固体火箭技术
固體火箭技術
고체화전기술
JOURNAL OF SOLID ROCKET TECHNOLOGY
2014年
4期
535-540
,共6页
肖啸%甘宁%刘庆%卢先明%莫洪昌%葛忠学
肖嘯%甘寧%劉慶%盧先明%莫洪昌%葛忠學
초소%감저%류경%로선명%막홍창%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、苯酚钠和环氧氯丙烷( 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,合成出环三磷腈基三臂氯化聚醚TCPCP。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TCPCP的结构进行了表征。重点研究了以1,3,5-三(4-羟甲基苯氧基)-1′,3′,5′-三(苯氧基)环三磷腈(PN-3OH)为起始剂、ECH为聚合单体、三氟化硼乙醚络合物( BF3·Et2 O)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)=1∶1,引发反应温度为20~25℃,聚合反应温度为0℃。并对产物TCPCP进行了热性能研究,结果表明,TCPCP的玻璃化转变温度( Tg )为-43.66℃,800℃时的残焦量为4.89%。
以六氯環三燐腈、對羥基苯甲醛、苯酚鈉和環氧氯丙烷( 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,閤成齣環三燐腈基三臂氯化聚醚TCPCP。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TCPCP的結構進行瞭錶徵。重點研究瞭以1,3,5-三(4-羥甲基苯氧基)-1′,3′,5′-三(苯氧基)環三燐腈(PN-3OH)為起始劑、ECH為聚閤單體、三氟化硼乙醚絡閤物( BF3·Et2 O)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)=1∶1,引髮反應溫度為20~25℃,聚閤反應溫度為0℃。併對產物TCPCP進行瞭熱性能研究,結果錶明,TCPCP的玻璃化轉變溫度( Tg )為-43.66℃,800℃時的殘焦量為4.89%。
이륙록배삼린정、대간기분갑철、분분납화배양록병완( ECH)위원료,의차경친핵취대반응、환원반응화양리자개배취합반응,합성출배삼린정기삼비록화취미TCPCP。이용홍외광보、핵자공진、원소분석화증기삼투압법( VPO),대소득중간체급TCPCP적결구진행료표정。중점연구료이1,3,5-삼(4-간갑기분양기)-1′,3′,5′-삼(분양기)배삼린정(PN-3OH)위기시제、ECH위취합단체、삼불화붕을미락합물( BF3·Et2 O)위최화제적양리자개배취합반응,학정료최가반응조건:이갑분화1,2-이록을완적혼합용제(V(갑분)∶ V(1,2-이록을완)=1∶3)위반응용제,n(BF3·Et2O)∶ n(-OH)=1∶1,인발반응온도위20~25℃,취합반응온도위0℃。병대산물TCPCP진행료열성능연구,결과표명,TCPCP적파리화전변온도( Tg )위-43.66℃,800℃시적잔초량위4.89%。
Three armed polyepichlorohydrin adhesive based on cyclotriphosphazene ( TCPCP ) was prepared by nucleophilic substitution, reduction and cationic ring opening polymerization reaction in sequence using hexachlorocyclotriphosphazene, p-hydroxybenzaldehyde, sodium phenate and epichlorohydrin(ECH) as raw materials.The products were structurally characterized by FT-IR,NMR,elemental analysis and vapor pressure osmometry(VPO).The cationic ring opening polymerization reaction of Hexakis [ p-( hydroxymethyl) phenoxy] cyclotriphosphazene( PN-3OH) ,ECH and BF3 ·Et2 O was investigated. The optimized process condi-tions were:the mixture of toluene and 1,2-dichloroethane( V( toluene):V( 1,2-dichloroethane)=1 ∶ 3) used as reaction reagent,n (BF3·Et2O) ∶ n(-OH)=1 ∶ 1, initiation reaction temperature was 20~25℃, polymerization temperature was 0℃.The thermal properties of TCPCP were also studied.The results show that the glass state temperature is -43.66 ℃ and the char yield at 800℃is 4.89%.