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1.
制备参数对ZrO2气凝胶超细粉织构和结构性质的影响 Ⅰ.水凝胶pH值 总被引:5,自引:4,他引:5
用超临界流体干燥(SCFD)法制备出大孔高比表面ZrO2气凝胶超细粉,详细考察了初始水凝胶pH值对ZrO2超细粉形貌、晶相组成、颗粒大小与分布、比表面积及孔结构等织构和结构性质的影响。在实验范围内,当水凝胶pH值为10.30时,所制得的ZrO2超细粉具有最大的比表面积和孔体积,最小的表观堆密度和平均粒径,颗粒分布均匀狭窄,颗粒间连接成三维网络构状态,较好地保持了凝胶原始织构。 相似文献
2.
表层二氧化锆/硅基-CDMPC手性固定相的制备及联苯双酯类保肝药的直接拆分 总被引:1,自引:0,他引:1
用分子自组装的方法制备了表层纳米氧化锆包覆多孔微米硅球,得到的氧化锆 /硅胶微球用作高效液相色谱担体,本方法制备的担体具有氧化锆的表面特性并保 持了硅胶的颗粒均匀、表面积大、渗透性好的优点,可以制备大涂敷量的手性固定 相,以增加固定相的手性识别能力,以涂敷量为20%的纤维素-三(3,5-二甲基苯 基氨基甲酸酯)-氧化锆/硅胶手性固定相(CDMPC-coated ZrO_2/SiO_2)上,对 联苯双酯类保肝药物进行直接拆分,考察了流动相极性、第二种极性改性剂对样品 保留和拆分的影响;并对手性拆分机理进行了阐述,结果表明:CDMPC- ZrO_2/SiO_2手性固定相比CDMPC-ZrO_2具有更好的手性拆分能力。 相似文献
3.
不同干燥过程对超细TiO2粉体性质的影响 总被引:12,自引:0,他引:12
考察了采用不同干燥工艺制备的TiO2粉体在粒子形貌、颗粒大小与分布、晶相组成以及比表面积和孔结构等织构和结构性质方面的差异。结果表明,利用常规的干燥方法,由水凝胶脱水所得的颗粒,颗粒间严重团聚,颗粒粒径大且分布不均匀,比表面积和孔体积最小;由醇凝胶直接脱水,则可以显著提高粉体的织构性能.而采用超临界流体干燥法则可以进一步提高粉体的性能,比表面积由水凝胶的4.88m2·g-1增大到113.8m2·g-1,提高了近30倍;孔体积由0.027cm3·g-1增大到0.41cm3·g-1.大约提高了15倍;而且其能够有效地防止粒子间的团聚,较好地保持了湿凝胶的网络结构,使颗粒尺寸降低且分布均匀,可重复性好. 相似文献
4.
由高碳醇制备O/W微小乳状液 总被引:1,自引:0,他引:1
中碳醇与高浓度的离子型表面活性剂(15%~30%)混合可制备O/W型微乳,分散质点为0.01~0.1μm。以高碳醇与低浓度离子型表面活性剂(0.6%~3%)为混合乳化剂,可制得内相体积为25%的苯乙烯在水中的微小乳状液(miniemulsion)粒子大小为0.1~0.4μm,与普通乳状液相比,具有颗粒小、分散均匀、稳定性高的特点。本文研究季胺盐等离子型表面活性剂与高碳醇混合乳化剂体系中制备微小乳状液的条件及其稳定机制。 相似文献
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颗粒乳化剂的研究及应用 总被引:2,自引:0,他引:2
近年来,颗粒乳化剂因其在食品、采油、化妆品、医药、催化以及功能纳米材料制备等领域具有潜在应用前景而备受关注。本文综述了近来颗粒乳化剂的研究进展,归纳了颗粒乳化剂的种类,包括:无机纳米粒子、表面改性或杂化的无机粒子、有机纳米粒子以及特殊的颗粒乳化剂Janus粒子;并对颗粒乳化剂能够在油水界面稳定吸附的热力学机理和动力学行为进行了阐述,颗粒乳化剂在油水界面接触角以及粒径大小是其在界面稳定吸附的关键参数,而颗粒在油水界面的排布方式则主要受粒子之间相互作用的影响。重点介绍了颗粒乳化剂的热点应用,包括:(1)利用颗粒乳化剂制备Pickering乳液,以及通过对颗粒乳化剂的功能化,使得Pickering乳液具备环境响应性(即pH、盐浓度、温度、紫外光、磁场敏感响应性);(2)以颗粒乳化剂为构筑基元、以Pickering乳液为模板制备Janus颗粒、Colloidosome、具有多级结构的粒子或膜,以及多孔结构材料;(3) Janus粒子在催化领域的应用。 相似文献
6.
在水/环己烷微乳体系中制备纳米级氧化锆微粒 总被引:15,自引:0,他引:15
研究了在水 环己烷 正己醇 Triton X 100的微乳体系中, 几种主要实验参数对由氯氧化锆制备氧化锆纳米粒子的比表面积及其颗粒大小的影响.实验结果表明,微乳体系中水与表面活性剂的摩尔比ro、氯氧化锆的浓度以及微乳沉淀反应的温度都对氧化锆的比表面积有很大影响.在不同温度的微乳体系,氯氧化锆浓度对最终氧化锆粒子的比表面积的影响不同.通过优化制备条件,制得了比表面积为212 m2•g-1(450 ℃焙烧后)的氧化锆纳米粉体.文中还对所制备的氧化锆样品进行了X射线衍射(XRD)、透射电镜(TEM)和氮气吸附的分析. 相似文献
7.
乳状液按其颗粒大小可分为普通乳状液(约IN10pm,微小乳状液(01~0·4Pm),微乳状液(001卜0.lPm).其中微小乳状液比普通乳状液颗粒小,分散均匀,稳定性好,比微乳状液所需乳化剂的用量要低得多,在实际应用中很有前景.但有关微小乳状液的研究工作做得很少[’-‘].在乳化过程中,若不需外界做功,靠乳化剂的自身作用,使两种不相混溶的液体自动混合,生成乳状液称为自发乳化,无需专门的乳化设备即可方便地制备出乳状液.目前自发乳化所得的乳状液颗粒都较大,稳定性较差卜一\若将微JJ、乳状液的制备与其自发形成的条件结合… 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
12.
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
13.
Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
14.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
15.
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
16.
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
17.
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
18.
N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
19.
Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
20.
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