC analyses in a static air at-mosphere. In a temperature range from 168 ℃ to 436 ℃, a mass loss of 76.67% was observed.The last solid residue was consid-ered generally as the remnants of biphenyl skeleton after incom-plete combustion. The maximum peak of heat release at 272 ℃ in DTG was resulted from exothermal decomposition reactions. The maximum peak of heat absorption at 210 ℃ and 302 ℃ in DSC was resulted from endothermic reactions, respectively. The test re-sults showed the compound had higher thermal stability at 168 ℃.