钢铁, 2017, 52(6): 83-86.
10.13228/j.boyuan.issn0449-749x.20160519
低温轧制提高65Mn盘条塑韧性能机理分析

晁月林 1, , 张玮 2, , 邓素怀 3, , 孙齐松 4, , 柳洋波 5,

1.首钢技术研究院特钢所,北京 100043;绿色可循环钢铁流程北京市重点实验室,北京 100043;
2.首钢技术研究院特钢所,北京,100043;
3.首钢技术研究院特钢所,北京,100043;
4.首钢技术研究院特钢所,北京,100043;
5.首钢技术研究院特钢所,北京,100043

通过常规工艺、低温开轧、低温精轧3种试验工艺研究了低温轧制对提高65Mn塑韧性能的影响,利用金相显微镜OM、扫描电镜SEM、EBSD等分析了3种试验工艺的组织、大小角度晶界、晶粒尺寸以及片层间距,研究结果表明,低温工艺显著提高弹簧钢的面缩率,降低同圈波动;大小角度晶界、细化的原始奥氏体晶粒与珠光体球团、片层间距是弹簧钢塑韧性能提高的关键所在.
引用: 晁月林, 张玮, 邓素怀, 孙齐松, 柳洋波 低温轧制提高65Mn盘条塑韧性能机理分析. 钢铁, 2017, 52(6): 83-86. doi: 4-丁炔(BOZ),所得镀层表面形貌及组成结构用扫描电镜与X射线衍射仪进行表征,得到了光亮的Ni-P-C-O镀层,镀层硬度高,耐酸蚀性强;探讨了BOZ在反应体系中的作用机理.结果表明,BOZ不仅是光亮剂,而且参与该体系的氧化还原反应,BOZ分解反应的宏观动力学表现为准一级;当BOZ的初始含量为60~123 mg/dm3时,其参与氧化还原的量与温度和初始浓度呈正相关性,温度起主导作用;当BOZ的初始含量为123~240 mg/dm3时,其参与氧化还原的量与温度和初始浓度呈负相关性,浓度起主导作用.","authors":[{"authorName":"刘少友","id":"889ea17d-4a66-4110-87e1-a3810f28acd6","originalAuthorName":"刘少友"},{"authorName":"唐文华","id":"651c408b-8ff2-45fe-a7fb-e5ee794a1452","originalAuthorName":"唐文华"},{"authorName":"邹勇","id":"6c8e5ee7-95f0-42f4-8128-3c2918d347ec","originalAuthorName":"邹勇"},{"authorName":"肖尊宏","id":"199b6fbf-dd1f-4a43-98fa-f9761027f32d","originalAuthorName":"肖尊宏"}],"doi":"10.3969/j.issn.1001-1560.2006.09.004","fpage":"10","id":"fa1625ba-6b7e-40c9-9588-31ba90c130f1","issue":"9","journal":{"abbrevTitle":"CLBH","coverImgSrc":"journal/img/cover/CLBH.jpg","id":"7","issnPpub":"1001-1560","publisherId":"CLBH","title":"材料保护"},"keywords":[{"id":"a7018b1c-e47d-47ac-8dc4-86e044533b07","keyword":"化学镀","originalKeyword":"化学镀"},{"id":"ad26abce-e779-4479-afc7-44a35522d5a4","keyword":"镍-磷-氧-碳镀层","originalKeyword":"镍-磷-氧-碳镀层"},{"id":"5d7dcd4d-b2a9-4946-b052-a0b0e0bb5609","keyword":"1","originalKeyword":"1"},{"id":"88444d6d-ee6a-410c-88e1-58f112ff46c9","keyword":"4-丁炔","originalKeyword":"4-丁炔二醇"},{"id":"6de3015f-dd6e-4ddb-8119-aa7a6629e706","keyword":"光亮剂","originalKeyword":"光亮剂"},{"id":"c4e20ca4-39b4-4356-a940-018025d9e98d","keyword":"表征","originalKeyword":"表征"},{"id":"91e89620-d77f-46bf-b5d0-d7568fd8ef92","keyword":"作用机理","originalKeyword":"作用机理"}],"language":"zh","publisherId":"clbh200609004","title":"镍-磷-碳-氧化学镀层的制备、表征及1,4-丁炔在体系中的作用","volume":"39","year":"2006"},{"abstractinfo":"为了探讨1,4-丁炔对纳米晶镍镀层硬度和耐蚀性的影响,采用直流电沉积法在黄铜表面制备了纳米晶镍镀层.