固体火箭技术
固體火箭技術
고체화전기술
JOURNAL OF SOLID ROCKET TECHNOLOGY
2014年
3期
381-386
,共6页
甘宁%肖啸%刘庆%卢先明%苏海鹏%葛忠学
甘寧%肖嘯%劉慶%盧先明%囌海鵬%葛忠學
감저%초소%류경%로선명%소해붕%갈충학
阳离子开环聚合%环三磷腈%氯化聚醚%合成%热性能
暘離子開環聚閤%環三燐腈%氯化聚醚%閤成%熱性能
양리자개배취합%배삼린정%록화취미%합성%열성능
cationic ring opening polymerization%cyclotriphosphazene%polyepichlorohydrin%synthesis%thermal property
以六氯环三磷腈、对羟基苯甲醛和环氧氯丙烷( ECH)为原料,依次经亲核取代反应、还原反应和阳离子开环聚合反应合成出环三磷腈基六臂氯化聚醚HCPCP。利用红外光谱、核磁共振、元素分析和蒸汽渗透压法( VPO)对所得中间体及HCPCP的结构进行了表征。重点研究了以PN-6OH为起始剂、ECH为聚合单体、三氟化硼乙醚络合物(BF3·Et2O)为催化剂的阳离子开环聚合反应,确定了最佳反应条件:以甲苯和1,2-二氯乙烷的混合溶剂( V(甲苯)∶ V(1,2-二氯乙烷)=1∶3)为反应溶剂,n(BF3·Et2O)∶ n(-OH)=6∶1,引发反应温度为40~50℃,聚合反应温度为0~5℃,并对产物HCPCP进行了热性能研究,结果表明,HCPCP的玻璃化转变温度Tg=-37.98℃,800℃时的残焦量为24.38%。
以六氯環三燐腈、對羥基苯甲醛和環氧氯丙烷( ECH)為原料,依次經親覈取代反應、還原反應和暘離子開環聚閤反應閤成齣環三燐腈基六臂氯化聚醚HCPCP。利用紅外光譜、覈磁共振、元素分析和蒸汽滲透壓法( VPO)對所得中間體及HCPCP的結構進行瞭錶徵。重點研究瞭以PN-6OH為起始劑、ECH為聚閤單體、三氟化硼乙醚絡閤物(BF3·Et2O)為催化劑的暘離子開環聚閤反應,確定瞭最佳反應條件:以甲苯和1,2-二氯乙烷的混閤溶劑( V(甲苯)∶ V(1,2-二氯乙烷)=1∶3)為反應溶劑,n(BF3·Et2O)∶ n(-OH)=6∶1,引髮反應溫度為40~50℃,聚閤反應溫度為0~5℃,併對產物HCPCP進行瞭熱性能研究,結果錶明,HCPCP的玻璃化轉變溫度Tg=-37.98℃,800℃時的殘焦量為24.38%。
이륙록배삼린정、대간기분갑철화배양록병완( ECH)위원료,의차경친핵취대반응、환원반응화양리자개배취합반응합성출배삼린정기륙비록화취미HCPCP。이용홍외광보、핵자공진、원소분석화증기삼투압법( VPO)대소득중간체급HCPCP적결구진행료표정。중점연구료이PN-6OH위기시제、ECH위취합단체、삼불화붕을미락합물(BF3·Et2O)위최화제적양리자개배취합반응,학정료최가반응조건:이갑분화1,2-이록을완적혼합용제( V(갑분)∶ V(1,2-이록을완)=1∶3)위반응용제,n(BF3·Et2O)∶ n(-OH)=6∶1,인발반응온도위40~50℃,취합반응온도위0~5℃,병대산물HCPCP진행료열성능연구,결과표명,HCPCP적파리화전변온도Tg=-37.98℃,800℃시적잔초량위24.38%。
Polyepichlorohydrin adhesive based on cyclotriphosphazene(HCPCP) was prepared by reaction of nucleophilic sub-stitution,reduction and cationic ring opening polymerization in sequence with hexachlorocyclotriphosphazene,p-hydroxybenzaldehyde and epichlorohydrin( ECH) as raw materials. The product was structurally characterized by FT-IR,NMR,elemental analysis and va-por pressure osmometry(VPO). The cationic ring opening polymerization reaction of Hexakis[p-(hydroxymethyl)phenoxy]cyclot-riphosphazene(PN-6OH),ECH and BF3·Et2O was investigated. The optimized process conditions were: the mixture of toluene and 1,2-dichloroethane(V(toluene):V(1,2-dichloroethane)=1 ∶ 3) was used as reaction reagent,n(BF3·Et2O): n(-OH)=6 ∶ 1,initiation reaction temperature was 40~50℃,polymerization temperature was 0~5℃. The thermal properties of HCPCP were also studied. The results show that the glass state temperature was -37.98℃ and the char yield at 800℃ was 24.38%.