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1.
用Grignard试剂C6H5MgBr合成苯甲醛   总被引:1,自引:0,他引:1  
苯甲醛广泛用于医药、农药、染料、香料等行业[1] 。为了寻找产率高、成本低的新合成方法 ,人们进行了广泛的研究[1 7] 。本文用Grignard试剂与苯并咪唑盐[8] 合成苯甲醛。合成路线如下 :1 实验部分XT 2型数字显微熔点仪 (温度计未经校正 ) :PE 2 40 0CHN元素分析仪 ;VarianINOVA 40 0核磁共振仪 ;试剂均为化学纯。参考文献 [9]合成Grignard试剂C6 H5MgBr,以四氢呋喃作溶剂。1 1 苯并咪唑的合成在 1 0 0ml圆底烧瓶中加入 1 0 8g(0 1mol)邻苯二胺和 8ml(0 2mol) 90 %甲酸 ,90℃下…  相似文献   

2.
苯并咪唑衍生物具有一定的抗病毒能力[1 ] ,一些苯并咪唑衍生物已用作农用抗植物病毒剂[2 ] 。一锅煮合成反应时间较长 ,产率中等[3,4] 。本文用取代邻苯二胺和水杨酸为原料 ,吡啶为溶剂 ,POCl3为催化剂 ,微波辐射法合成了标题化合物。合成路线如下 :1 实验部分1 1 仪器WC 1型熔点测定仪 (温度计未校正 ) ;日本岛津IR 435红外光谱仪 (KBr压片 ) ;TEOL FX90Q核磁共振仪 ,DMSO d6 为溶剂 ;日本柳公C·H·N元素分析仪MT 3;苏州三星电子有限公司产新天地M9K88型微波炉 ,输出功率 85 0W ,2 4 5 0Hz。1 2 …  相似文献   

3.
复合固体超强酸SO_4~(2-)/TiO_2-Fe_2O_3催化合成丁酸异丁酯   总被引:3,自引:0,他引:3  
采用溶胶 凝胶法制备的复合固体超强酸催化剂SO2-果表明物质的量比n(Ti)∶n(Fe)=2∶1时催化剂活性最高,这与文献结果[2]有所不同。1 实验部分1 1 试剂和仪器丁酸、异丁醇、苯、表面活性剂(PEG-600)、乙醇、三氯化铁等为分析纯;钛酸四丁酯为化学纯。上海产WZS-1型阿贝折射仪;日本岛津GC-16A气相色谱仪;GEMINI2360型氮气吸附全自动表面分析仪。1 2 催化剂SO2-4/TiO2-Fe2O3的制备、酸强度及BET表面积测定  取一定量的钛酸四丁酯剧烈搅拌下缓慢滴加到80ml无水乙醇中,搅拌20min,快速加入80ml2…  相似文献   

4.
TiSiW12O40/TiO2催化合成丙酸异戊酯   总被引:15,自引:0,他引:15  
丙酸异戊酯是一种具有菠萝或洋梨果香味的无色液体 ,可作食用香料及多种工业溶剂。传统工业采用浓硫酸催化丙酸和异戊醇合成丙酸异戊酯[1 ,2 ] ,但原料利用率及产率较低 ,环境污染严重。近年来 ,有关杂多酸及其盐类的催化作用的研究发展迅速[3~ 7] 。我们合成了杂多酸盐TiSiW1 2 O40 /TiO2 催化剂 ,研究其对丙酸异戊酯的催化合成反应 ,取得了较为满意的结果。1 实验1 1 仪器试剂PKW 型电子节能控温仪 ;Abbe折光仪 ;IMP41 0红外光谱仪 (KBr压片 ,40 0~2 0 0 0cm- 1 ) ;D/MAX ⅢC自动X射线衍射仪 (Cu靶 …  相似文献   

5.
三氮烯试剂与第IB、IIB族金属元素有高灵敏的显色反应 1 [1] ,可用来测定样品中微量的Cd2 + 、Hg2 + 、Zn2 + 、Ni2 + 。随着表面活性剂引入该显色体系 ,使该试剂与金属离子显色反应的灵敏度有了很大的提高。目前报道的三氮烯显色剂与Hg2 + 显色反应的灵敏度一般在ε =1 .0× 1 0 5L·mol-1·cm-1左右 ,但也有部分试剂的灵敏度较高 ,如OC Cadion[2 ] 的ε =1 .77× 1 0 5L·mol-1·cm-1,DNAAB[3 ] ε=1 .74× 1 0 5L·mol-1·cm-1,MDAA[4]的ε=1 .8× 1 0 5L·mol-1·cm-1,APD…  相似文献   