利用X7000 X射线衍射仪、FEI Quanta600 FE-SEM扫描电镜、DUH-211S动态超显微微米压痕仪、动电位极化曲线及阻抗谱,研究了不同浓度1,4-丁炔对镍镀层结构、硬度及耐蚀性的影响规律.结果表明:随着镀液中1,4-丁炔浓度的增加,镍镀层晶面的择优取向由(200)织构向(111)转变,晶粒尺寸减小;镍镀层硬度增加,在1,4丁炔浓度为0.5 g/L时达到654 HV;在3.5%NaCl(质量分数)溶液中当1,4-丁炔浓度为0.1 g/L时,镍镀层的耐腐蚀性最好.","authors":[{"authorName":"朴楠","id":"54537e43-9d6e-4012-a4f4-2cc803bec4f9","originalAuthorName":"朴楠"},{"authorName":"陈吉","id":"03ef006d-07e4-41c8-a20f-25fe20c1746f","originalAuthorName":"陈吉"},{"authorName":"孙彦伟","id":"f0a9f847-41b1-4c7f-a65b-354f248f4044","originalAuthorName":"孙彦伟"},{"authorName":"许志显","id":"7404f5bd-aabe-4dc8-8872-e79331d5a7cb","originalAuthorName":"许志显"},{"authorName":"陈晓明","id":"d0f7765d-41bb-4ba0-860c-6829619bf1f9","originalAuthorName":"陈晓明"},{"authorName":"韩啸","id":"20cea98d-b1f3-4bdd-8620-c5c911e9ab68","originalAuthorName":"韩啸"}],"doi":"","fpage":"5","id":"8ce28b1f-8787-441a-b5dc-102c170bb3d4","issue":"2","journal":{"abbrevTitle":"CLBH","coverImgSrc":"journal/img/cover/CLBH.jpg","id":"7","issnPpub":"1001-1560","publisherId":"CLBH","title":"材料保护"},"keywords":[{"id":"d420935d-9bbf-4619-af3e-116b7669092a","keyword":"直流电沉积","originalKeyword":"直流电沉积"},{"id":"aa4e02c1-c788-4c1b-a0b5-e8b31ee99d0c","keyword":"纳米晶镍","originalKeyword":"纳米晶镍"},{"id":"c02fbb8e-a58b-4bb7-a4fc-195d7e86195b","keyword":"1,4-丁炔","originalKeyword":"1,4-丁炔二醇"},{"id":"2ba9697c-538f-473e-a4bb-1e8c73eb099d","keyword":"镀层结构","originalKeyword":"镀层结构"},{"id":"59382766-5184-4a70-b1ce-911a29bd45a8","keyword":"硬度","originalKeyword":"硬度"},{"id":"bc104d1d-2959-4c4b-b2fd-f946e6535e3c","keyword":"耐蚀性","originalKeyword":"耐蚀性"}],"language":"zh","publisherId":"clbh201502002","title":"1,4-丁炔对纳米晶镍镀层结构及性能的影响","volume":"48","year":"2015"},{"abstractinfo":"概述了以炔醛法合成1,4-丁炔催化剂的最新研究,通过介绍有机锂催化剂、Lewis酸催化剂、铜铋催化剂在炔醛化反应中的应用,分析了炔醛化反应原理及存在的副反应.