腈氧化物固化端羟基聚丁二烯  

Curing of Hydroxyl-terminated Polybutadiene(HTPB) with Nitrile Oxide

作　　者：王晓川[1] 舒远杰[1] 雷永林[2] 樊亚勤 卢先明[1] 舒尧 WANG Xiao-chuan1 , SHU Yuan-jie1 , LEI Yong-lin2, FAN Ya-qin2, LU Xian-ming1 , SHU Yao1(1. Xi＇an Modern Chemistry Research Institute Xi＇an 710065, Shaanxi, China; 2. Southwest University of Science and Technology, Mianyang 621000, Sichuan , Chin)

机构地区：[1]西安近代化学研究所,陕西西安710065 [2]西南科技大学材料与工程学院,四川绵阳621000

出　　处：《精细化工》2018年第4期695-699,共5页Fine Chemicals

基　　金：国家自然科学基金(51373159)~~

摘　　要：首先,以1,2,4,5-四甲基苯为原料,经溴甲基化、氧化、缩合、脱氢氧化4步反应,得到了四甲基对苯二腈氧化物（TTNO）,各步产物的结构用FTIR、1HNMR和13CNMR进行了表征。然后,将TTNO用于端羟基聚丁二烯（HTPB）的室温固化,按照固化剂腈氧基团与HTPB中双键的物质的量之比（R值）分别为0.03、0.04、0.05、0.06和0.07制备了哑铃形聚合物弹性体。最后,通过FTIR、拉伸强度测试、DSC、TG和接触角测试对聚合物弹性体的结构和性能进行了考察。结果显示：随着R值的增加,聚合物弹性体的拉伸强度从0.135 MPa增至0.416MPa,玻璃化转变温度（Tg）从-73.08℃增至-66.70℃,接触角从98.80°减小到73.54°。在室温下,四甲基对苯二腈氧化物能实现HTPB的固化,固化后的聚合物弹性体有望用于复合固体推进剂。Tetramethyl-terephthalobisnitrile oxide（TTNO） was first synthesized from 1,2,4,5-tetramethylbenzene via bromomethylation,oxidation,condensation and dehydrogenation reactions. These compounds were characterized by means of FTIR,1 HNMR and13 CNMR. Then,TTNO was used to cure HTPB under room temperature. A series of dumbbell-shaped cross-linked polymers with different molar ratio of nitrile oxygen groups to carbon-carbon double bond were prepared,in which,the molar ratio of—CNO and CC was defined as R value,R = 0. 03,0. 04,0. 05,0. 06,0. 07. Finally,the cross-linked polymers were investigated by FTIR,tensile strength test,DSC,TG and contact angle test. The results showed that with the increase of R value,the tensile strength of cross-linked polymer increased from0. 135 MPa to 0. 416 MPa,and the glass transition temperature（Tg） increased from-73. 08 ℃ to-66. 70 ℃,however,the contact angle decreased from 98. 80° to 73. 54°. As a result,TTNO can cure HTPB under room temperature,and the cross-linked polymers are expected to be used in future composite solid propellants.

关 键 词：腈氧化物 室温 固化剂 HTPB 聚合物弹性体 粘合剂 

分 类 号：TQ433.42[化学工程]