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1.
微波辐照下无皂阳离子聚(St-MMA)高分子纳米粒子的制备和表征 总被引:10,自引:1,他引:10
讨论了微波辐照下 ,以丙酮 水为分散介质 ,利用阳离子型自由基引发剂偶氮二异丁基脒盐酸盐(AIBA)引发苯乙烯 (St)和甲基丙烯酸甲酯 (MMA)共聚 ,合成出表面带正电荷的P(St MMA)共聚物纳米粒子 ,考察了丙酮用量、单体和引发剂浓度对纳米粒子粒径、粒径分布和乳液稳定性的影响 .结果表明 ,丙酮 水的体积比由 0增加到 1 2 6∶1时 ,粒子的平均水化半径从 12 2 2 1nm降低到 2 4 6 8nm ,粒径分布变宽 ,乳液抗电解质稳定性逐渐增强 ;增加引发剂和共聚单体MMA的浓度 ,粒子的水化半径逐渐减小 ,粒径分散系数增大 . 相似文献
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超声辐照引发MMA微乳液聚合 总被引:17,自引:0,他引:17
研究了超声波引发甲基丙烯酸甲酯(MMA)的微乳液聚合.辐照40min时单体转化率高达90%.透射电镜观察发现,PMMA微乳液平均粒径为36.5nm,粒径分布窄,表明超声波引发是制备PMMA微乳液的有效方法.采用分光光度计对微乳液聚合过程中乳胶粒的形成和大小进行了间接表征,研究了超声功率输出、乳化剂、助乳化剂、单体和引发剂对MMA微乳液聚合的影响. 相似文献
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讨论了微波辐照下带正电荷的自由基引发剂偶氮二异丁基脒盐酸盐(AIBA)引发甲基丙烯酸甲酯(MMA)和甲基丙烯酸2-羟乙酯(HEMA)共聚,用透射电子显微镜、红外光谱仪、差热分析仪等对聚合产物进行表征.结果表明: 两种单体发生了共聚反应,制得均分散、表面洁净的无皂阳离子胶乳粒子;粒子的粒径随着单体HEMA浓度的增加先减小后增加.在微波辐照下共聚反应的速率非常快,几乎所有的反应在20 min之内就能完成.随着单体HEMA浓度的增加,乳液抗电解质稳定性提高. 相似文献
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研究了丙烯酸-β-羟丙酯存在下高浓度苯乙烯的无皂乳液聚合.[St]、[β-HPA]、[KPS]分别为2.66、0.228和5.8×10~(-3)mol/L,80℃反应5h,单体转化率可达90%;经TEM分析,求出了胶乳粒径D=0.23μm,粒子浓度N=3.13×10~(13)粒/cm~3,且胶乳粒径具有单分散性;并讨论了影响乳液稳定性的因素.经IR光谱和溶解性试验证实β-HPA参与了St共聚,推测了自交联机理;求出了聚合反应表观活化能(78.7kJ/mol)和80℃时的聚合反应速率常数(514.3L/mol·s). 相似文献
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高浓度窄分布无皂高分子纳米粒子胶乳的制备 总被引:17,自引:0,他引:17
在微波辐照和丙酮存在下,进行了苯乙烯(ST)和甲基丙烯酸甲酯(MMA)的无皂乳液聚合.当丙酮的含量在50%以下时,可以得到稳定的窄分布的纳米粒子胶乳.丙酮的含量由0增加到50%,粒子的平均水化半径由278nm降低到35.4nm.在一定的浓度范围内,固定引发剂过硫酸钾(KPS)的用量,则粒子的平均水化半径与单体的浓度成正比;当单体浓度一定时,随着引发剂浓度的增加,粒子平均水化半径从25nm减少到22nm然后又增大.考虑到引发剂既是粒子表面电荷的来源,又增加了体系的离子强度,在粒子形成过程中,起着稳定和絮凝的双重作用,我们得到了一个简单的公式用以描述粒子的平均水化半径<R 相似文献
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MMA—St无皂乳液聚合成核机理探讨 总被引:5,自引:0,他引:5
讨论了MMA-St无皂乳液聚合,当[KPS]=2.77×10~(-3)mol/L,[MMA]0.51mol/L,[St]=0.49mol/L,70℃反应5.0小时,能得到较高的聚合转化率,较小的胶乳粒径和较大的粒子浓度,并对不同反应时期聚合物的分子量及其分布进行了测定,认为该无皂乳液聚合体系为均相沉淀成核机理。当转化率大于30.9%时,胶乳粒的凝聚程度大于胶乳粒的生成速度。KPS分解产生的自由基起到了稳定乳液的作用。 相似文献
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在微波辐照下,以过硫酸钾(KPS)为引发剂,丙酮水溶液(质量比1∶ 1)为分散介质,进行了苯乙烯(ST)和其它共聚单体:甲基丙烯酸甲酯(MMA)、甲基丙烯酸丁酯(BMA)、丙烯酸乙酯(EA)及顺丁烯二酸酐(BDA)的无皂乳液聚合,得到了稳定的纳米胶乳粒子.讨论了共聚单体的种类和浓度对粒子水化半径的影响.增加配方中亲水性单体含量,使引发反应中引发剂的消耗量增加,粒子表面电荷密度增大,同时亲水性增加,油水界面张力减小,粒子变得稳定,有利于小粒子的生成.粒子的大小随亲水性单体的含量呈曲线关系,曲线上有最低点. 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献