6.
羟基磷灰石合成工艺研究   总被引:1,自引:0,他引:1  
羟基磷灰石 [Ca10 (PO4 ) 6(OH) 2 ,简称HAP]是80年代发展起来的新型牙科、骨科材料 ,其成份接近生物体骨质的无机成份 ,能诱发新骨生长 ,具有良好的生物相容性。HAP的制备方法较多 ,有溶胶 凝胶法[1,2 ] 、沉淀法、电化学合成法[3 ,4 ] 等。1 实验1 1 试剂与仪器所用试剂除磷酸三丁酯为化学纯外 ,其它都是分析纯。美国尼高力公司 (NICOLET)傅里叶变换红外光谱仪 (MAGNA 5 5 0 (Ⅱ ) )。1 2 HAP的制备1 2 1 溶胶 凝胶法合成HAP 我们以不同原料制备了HAP。第一种方法是以Ca(NO3)2 与磷酸三丁…  相似文献   

7.
FERROMAGNETICALLY COUPLED BINUCLEAR Fe(Ⅲ) COMPLEXES THROUGH ISOPHTHALATO-BRIDGEFERROMAGNETICALLYCOUPLEDBINUCLEARFe(Ⅲ)COMPLEXE...  相似文献   

8.
PdSAPO-5分子筛在甲醇转化反应中的催化性能及机理   总被引:1,自引:0,他引:1  
用连续-脉冲激反应色谱评价了不同SAPO-5分子筛及一步法合成的PdSAPO-5催化剂对甲醇制烯烃(MTO)反应的催化性能,用TPD-MS及13CCPMASNMR研究了其催化反应机理.结果表明,PdSAPO-5比SAPO-5和Pd/SAPO-5有更高的烯烃选择性,这是由于反应物凝胶中加入的钯对分子筛的酸性具有调节作用,加入不同形式的钯源,其调节作用有较大的差别,并使分子筛上甲醇及生成的二甲醇的脱附温度不同.此外,钯还充当了脱氢中心,可从二甲基已基氧离子中脱下一个氢原子,从而有利于乙烯的生成.NMR结果表明,此类催化剂上的结炭存在多种形式.反应生成乙烯的甲氧基离子主要是二甲基乙基氧离子;甲醇在此类催化剂的部分钯粒子上脱氢生成CH2O.  相似文献   

9.
GRAFTCOPOLYMERIZATIONOFBUTYLACRYLATEONTOCASEININITIABYPOTASSIUMDIPERIODATOARGENTATE¥WeiHongLIU;YiugHatLIU;YaJuanSHANG,MingJun...  相似文献   

10.
THE SUPPORTED GOLD CATALYST FOR REMOVING CARBON MONOXIDE AT AMBIENT TEMPERATURETHESUPPORTEDGOLDCATALYSTFORREMOVINGCARBONMONOX...  相似文献   

11.
We introduce well-defined nanopillar arrays of a poly(ethylene glycol) (PEG) hydrogel as a cell culture platform to guide a 3D construct of primary rat cardiomyocytes in vitro for potential tissue engineering applications. Ultraviolet (UV)-assisted capillary lithography was used to fabricate highly uniform approximately 150 nm PEG pillars with approximately 400 nm height. It was found that cell adhesion was significantly enhanced on PEG nanopillars (132 +/- 29 cells/mm2) compared to that on the bare PEG control (39 +/- 17 cells/mm2) (p < 0.05) but substantially reduced compared to that on the glass control (502 +/- 45 cells/mm2) (p < 0.01). Furthermore, in colonizing cardiomyocytes, the nanopillars stimulated self-assembled aggregates among the contacting cells with 3D growth, which is a unique feature for nanopatterned PEG hydrogels as a cell culture substrate. The 3D-grown cardiomyocytes retained their conductive and contractile properties, as evidenced by the observation of beating cardiomyocytes with robust action potential generation.  相似文献   

12.
Separation of endo-polygalacturonase using aqueous two-phase partitioning   总被引:2,自引:0,他引:2  
The partitioning of endo-polygalacturonase (endo-PG) in polyethylene glycol (PEG)-polyvinyl alcohol (PVA10000) and PEG-hydroxypropyl starch (Reppal PES100) aqueous two-phase systems was studied, and revealed the possibility of using aqueous two-phase extraction to purify and concentrate endo-PG from its clarified fermentation broth. For the PEG8000-PVA10000 system, endo-PG presented in the fermentation broth (at concentration that is more than 40% of total protein) mainly dominates in the top phase with a partitioning coefficient of 6, while total protein concentrates in the bottom phase. A separation scheme consisting of two consecutive aqueous two-phase extraction steps was proposed: a first extraction in polyethylene glycol (PEG8000)-polyvinyl alcohol system, followed by a second extraction in PEG8000-(NH4)2SO4 system. This allowed the separation of endo-PG from polymer and the recycling of PEG polymer, since endo-PG was very strongly partitioned into the bottom phase of the PEG8000-(NH4)2SO4 system. Laboratory-scale experiments were performed to test the efficiency of this scheme. It was found that enzyme recovery was up to 91% with a total purification factor of about 1.9 and a concentration factor of more than 5. About 90% of the total PEG added into the systems can be recovered, and no reduction was obtained in the purification factor using recycled PEG.  相似文献   

13.
Summary: Poly(ethylene glycol) (PEG) networks were synthesized by γ‐irradiation. The crystalline behavior of PEG was investigated by differential scanning calorimetry (DSC) and wide‐angle X‐ray diffraction (WAXD). It was shown that the crystallinity of PEG is dramatically lower in the cross‐linked networks than in pure PEG. When the molecular weight of PEG in the networks decreased to 1 000, it could not crystallize at all. Moreover, we also found that the melting temperature of PEG is greatly affected by the presence of a cross‐linked network.

