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第 2 期                   王艳丽,等:  聚十二烷基三苯乙炔基硅烷树脂的制备与热性能                                    ·205·


            过 Grignard 反应成功制备 DTPES,产物结构经 FTIR                 [12]  Zhou  Q,  Feng  X,  Ni  L,  et al.  Novel  heat  resistant  methyl-tri
                                                                   (phenylethynyl) silane resin: synthesis, characterization and thermal
            和 NMR 确证,该方法能够实现该系列单体在温和                               properties[J]. J Appl Polym Sci, 2006, 102(3): 2488-2492.
                                                               [13]  Liu  H,  Harrod  J.  Copper  (I)  chloride-catalyzed  cross-
            条件下的简易合成,利于产品的工业化生产。                                   dehydrocouplingreactions between silanes and ethynyl compounds: A
                                                                   new method for the copolymerization of silanes and alkynes[J]. Can J
                 (2)热重分析显示,PDTPES 树脂在升温速率                          Chem, 1990, 68(7): 1100-1104.
            为 10  ℃/min 下的 T d5 分解温度为 440  ℃,800  ℃            [14]  Kownacki I, Orwat B, Marciniec B, et al. A new and efficient route
                                                                   for  the  synthesis  of  alkynyl  functionalized  silicon  derivatives[J].
            下树脂残炭率在 48.1%,树脂具有较好的热稳定性,                             Tetrahedron Lett, 2014, 55(2): 548-550.
                                                               [15]  Iwasaki  T,  Shimizu  R,  Imanishi  R,  et al.  Copper-catalyzed
            能够满足高温材料树脂基体的使用要求,有望成为                                 regioselective hydroalkylation of 1, 3-dienes with alkyl fluorides and
                                                                   grignard reagents[J]. Angew Chem Int Ed, 2015, 54(34): 9347-9350.
            耐高温复合材料用树脂基体。                                      [16]  Chen Mingfeng (陈明锋), Zhou Quan (周权), Ni Lizhong (倪礼忠),
                 (3)通过 Kissinger、Ozawa、Achar、Cosat-                et al. Synthesis and fluorescence properties of conjugated monomers
                                                                   containing  phenylacetylene[J].  Polymer  Materials  Science  and
            Redfern、Friedman 和 Vyazonvkin-Weight 法这 6 种            Engineering (高分子材料科学与工程), 2013, 29(12): 1-4.
                                                               [17]  Tan D, Wang Y, Li Z, et al. Synthesis and cure kinetics of diphenyl
            热分解动力学方法求得树脂的热分解活化能 E a 分别                             (diphenylethynyl)silane  monomer[J].  Res  Chem  Intermed,  2013,
                                                                   39(7): 3427-3440.
            为 182.76 、 181.53 、 179.48 、 179.45 、 187.53 和     [18]  Tan D, Wu X, Wang Y, et al. Synthesis, characterization and curing
            178.33 kJ/mol,活化能相差不大;指前因子分别为                          behavior of methyl-tri (phenylethynyl)silane[J]. Res Chem Intermed,
                                                                   2016, 42(5): 4669-4681
                             10
                   12
                                      12
                                                11
            1.05×10 、3.40×10 、3.79×10 、1.88×10 、5.73×10  11    [19]  Zhou Q, Feng X, Ni L, et al. Thermal characteristics and pyrolysis of
                                                                   methyl-di  (phenylethynyl)  silane  resin[J].  J  Appl  Polym  Sci,  2007,
                        s ,分解过程符合第 26 号机理函数,
            和 1.52×10 11  –1                                       103(1): 605-610.
            即随机 成核 和随后 生长 ,其微 分式 为: f( )                     [20]  Hu Rongzu (胡荣祖), Gao Shengli (高胜利), Zhao Fengqi (赵凤起).
                                                                   Thermal analysis kinetics[M]. Beijing: Beijing Science Press (北京
                 1                    3                            科学出版社), 2008: 151-159.