重点介绍了铜铋催化剂在工业炔醛法生产1,4-丁炔中的研究及应用,讨论了载体、颗粒大小、金属负载量对铜铋催化剂性能的影响,分析了催化剂结构与催化效果之间的关系,并展望了催化剂的发展前景.","authors":[{"authorName":"杨桂花","id":"5ed6b0db-5b19-484d-afa0-dfe1aae0f1d7","originalAuthorName":"杨桂花"},{"authorName":"王吉德","id":"07690a0f-dfc8-44ad-84f0-d2a668dbd158","originalAuthorName":"王吉德"},{"authorName":"徐世美","id":"b37d7c74-5cab-4482-b585-f90da3b46436","originalAuthorName":"徐世美"},{"authorName":"谢亚红","id":"66677b49-2705-4c5e-bb34-be554f45be4a","originalAuthorName":"谢亚红"}],"doi":"10.11896/j.issn.1005-023X.2014.19.014","fpage":"68","id":"942e7a5e-28c7-45a3-bb7a-9b48ff45d49a","issue":"19","journal":{"abbrevTitle":"CLDB","coverImgSrc":"journal/img/cover/CLDB.jpg","id":"8","issnPpub":"1005-023X","publisherId":"CLDB","title":"材料导报"},"keywords":[{"id":"545499aa-e8c3-41b9-86e1-98351efbd682","keyword":"1,4-丁炔","originalKeyword":"1,4-丁炔二醇"},{"id":"dadd8b4e-fca2-4cf7-8fac-96e13a381150","keyword":"1,4-","originalKeyword":"1,4-丁二醇"},{"id":"c24e0e2a-2ccf-4b44-9098-286730d14a98","keyword":"炔醛法","originalKeyword":"炔醛法"},{"id":"fe0037d1-0532-4625-a56d-7ea551362b6f","keyword":"炔","originalKeyword":"炔醇"},{"id":"8032a36a-b750-498f-9609-ed2568d19376","keyword":"催化剂","originalKeyword":"催化剂"}],"language":"zh","publisherId":"cldb201419014","title":"炔醛法合成1,4-丁炔催化剂研究进展","volume":"28","year":"2014"},{"abstractinfo":"研究了硫酸盐镀镍电解液中1,4-丁炔对电解液电流效率、分散能力、阴极极化及镍镀层光亮度、硬度及内应力的影响.采用扫描电镜和X-射线衍射分析表征了镍镀层表面形貌和微观结构.结果表明,1,4-丁炔的加入使镍镀层的光亮度有所改善,但达不到镜面光亮;而对电解液的电流效率、分散能力影响不大;当ρ(1,4-丁炔)达0.3 g/L时,镍镀层的硬度逐渐减小,镍镀层的拉应力则先增大后略有降低;继续增加1,4-丁炔的质量浓度,镍镀层的硬度和拉应力随之增大;在较低的过电位下1,4-丁炔能够显著增加镍沉积的电位,细化镍镀层晶粒尺寸,使其表面更加平滑;呈现出(200)面择优取向.","authors":[{"authorName":"李延伟","id":"b50b0892-1a7e-45a0-8829-ecc4d08c3bb9","originalAuthorName":"李延伟"},{"authorName":"黄晓曦","id":"5f9f41a1-accc-4e6c-bf7e-becd278448fd","originalAuthorName":"黄晓曦"},{"authorName":"姚金环","id":"d5008929-0f14-4151-961f-5e762bbbbf54","originalAuthorName":"姚金环"},{"authorName":"尚雄","id":"bf44e012-e15c-47d7-8ccf-4c65366309ad","originalAuthorName":"尚雄"},{"authorName":"杨哲龙","id":"59b87f18-4fb4-4942-a615-a96decc94d1e","originalAuthorName":"杨哲龙"}],"doi":"10.3969/j.issn.1001-3849.2011.10.002","fpage":"8","id":"feeae69d-fe2b-473e-8429-9481656b800a","issue":"10","journal":{"abbrevTitle":"DDYJS","coverImgSrc":"journal/img/cover/DDYJS.jpg","id":"20","issnPpub":"1001-3849","publisherId":"DDYJS","title":"电镀与精饰 "},"keywords":[{"id":"adc6d0d1-7421-4db4-9cbe-e2809d5f793e","keyword":"电镀镍","originalKeyword":"电镀镍"},{"id":"2d534ba3-5e6e-4a32-af33-fee78ed60021","keyword":"硫酸盐","originalKeyword":"硫酸盐"},{"id":"cf6cbb98-06ec-4f1f-b396-446271af2ccf","keyword":"1,4-丁炔","originalKeyword":"1,4-丁炔二醇"},{"id":"1c8c5cef-897f-4588-ac0e-35f8ee2a54ba","keyword":"镀层性能","originalKeyword":"镀层性能"},{"id":"01c20294-b89c-44e9-98ea-a6990452dad9","keyword":"镀液性能","originalKeyword":"镀液性能"}],"language":"zh","publisherId":"ddjs201110002","title":"1,4-丁炔对硫酸盐镀镍液及镀层性能的影响","volume":"33","year":"2011"},{"abstractinfo":"由1,4-碘代苯出发,经过两步Sonogashira偶联反应合成了标题配合物2-甲基4.(4-(吡啶-3-乙炔基)苯基)-3-丁炔-2-.通过1H NMR、13C NMR核磁共振、Ⅹ-射线单晶衍射等手段对化合物的结构进行了表征.结果表明,该化合物晶体属于单斜晶系,空间群为P21/c.晶体学参数:a=3.3321 (4) nm,b=1.00539(11) nm,c=0.89158(10) nm,α =90.00°,β=92.442(2)°,y=90.00°,V=2984.2(6) nm3,Z =4.","authors":[{"authorName":"刘巧茹","id":"a94a9c56-96ea-418c-81bf-fd725626ddbb","originalAuthorName":"刘巧茹"},{"authorName":"张晓丽","id":"d0ac937f-3eac-4066-a18c-eb99480c2d29","originalAuthorName":"张晓丽"},{"authorName":"程国平","id":"af3bd056-1846-4e49-ba9c-cce859d700b3","originalAuthorName":"程国平"},{"authorName":"杨凤岭","id":"923eda08-28e1-42d8-919b-fdbad5b2132a","originalAuthorName":"杨凤岭"}],"doi":"","fpage":"2461","id":"8f96c62f-fa97-4898-92f0-3058ac548522","issue":"11","journal":{"abbrevTitle":"RGJTXB","coverImgSrc":"journal/img/cover/RGJTXB.jpg","id":"57","issnPpub":"1000-985X","publisherId":"RGJTXB","title":"人工晶体学报"},"keywords":[{"id":"67143600-f6a6-42f9-aa69-8d8cbe30c608","keyword":"合成","originalKeyword":"合成"},{"id":"cec39769-9c14-4b64-987f-7911f3efde7f","keyword":"晶体结构","originalKeyword":"晶体结构"},{"id":"45c1d8cc-f2c1-4ede-9a15-6879237fe67e","keyword":"2-甲基-4-(4-(吡啶-3-乙炔基)苯基)-3-丁炔-2-","originalKeyword":"2-甲基-4-(4-(吡啶-3-乙炔基)苯基)-3-丁炔-2-醇"}],"language":"zh","publisherId":"rgjtxb98201311043","title":"2-甲基4-(4-(吡啶-3-乙炔基)苯基)-3-丁炔-2-的合成及晶体结构","volume":"42","year":"2013"},{"abstractinfo":"用电化学方法和红外光谱技术研究了1,4-丁炔缓蚀剂在环氧涂料中缓蚀作用。