Preparation of carboxyl‐functionalized polyhedral oligomeric silsesquioxane by a structural transformation reaction from soluble rod‐like polysilsesquioxane

Kozuma Tomoya; Kaneko Yoshiro

摘要

ABSTRACT > Carboxyl‐functionalized polyhedral oligomeric silsesquioxane (SQ; POSS‐COOH ) was successfully prepared by a structural transformation reaction, that is, a process of heating and concentrating soluble carboxyl‐functionalized rod‐like polySQ (PolySQ ‐COOH ) using the aqueous superacid trifluoromethanesulfonic acid (HOTf) as the catalyst and solvent. The obtained POSS‐COOH was a mixture of a cage‐like decamer (T <sub>10</sub> ‐POSS), which was the main product, and an octamer (T <sub>8</sub> ‐POSS) and a dodecamer (T <sub>12</sub> ‐POSS), which were the minor products. The product obtained by heating and concentrating PolySQ‐COOH using aqueous hydrochloric acid (HCl) as the catalyst and solvent was soluble polySQ rather than POSS. For comparison, heating and concentrating POSS‐COOH in aqueous HOTf and HCl were performed, which yielded POSS‐COOH and PolySQ‐COOH , respectively. Based on these results, the process of heating and concentrating each starting material ( PolySQ‐COOH and POSS‐COOH ) in aqueous HOTf afforded POSS‐COOH , and a similar process in aqueous HCl yielded PolySQ‐COOH . ? 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019 , 57 , 2511–2518 </abstract> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> <div class="translation abstracttxt"> <span class="zhankaihshouqi fivelineshidden" id="abstract"> <span>机译：</span><abstract type =“main”xml：lang =“en”> <标题类型=“main”>抽象</ title> > 羧基官能化多面体低聚Silsesquioxane（SQ; poss-cooh </ b> 通过结构转化反应成功制备，即加热和浓缩羧基官能化棒状多杆（Polysq -cooh </ b> ）使用水性超酸三氟甲磺酸（HotF）作为催化剂和溶剂。获得的 poss-cooh </ b> 是笼状的腐烂的混合物（t <sub> 10 </ sub> -poss），是主要产品和八寡头（t <sub> 8 </ sub> -poss）和dodecamer（t <sub> 12 </ sub> -POSS），这是次要产品。通过加热和浓缩获得的产品 polysq-cooh </ b> 使用盐酸水溶液（HCl）作为催化剂和溶剂是可溶性的多面动杆而不是POSS。用于比较，加热和浓缩 poss-cooh </ b> 在水溶液中进行，均产生水溶液和HCl poss-cooh </ b> 和 polysq-cooh </ b> ，分别。基于这些结果，加热和浓缩每个起始材料的过程（ polysq-cooh </ b> 和 poss-cooh </ b> ）在水性的水上提供 poss-cooh </ b> 和HCl水溶液中的类似方法产生 polysq-cooh </ b> 。还是2019 Wiley期刊，Inc.J.Colom。 SCI。，A部分：polym。化学。 2019 </ b> 那 57 </ i> ，2511-2518 </ p> </摘要> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> </div> <div class="record"> <h2 class="all_title" id="enpatent33" >著录项</h2> <ul> <li> <span class="lefttit">来源</span> <div style="width: 86%;vertical-align: text-top;display: inline-block;"> <a href='/journal-foreign-35621/'>《Journal of Polymer Science, Part A. Polymer Chemistry》</a> <b style="margin: 0 2px;">|</b><span>2019年第24期</span><b style="margin: 0 2px;">|</b><span>共8页</span> </div> </li> <li> <div class="author"> <span class="lefttit">作者</span> <p id="fAuthorthree" class="threelineshidden zhankaihshouqi"> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Kozuma Tomoya&option=202" target="_blank" rel="nofollow">Kozuma Tomoya;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Kaneko Yoshiro&option=202" target="_blank" rel="nofollow">Kaneko Yoshiro;</a> </p> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zkzz" style="display: none;">展开▼</span> </div> </li> <li> <div style="display: flex;"> <span class="lefttit">作者单位</span> <div style="position: relative;margin-left: 3px;max-width: 639px;"> <div class="threelineshidden zhankaihshouqi" id="fOrgthree"> <p>Graduate School of Science and EngineeringKagoshima University1‐21‐40 Korimoto Kagoshima 890‐0065 Japan;</p> <p>Graduate School of Science and EngineeringKagoshima University1‐21‐40 Korimoto Kagoshima 890‐0065 Japan;</p> </div> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zhdw" style="display: none;">展开▼</span> </div> </div> </li> <li > <span class="lefttit">收录信息</span> <span style="width: 86%;vertical-align: text-top;display: inline-block;"></span> </li> <li> <span class="lefttit">原文格式</span> <span>PDF</span> </li> <li> <span class="lefttit">正文语种</span> <span>eng</span> </li> <li> <span class="lefttit">中图分类</span> <span><a href="https://www.zhangqiaokeyan.com/clc/1184.html" title="有机化学">有机化学;</a></span> </li> <li class="antistop"> <span class="lefttit">关键词</span> <p style="width: 86%;vertical-align: text-top;"> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=carboxyl group&option=203" rel="nofollow">carboxyl group;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=inorganic materials&option=203" rel="nofollow">inorganic materials;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=inorganic polymers&option=203" rel="nofollow">inorganic polymers;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=polysiloxanes&option=203" rel="nofollow">polysiloxanes;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=POSS&option=203" rel="nofollow">POSS;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=silsesquioxane&option=203" rel="nofollow">silsesquioxane;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=superacid&option=203" rel="nofollow">superacid;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=transformation reaction&option=203" rel="nofollow">transformation reaction;</a> </p> <div class="translation"> 机译：羧基;无机材料;无机聚合物;聚硅氧烷;poss;silsesquioxane;超级酸;转化反应; </div> </li> </ul> </div> </div> <div class="literature cardcommon" id="literaturereference" style="display:none"> <div class="similarity "> <h3 class="all_title" id="enpatent111">引文网络</h3> <div class="referencetab clearfix"> <ul id="referencedaohang"> <li dataid="referenceul">参考文献</li> <li dataid="citationul">引证文献</li> <li dataid="commonreferenceul">共引文献</li> <li dataid="commoncitationul">同被引文献</li> <li dataid="tworeferenceul">二级参考文献</li> <li dataid="twocitationul">二级引证文献</li> </ul> </div> <div class="reference_details" id="referenceList"> <ul id="referenceul"></ul> <ul id="citationul"></ul> <ul id="commonreferenceul"></ul> <ul id="commoncitationul"></ul> <ul id="tworeferenceul"></ul> <ul id="twocitationul"></ul> </div> </div> </div> <div class="literature cardcommon"> <div class="similarity "> <h3 class="all_title" id="enpatent66">相似文献</h3> <div class="similaritytab clearfix"> <ul> <li class="active" >外文文献</li> <li >中文文献</li> <li >专利</li> </ul> </div> <div class="similarity_details"> <ul > <li> <div> <b>1. </b><a class="enjiyixqcontent" href="/journal-foreign-detail/0704020725817.html">Preparation of carboxyl‐functionalized polyhedral oligomeric silsesquioxane by a structural transformation reaction from soluble rod‐like polysilsesquioxane</a> <b>[J]</b> . <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Kozuma Tomoya&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">Kozuma Tomoya,</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Kaneko Yoshiro&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">Kaneko Yoshiro </a> <a href="/journal-foreign-35621/" target="_blank" rel="nofollow" class="tuijian_authcolor">Journal of Polymer Science, Part A. 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href="/academic-journal-cn_advanced-materials-industry_thesis/0201296412553.html">有机官能化系列笼型倍半硅氧烷纳米材料制备技术</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . </a> <span> <a href="/journal-cn-7696/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 新材料产业 </a> </span> <span> . 