             2   2  ;积分式为: g( )    ;热分解动力学方程              [21]  Guo K, Li Y, Zhu Y, et al. Thermal curing and degradation behavior
                                      2
             3                                                     of  silicon-containing  arylacetylene  resins[J].  Polym  Degrad  Stab,
                                                                   2016, 131: 98-105.
                         
                 d   9.65 10 11    181.51 10     3  2   1  [22]  Ratio  J,  Dynes  P,  Hammeresh  C.  The  synthesis  and  thermal
            为:               exp                 2  。通过      polymerization of 4, 4′- diethynylphenylether[J]. J Polym Sci Polym
                 d                   RT  T      3         [23]  Wu  Xiaole  (吴小乐).  Synthesis,  cure  kinetics  and  properties  of
                                                                   Chem, 1980, 18(3): 1035-1046.
            热分析动力学的分析显示,树脂分解活化能较高,                                 triphenylthynylsilane[D].Huainan:  Anhui  University  of  Science  and
                                                                   Technology (安徽理工大学), 2016.
            形成的网络交联结构紧密,树脂分解过程中显示随                             [24]  Xu Yuan (徐远). Synthesis,kinetics and property of arylalkynylsilane
                                                                   resin[D]. Huainan:Anhui University of Science and Technology (安
            机性,不是单一方向的断链反应。                                        徽理工大学), 2017.
                                                               [25]  Tan  Dexin  (谭德新).  Preparations,  structures  and  properties  of
            参考文献:                                                  triphenylethynylsilaneresins  and  their  SiC/C  (TiN/C)  composite
                                                                   woodceramics[D]. Hefei: Hefei University of Technology (合肥工业
            [1]   Sastri S, Armistead J, Keller  T. Cure  kinetics of a  multisubstituted   大学), 2011.
                 acetylenic monomer[J]. Polymer, 1995, 36(7): 1449-1454.     [26]  Tan  D,  Shi  T,  Li  Z.  Synthesis,  characterization  and  non-isothermal
            [2]   Chen  M,  Liu  C,  Lin  J.  Correlation  of  cross-linked  structures  and   curing kinetics of two silicon-containing arylacetylenicmonomers[J].
                 properties in the characterization of dimethyl-diphenylethynyl-silane   Res Chem Intermed, 2011, 37(8): 831-845.
                 using  DSC,  TGA  and  Py-GC/MS  analysis[J].  Polym  Degrad  Stab,   [27]  Naktiyok  J,  Bayrakceken  H,  Özer  A,  et al.  Kinetics  of  thermal
                 2015, 112: 35-42.                                 decomposition  of  phospholipids  obtained  from  phosphate  rock[J].
            [3]   Han  M,  Guo  K,  Wang  F,  et al.  Synthesis,  characterization,  and   Fuel Process Technol, 2013, 116(4): 158-164.
                 properties  of  thermosets  based  on  the  cocuring  of  an  acetylene-   [28]  Kissinger  H.  Reaction  kinetics  in  differential  thermal  analysis[J].
                 terminated  liquid-crystal  and  silicon-containing  arylacetylene   Analytical Chemistry, 1957, 29(11): 1702-1706.
                 oligomer[J]. J Appl Polym Sci, 2017, 134(33): 45141-45151.     [29]  Ozawa  T.  A  new  method  of  analyzing  thermogravimetric  data[J].
            [4]   Itoh  M,  Inoue  K,  Iwata  K,  et al.  A  heat-resistant  silicon-based   Bull Chem Soc Jpn, 1965, 38: 1881-1886.
                 polymer[J]. Adv Mater, 1997, 9(15): 1187-1190.     [30]  Vlase T, Vlase G, Birta N, et al. Comparative results of kinetic data
            [5]   Chen  H,  Xin  H,  Lu  J,  et al.  Synthesis  and  properties  of  poly   obtained with different methods for complex decomposition steps[J].