结果表明:缓蚀剂的加入可以明显改变涂层的阻抗,当缓蚀剂加入量小于0.5mass%时,涂层的阻抗随着缓蚀剂量的增多而增大;对所测得的缓蚀涂层的交流阻抗数据进行似合并结合红外光谱分析认为,在基底和涂层之间生成了一层不完整的聚合物覆盖膜,在此基础上采用电化学技术探讨了此覆盖膜在涂层中的缓蚀机理。","authors":[{"authorName":"陈立庄","id":"8d4a84b1-517b-4af1-a0bc-67cefc7a1b4c","originalAuthorName":"陈立庄"},{"authorName":"高延敏","id":"97d2f423-9bbf-438e-9477-76508400f85b","originalAuthorName":"高延敏"}],"categoryName":"|","doi":"","fpage":"332","id":"ea2b86a3-b04e-461a-94bd-37ac4730d9ee","issue":"6","journal":{"abbrevTitle":"ZGFSYFHXB","coverImgSrc":"journal/img/cover/中国腐蚀封面19-3期-01.jpg","id":"81","issnPpub":"1005-4537","publisherId":"ZGFSYFHXB","title":"中国腐蚀与防护学报"},"keywords":[{"id":"6a8a56ef-f2dc-4dd8-a160-1ce6d99eea65","keyword":"1","originalKeyword":"1"},{"id":"8d5671dc-7ec5-4686-a5e8-9227d5ad3ce5","keyword":"4-butynediol","originalKeyword":"4-butynediol"},{"id":"7be0dd1c-cb16-4b34-95b8-83d902dc1030","keyword":"","originalKeyword":""},{"id":"52c54899-bb14-452d-beff-91a1a8f014ea","keyword":"epoxy coating","originalKeyword":"epoxy coating"},{"id":"9abc2ef2-3862-4ae1-bf55-e38d70f8c0fe","keyword":"Electrochemical method","originalKeyword":"Electrochemical method"}],"language":"zh","publisherId":"1005-4537_2006_6_11","title":"1,4-丁炔缓蚀剂在环氧涂层中的缓蚀机理研究","volume":"26","year":"2006"},{"abstractinfo":"1,4-丁炔(BYD)部分加氢生成1,4-丁烯(BED),BED进一步加氢生成1,4-(BDO).此外,BYD,BED和BDO还会发生脱水反应生成单醇类产物.工业上BYD加氢反应主要用于生产BDO.由于传统的单金属加氢催化剂很难控制反应的加氢程度,因此一般通过提高反应温度和压力使BYD尽量转化为完全加氢产物BDO,以减少部分加氢产物BED对最终产品收率的影响.部分加氢产物BED在精细化工领域也具有重要的应用,所以选择合适的催化剂和反应条件来提高部分加氢产物BED的选择性具有重要的理论意义和潜在应用价值.文献中常采用Zn、微生物等活性抑制剂来降低贵金属催化剂的加氢活性.这些方法往往比较复杂,所使用的添加剂不仅存在毒性和污染产物,还会增加成本.这些方法得到的催化材料虽然可以提高烯的选择性,但是仍需要严格控制反应条件才能得到较高收率的部分加氢产物.本文基于MOFs材料独特的结构和性质,探索了MOFs负载型贵金属催化剂在选择加氢反应中的催化性能.首先制备了一种羧酸根保护的Pt纳米溶胶,并以水为溶剂,增加2-甲基咪唑的加入量,实现了室温下ZIF-8晶体的快速生成.在室温合成ZIF-8的过程中加入羧酸根保护的Pt纳米溶胶,通过羧酸根与ZIF-8之间存在的化学吸附力,实现ZIF-8对Pt纳米粒子的包覆.羧酸根不仅可以稳定溶液中的纳米粒子,同时还起着“桥梁”的作用.羧酸根中的C=O基团与ZIF-8中的Zn原子或有机骨架之间弱的配位作用,增加了纳米粒子和ZIF-8之间的亲和力,实现了金属纳米粒子被ZIF-8包围.Pt纳米粒子的引入对ZIF-8的形成也没有影响,得到的Pt@ZIF-8材料拥有良好的晶体结构和高的比表面积.