2009</span><span>,第10期</span> </span> </div> </li> <li> <div> <b>5. </b><a class="enjiyixqcontent" href="/academic-journal-cn_detail_thesis/0201296046496.html">多面体低聚倍半硅氧烷杂化丙烯酸树脂的制备及性能</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=陈雅&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 陈雅</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=安秋凤&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,安秋凤</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=李卫卫&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,李卫卫</a> <span> <a href="/journal-cn-56862/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 高分子材料科学与工程 </a> </span> <span> . 2020</span><span>,第9期</span> </span> </div> </li> <li> <div> <b>6. </b><a class="enjiyixqcontent" href="/academic-conference-cn_meeting-28402_thesis/020222007802.html">有机硅氧烷改性天然胶乳的研究Ⅰ.有机硅氧烷接枝改性天然胶乳的制备及结构表征</a> <b>[C]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=何映平&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 何映平</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=孙燕&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,孙燕</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=谭海生&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,谭海生</a> <span> <a href="/conference-cn-28402/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 中国热带作物学会2004年会 </a> <span> <span> . 2004</span> </span> </div> </li> <li> <div> <b>7. </b><a class="enjiyixqcontent" href="/academic-degree-domestic_mphd_thesis/02031757981.html">羧基与呋喃基官能化多面体低聚倍半硅氧烷的合成与应用</a> <b>[A] </b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=钟廷家&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 钟廷家</a> <span> . 2015</span> </span> </div> </li> </ul> <ul style="display: none;"> <li> <div> <b>1. </b><a class="enjiyixqcontent" href="/patent-detail/061202083069.html">多面体结构聚硅氧烷改性体、多面体结构聚硅氧烷系组合物、固化物及光半导体器件</a> <b>[P]</b> . <span> 中国专利： CN103119048B </span> <span> . 2016.06.01</span> </div> </li> <li> <div> <b>2. </b><a class="enjiyixqcontent" href="/patent-detail/06120101884532.html">多面体结构聚硅氧烷改性体、多面体结构聚硅氧烷系组合物、固化物及光半导体器件</a> <b>[P]</b> . <span> 中国专利： CN103119048A </span> <span> . 2013-05-22</span> </div> </li> <li> <div> <b>3. </b><a class="enjiyixqcontent" href="/patent-detail/06130424959857.html">PREPARATION OF POLYHEDRAL OLIGOMERIC SILSESQUIOXANE SILANOLS AND SILOXIDES FUNCTIONALIZED WITH OLEFINIC GROUPS</a> <b>[P]</b> . <span> 外国专利：  EP1931687A4 </span> <span> . 2011-05-04</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：具有烯烃基的多面体低聚倍半硅氧烷硅氧烷和硅氧烷的制备 </span> </p> </li> <li> <div> <b>4. </b><a class="enjiyixqcontent" href="/patent-detail/06130423103754.html">Preparation of polyhedral oligomeric silsesquioxane silanols and siloxides functionalized with olefinic groups</a> <b>[P]</b> . <span> 外国专利：  US8076443B2 </span> <span> . 2011-12-13</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：烯基官能化的多面体低聚倍半硅氧烷硅烷醇和氧化硅的制备 </span> </p> </li> <li> <div> <b>5. </b><a class="enjiyixqcontent" href="/patent-detail/06130425298211.html">PREPARATION OF POLYHEDRAL OLIGOMERIC SILSESQUIOXANE SILANOLS AND SILOXIDES FUNCTIONALIZED WITH OLEFINIC GROUPS</a> <b>[P]</b> . <span> 外国专利：  SG166863A1 </span> <span> . 2010-12-29</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：具有烯烃基的多面体低聚倍半硅氧烷硅氧烷和硅氧烷的制备 </span> </p> </li> </ul> </div> </div> </div> <div class="theme cardcommon" style="overflow: auto;display:none"> <h3 class="all_title" id="enpatent55">相关主题</h3> <ul id="subject"> </ul> </div> </div> </div> </div> <div class="right rightcon"> <div class="details_img cardcommon clearfix" style="margin-bottom: 10px;display:none;" > </div> </div> </div> <div id="thesis_get_original1" class="downloadBth" style="bottom: 19px;z-index: 999;" onclick="ywcd('0704020725817','4',7,2,1,'',this,24)" class="delivery" prompt="010401" 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