                 (dimethylsilylene-ethynylene-phenoxyphenoxyphenylene-ethynylene)[  J Therm Anal Calorim, 2007, 88(3): 631-635.
                 J]. High Perform Polym, 2016, 29(5): 1-7.     [31]  Ren Y, Cheng B, Zhang J, et al. Thermal degradation kinetics of N,
            [6]   Bu X, Zhou Y, Huang F. The strengthening and toughening effects of   N'-di  (diethoxythiophosph-oryl)-1,  4-phenylenediamine[J].  Chem
                 a  novel  octa  (propargylpropylsulfide)  POSS    (OPPSP)  on   Res Chinese U, 2008, 24(5): 628-631.
                 silicon-containing  arylacetylene    (PSA)  resin[J].  Mater  Lett,  2016,   [32]  Vyazovkin S, Wight C. Model-free and model-fitting approaches to
                 174: 21-23.                                       kinetic  analysis  of  isothermal  and  nonisothermal  data[J].
            [7]   GuYuanbo  (顾渊博),  HuYanhong  (扈艳红),  Du  Lei  (杜磊),  et al.   Thermochim Acta, 1999, 340/341: 53-68.
                 Reinforcement and tougheness of quartz fiber/siliconcontainingarylacetylene   [33]  Díaz-Celorio  E,  Franco  L,  Márquez  Y,  et al.  Thermal  degradation
                 with  heatresistantpolyetherimide  macromolecular  coupling  agent[J].   studies  on  homopolymers  and  copolymers  based  on  trimethylene
                 Chem J Chin U (高等学校化学学报), 2017, 38(9): 1670-1677.     carbonate  and  glycolide  units[J].  Thermochimica  Acta,  2012,  528:
            [8]   Wrackmeyer B,  Bayer S,  Tok O, et al. Alkynylsilanes and alkynyl   23-31.
                 (vinyl)  silanes.  Synthesis,  molecular  structures  and  multinuclear   [34]  Gao  J,  Tang  Q,  Chen  X.  Decomposition  kinetics  and  process
                 magnetic resonance study[J]. Zeitschrift Für Naturforschung B, 2010,   experiments  on  dolomite[J].  Journal  of  Functional  Materials,  2012,
                 65(6): 725-744.                                   43(23): 3194-3196.
            [9]   Chen  Qi  (陈麒),  Li  Yang  (李扬), Dai Zeliang  (戴泽亮),  et al.   [35]  Friedman H. Kinetics of thermal degradation of char-forming plastics
                 Synthesis  and  characterization  of  methyl-di  (phenylethynyl)  silane   from thermogravimetry[J]. J Polym Sci Part C: Polym Symp, 1964,
                 and its network polymer[J]. Acta Chimica Sinica (化学学报), 2005,   6(1): 183-195.
                 63(3): 254-258.                               [36]  Vyazovkin E. Evaluation of activation energy of thermally stimulated
            [10]  Tan D, Wu X, Wang Y, et al. Synthesis, characterization and curing   solid-state  reactions  under  arbitrary  variation  of  temperature[J].  J
                 behavior of propyl-tri (phenylethynyl) silane[J]. Iran Polym J, 2016,   Comput Chem, 1997, 18: 393-402.
                 25(8): 687-695.                               [37]  Zhang Laying (张腊莹), Zhu Xinhua (朱欣华), Qing Hui (卿辉), et
            [11]  Kim  C,  Jeong  K,  Jung  I.  Progress  toward  limiting  generation  of   al. Thermal behavior and non-isothermal decomposition kinetics of
                 dendritic  ethynylsilanes  (PhC≡C) 4−nMe nSi  (n=  0~2)[J].  J  Polym  Sci   3, 4-bis (3', 5'-dinitrophenyl-1'-yl)furoxan[J]. Journalof Solid Rocket
                 Polym Chem, 2000, 38(15): 2749-2759.              Technology (固体火箭技术), 2011, 34(5): 623-627.
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