采用XRD、N2吸附和TEM等表征揭示了Pt@ZIF-8的结构特点,并研究了其在水相1,4-丁炔加氢反应中的催化性能.结果显示,该材料不仅具有很高的活性,还具有突出的部分加氢选择性.在5次循环反应中,BYD转化率没有明显变化,说明催化剂在反应过程中活性没有降低.在多次反应之后,反应产物的分布也没有发生明显变化,1,4-丁烯选择性在5次反应中都保持在94%以上.结构表征结果则显示,在4次循环使用之后,催化剂的结构已经遭到破坏;5次循环使用之后,催化剂的XRD谱图中ZIF-8的特征衍射峰完全消失.其余谱峰为ZnO特征衍射峰,说明由于反应温度较高,催化剂在多次反应之后其载体ZIF-8发生了分解.循环寿命实验说明,ZIF-8中Zn离子和含氮有机骨架的抑制作用是导致1,4-丁烯高选择性的重要原因.ZIF-8的分解虽然会使孔道塌陷,但是结构中的Zn和含氮的有机骨架组成依然存在,仍然可以达到抑制烯进一步加氢的效果,并且Pt纳米溶胶主要存在于外表面,所以催化剂的活性和选择性没有发生明显变化.","authors":[{"authorName":"李闯","id":"b74fb257-f193-4614-b863-909a06f48763","originalAuthorName":"李闯"},{"authorName":"张明明","id":"4527aff8-c062-449f-b31f-6309d9187d1d","originalAuthorName":"张明明"},{"authorName":"邸鑫","id":"377117b1-8eb0-4c10-9977-52eba40abaa5","originalAuthorName":"邸鑫"},{"authorName":"殷东东","id":"74bb2810-123b-45cf-b379-22fa2ced6035","originalAuthorName":"殷东东"},{"authorName":"李文震","id":"2f594c29-83bf-47e2-8fca-edec4ea29f18","originalAuthorName":"李文震"},{"authorName":"梁长海","id":"306dfc83-693a-4663-8ccf-8bd593de4616","originalAuthorName":"梁长海"}],"doi":"10.1016/S1872-2067(16)62497-X","fpage":"1555","id":"887fa0d4-696e-4d16-895d-863e9a9a3023","issue":"9","journal":{"abbrevTitle":"CHXB","coverImgSrc":"journal/img/cover/CHXB.jpg","id":"18","issnPpub":"0253-9837","publisherId":"CHXB","title":"催化学报 "},"keywords":[{"id":"e769bfa3-7f80-4fe8-bf29-ea62c383865e","keyword":"铂溶胶","originalKeyword":"铂溶胶"},{"id":"65270361-f415-4947-8ecc-ab732553506b","keyword":"ZIF-8","originalKeyword":"ZIF-8"},{"id":"3ba2f70c-d3cb-4471-84bd-96a273451a8c","keyword":"一步合成","originalKeyword":"一步合成"},{"id":"7c62cb27-3b94-43ee-a094-c7d89a88ff7f","keyword":"1,4-丁炔","originalKeyword":"1,4-丁炔二醇"},{"id":"6d2ab62d-fa22-4455-a8eb-8dbc80bf2a16","keyword":"选择加氢","originalKeyword":"选择加氢"}],"language":"zh","publisherId":"cuihuaxb201609016","title":"一步法合成Pt@ZIF-8及其在1,4-丁炔选择加氢中的应用","volume":"37","year":"2016"},{"abstractinfo":"用浸渍法混合负载制备了一种分子筛负载复合氧化物催化剂CuO/Bi2O3/ZSM-5,并探讨了催化剂的制备条件与反应条件对催化甲醛乙炔化生成1,4-丁炔反应的催化活性的影响.实验结果表明,CuO/Bi2O3/ZSM-5催化剂用于甲醛乙炔化反应的适宜的反应条件是:常压、363 K,催化剂用量为每50 mL甲醛溶液(初始浓度为37%)5 g催化剂,乙炔空速0.14~0.16 s-1,反应24 h.