The DSC curves of PEG ( = 1 500) and the corresponding cross‐linked PEG.  相似文献   


14.
Nanoporous alumina surfaces have a variety of applications in biosensors, biofiltration, and targeted drug delivery. However, the fabrication route to create these nanopores in alumina results in surface defects in the crystal lattice. This results in inherent charge on the porous surface causing biofouling, that is, nonspecific adsorption of biomolecules. Poly(ethylene glycol) (PEG) is known to form biocompatible nonfouling films on silicon surfaces. However, its application to alumina surfaces is very limited and has not been well investigated. In this study, we have covalently attached PEG to nanoporous alumina surfaces to improve their nonfouling properties. A PEG-silane coupling technique was used to modify the surface. Different concentrations of PEG for different immobilization times were used to form PEG films of various grafting densities. X-ray photoelectron spectroscopy (XPS) was used to verify the presence of PEG moieties on the alumina surface. High-resolution C1s spectra show that with an increase in concentration and immobilization time, the grafting density of PEG also increases. Further, a standard overlayer model was used to calculate the thickness of PEG films formed using the XPS intensities of the Al2p peaks. The films formed by this technique are less than 2.5 nm thick, suggesting that such films will not clog the pores which are in the range of 70-80 nm.  相似文献   

15.
吴缨  范崇政  司靖宇 《应用化学》2005,22(11):1253-0
纳米TiO2光催化降解聚乙二醇反应;纳米二氧化钛; 光催化; 聚乙二醇  相似文献   

16.
The adsorption of poly(ethylene glycol) (PEG) and ammonium poly(methacrylate) (APMA) onto alumina has been examined both individually and in combination. The adsorption density of APMA was found to be higher than that of PEG onto alumina. The adsorption isotherms of PEG and APMA for alumina exhibited a Langmuirian behavior. The adsorption density of PEG was significantly reduced in the presence of APMA, but the reverse was not true. About 60% desorption of PEG from alumina was achieved, while in the case of APMA the amount desorbed was only 10% in the pH range of 3-6. The zeta potential values of alumina were decreased and the isoelectric point (i.e.p.) values were shifted toward acidic pH values, proportional to the concentration of APMA added. However, such changes in the electrokinetic behavior were not observed by the addition of PEG. The dispersion behavior of alumina in the combined presence of PEG and APMA essentially followed the trends obtained for the alumina-APMA system, corroborating the electrokinetic measurements. Coprecipitation tests confirmed complexation between aluminum species and APMA in the bulk solution, but not with PEG. The interaction between alumina and PEG is primarily governed by hydrogen-bonding forces, while both hydrogen bonding and chemical interaction are involved in the case of the alumina-APMA system. FTIR spectroscopic studies provided evidence in support of the interaction mechanisms proposed.  相似文献   

17.
Summary: The gelation rate of a poly(ethylene glycol)‐grafted hyaluronic acid (PEG‐graft‐HA) solution with adding α‐CD was investigated in term of the microphase separation between the grafted PEG and HA. The gelation rate of PEG‐graft‐HA exhibiting the microphase‐separated structure was two times higher than that of PEG‐graft‐HA showing a homogeneous miscible state.

The formation of microphases by PEG‐graft‐HA contributes to its rapid gelation upon the addition of α‐CDs.  相似文献   


18.
19.
The solubility of naphthalene was investigated in aqueous solutions of triblock copolymers poly(ethylene glycol)–poly(propylene glycol)–poly(ethylene glycol) (PEG–PPG–PEG) and (2-hydroxypropyl)cyclodextrins. The results with solutions of the individual solubilizers were as expected: the solubility enhancement was much higher with a micelle-forming copolymer than with the non-micellizing one and with (2-hydroxypropyl)--cyclodextrin (HPBCD) than with (2-hydroxypropyl)--cyclodextrin (HPACD). Although the formation of inclusion complexes between HPACD and PEG and between HPBCD and PPG is well established, the naphthalene solubility in mixed solutions does not significantly deviate from that predicted for a mixture of independent solubilizers. Thus the interactions between HPCD and PEG–PPG–PEG copolymers are not strong enough to disrupt micelles and aggregates formed by those copolymers. In fact, slight synergetic deviations were observed with the micellizing copolymer, indicating the existence of ternary naphthalene/HPCD/copolymer interactions. For pharmaceutical applications, it is important that the solubilization efficacy of PEG–PPG–PEG copolymers and that of cyclodextrins modified by the 2-hydroxypropyl group would not be compromised if these two types of solubilizers were co-administered.  相似文献   

20.
JPC – Journal of Planar Chromatography – Modern TLC - A simple, rapid, and effective method for TLC separation of two EU-authorized UV filters octyl methoxycinnamate (OMC) and...  相似文献   

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