在此条件下,丁炔得率为89%~92%,选择性为96%左右,副产物丙炔得率约为2%.","authors":[{"authorName":"蔡锦","id":"3ca72a3c-0c95-4fbf-a2f0-2c7ec234a088","originalAuthorName":"蔡锦"},{"authorName":"张晓凤","id":"e54fb8e7-2334-4f8a-949e-654c7c5815b6","originalAuthorName":"张晓凤"},{"authorName":"黄秋锋","id":"7909083a-9fa8-4411-b345-ad0a6ce471dc","originalAuthorName":"黄秋锋"},{"authorName":"林深","id":"dfd8398e-9964-4fb9-b7a8-b9d533d392cb","originalAuthorName":"林深"}],"doi":"","fpage":"82","id":"cb068dee-5902-4598-969b-8bc2f89d9826","issue":"4","journal":{"abbrevTitle":"CLDB","coverImgSrc":"journal/img/cover/CLDB.jpg","id":"8","issnPpub":"1005-023X","publisherId":"CLDB","title":"材料导报"},"keywords":[{"id":"8d90bb9b-06c3-49c4-9f1e-99e07a7fcf93","keyword":"丁炔","originalKeyword":"丁炔二醇"},{"id":"e98d26e7-426b-4669-907f-6784f530fa6e","keyword":"复合氧化物","originalKeyword":"复合氧化物"},{"id":"c3d28f8a-05e4-4c71-a4c4-9223b26d4b06","keyword":"ZSM-5","originalKeyword":"ZSM-5"},{"id":"1e6e32fa-2b2b-4a39-8b64-792e9b87faef","keyword":"乙炔化","originalKeyword":"乙炔化"},{"id":"40df7c22-c4ea-44be-b827-6f15c958d8d2","keyword":"淤浆床","originalKeyword":"淤浆床"}],"language":"zh","publisherId":"cldb201304022","title":"淤浆床法合成丁炔的催化剂研究","volume":"27","year":"2013"},{"abstractinfo":"在碱性条件下,甲基甲氧甲酰环己烯酮( 1)与碘甲烷经烷基化反应生成甲基甲氧甲酰环己烯酮( 2),通过选择性还原酮羰基制得目标产物甲基甲氧甲酰环己烯( 3),反应的总收率约为60%. 研究了攫氢剂和还原剂对2步反应的影响,结果表明,烷基化反应和酮羰基选择性还原反应的最佳攫氢剂和还原剂分别是氢化钠和氢化三叔丁氧基铝锂,在者作用下所得烷基化产物和还原产物的收率分别为90%和67%. 合成产物的结构经元素分析、UV-Vis、1H NMR、IR和MS得到了表征.","authors":[{"authorName":"胡炳成","id":"9087d761-15d4-4f5c-99b2-3b045d4a9339","originalAuthorName":"胡炳成"},{"authorName":"吕春绪","id":"2c31a333-66fe-455b-b184-23c3fc25bb3e","originalAuthorName":"吕春绪"},{"authorName":"张才","id":"e93193f9-b029-4276-90ec-9eda0e534b43","originalAuthorName":"张才"}],"doi":"10.3969/j.issn.1000-0518.2006.05.018","fpage":"548","id":"0f66c102-c193-4b98-bfb4-51955d2bc0e5","issue":"5","journal":{"abbrevTitle":"YYHX","coverImgSrc":"journal/img/cover/YYHX.jpg","id":"73","issnPpub":"1000-0518","publisherId":"YYHX","title":"应用化学"},"keywords":[{"id":"72024791-4080-4591-8a89-e4a6446b6e81","keyword":"甲基甲氧甲酰环己烯","originalKeyword":"二甲基甲氧甲酰环己烯醇"},{"id":"057ad4e4-e8cf-4ae0-a54e-2efea42ea022","keyword":"甲基甲氧甲酰环己烯酮","originalKeyword":"甲基甲氧甲酰环己烯酮"},{"id":"0c8c407b-df1c-43d8-a984-7164e41434bb","keyword":"甲基甲氧甲酰环己烯酮","originalKeyword":"二甲基甲氧甲酰环己烯酮"},{"id":"6de63930-7b1a-4c73-a0a9-8d439320f0f0","keyword":"氢化钠","originalKeyword":"氢化钠"},{"id":"daec3ba2-c543-4256-b6e0-2df74e70d95e","keyword":"氢化三叔丁氧基铝锂","originalKeyword":"氢化三叔丁氧基铝锂"}],"language":"zh","publisherId":"yyhx200605018","title":"2,3-甲基-4-甲氧甲酰-2-环己烯的合成","volume":"23","year":"2006"},{"abstractinfo":"以基于季戊四代硅碳烷树状氯化物PCSi-2G-Cl为脚手架、4-硝基-4'-羟己氧基偶氮苯(M-NO2)为介晶基元, 合成了以季戊四为核、端基含36个硝基偶氮苯的新型硅碳烷液晶树状物PCSi-2G-NO2.利用红外光谱(IR)、核磁共振(1H NMR)、元素分析(EA)、偏光显微镜(POM)和差示扫描量热法(DSC)进行了表征,PCSi-2G-NO2显示近晶相, 其液晶相行为是K57SE76SA111I110SA75SE56K.而对应的介晶基元M-NO2则为向列相,树状物与修饰单元在熔点、清亮点和液晶态温度区间等方面也存在较大差异.","authors":[{"authorName":"唐新德","id":"c4fbddf3-67f4-4023-951a-010a832ea288","originalAuthorName":"唐新德"},{"authorName":"张其震","id":"bda846be-7f7e-400e-aba2-fa70a1b2fede","originalAuthorName":"张其震"},{"authorName":"范星河","id":"92829c5b-cd63-438f-9408-f4d827045702","originalAuthorName":"范星河"},{"authorName":"周其凤","id":"15f3c9f0-bfae-4536-a6e2-d42c838aea45","originalAuthorName":"周其凤"}],"doi":"","fpage":"1036","id":"0dba4b1c-688b-4b3e-885d-22e83613e8ac","issue":"7","journal":{"abbrevTitle":"GNCL","coverImgSrc":"journal/img/cover/GNCL.jpg","id":"33","issnPpub":"1001-9731","publisherId":"GNCL","title":"功能材料"},"keywords":[{"id":"b4b11488-3e31-4a61-933c-b562a682ac29","keyword":"硅碳烷液晶树状物","originalKeyword":"硅碳烷液晶树状物"},{"id":"301dad28-531f-4335-ac53-67e3697bf405","keyword":"季戊四","originalKeyword":"季戊四醇"},{"id":"3b21201e-cc14-4474-bf9d-fb1f9abc1689","keyword":"4-硝基偶氮苯","originalKeyword":"4-硝基偶氮苯"},{"id":"afc785d8-dfcb-418b-b43b-f98012a919a8","keyword":"代树状物","originalKeyword":"二代树状物"},{"id":"14212994-85d8-42df-9270-fbd367fc1d50","keyword":"介晶基元","originalKeyword":"介晶基元"}],"language":"zh","publisherId":"gncl200607006","title":"基于季戊四代硅碳烷液晶树状物研究——端基含36个4-硝基偶氮苯基团","volume":"37","year":"2006"}],"totalpage":6055,"totalrecord":60546}