2—皮考胺树脂的合成及对金和铂族离子的吸附性

前文已报道了一些含杂环功能基树脂对贵金属离子的吸附性。本文按下列反应式合成了大孔型2-皮考胺树脂(2-picolyl amine resin):     

A Facile One-pot Method for the Synthesis of Vinyl Ethers from 2-Hydroxyalkyl Phenyl Selenides

chloride instead of primary or secondary organic halide, only 21% isolated yield of 1-tert-butoxy-1-phenylethene was obtained. Obviously, t-butyl chloride would tend to mainly take place the elimination reaction rather than the substitution reaction under sodium alkylate. Scheme 1 R1OHPhSe R2R3CHX 2NaH/THFR1OPhSeCHR2R3R1 OCHR2R3H2O21 3 4 Table 1 Preparation of vinyl ethers from 2-hydroxyalkyl phenyl selenides Entry R1 R2R3X Product a Yield (%) b 1 C6H5 CH2=CHCH2Br 4a 83 …     

锂离子电池高电压正极材料LiNiVO4的合成与表征

通过流变相反应法成功合成了LiNiVO4．利用热重-差热分析、粉末X射线衍射、扫描电子显微镜和粒度分析对产物进行了表征;采用循环伏安技术评价了其电化学性能．结果表明,利用流变相反应法在500℃即可制备纯相的LiNiVO4产物．与常规的固相反应产物相比,流变相产物表现出了较小的晶胞常数和颗粒尺寸,其中600℃的流变相产物具有良好的循环伏安特性．     

2-烷硫基-5-苯基亚甲基-4H-咪唑啉-4-酮的合成与表征

用2-硫代-3-正丁基-5-苯基亚甲基4-咪唑啉二酮的-S-烷基化反应合成了2-烷硫基-3-正丁基-5-苯基亚甲基-4H-咪唑啉-4-酮衍生物。探讨了S-烷基化反应的反应条件和所合成化合物的波谱性质。目标产物均为新的化合物，其结构经元素分析，IR，1H NMR和MS确正。     

新型锂离子电池正极材料LiVOPO4的制备与表征

Novel lithium-ion battery cathode material LiVOPO₄ was synthesized by sol-gel method using lithium hydroxide, ammonium metavanadate, phosphoric acid and citric acid as raw materials. The microstructure, surface morphology and electrochemical properties were characterized by various electrochemical methods in combination with thermogravimertric (TG) analysis and differential thermal analysis (DTA), X-ray diffraction (XRD), infrared (IR) spectroscopy, scanning electron microscope (SEM). Results show that the sample obtained by calcinating at 650 ℃ for 6 h is made up of uniform particles with size of 2～3 μm. The first discharge, charge capacity and columbic efficiency of LiVOPO₄ is 137.1 mAh·g^-1, 146.1 mAh·g^-1 and 93.8%, respectively. After 80 cycles the discharge capacity is kept at 130.4 mAh·g^-1, which is 95.1% of the first discharge capacity, and the capacity loss per cycle was only 0.061%, suggesting the LiVOPO₄ derived by this method is a promising cathode material for lithium ion batteries.     

Synthesis and Characterization of a Novel Copoly(aryl ether ketone) Containing 4, 4''''-Biphenyl-bis[4-phthalazin-1(2H)-one] Moiety

Poly(aryl ether ketone)s are a category of high performance engineering thermoplastics characterized by high glass transition temperature and excellent thermooxidative stability. And they have important applications in electronic, electric, aircraft and aerospace industries1~3. Considerable efforts have been made towards the improvement of solubility or processability of poly(aryl ether ketone)s4,5. In our work, a novel bis(phthalazinone) monomer 1 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] …     

New Method for the Synthesis of Benzyl Alkyl Ethers Mediated by FeSO4

The synthesis of benzyl alkyl ethers from benzyl bromides and alcohols using FeSO₄ as a recoverable and reusable mediator has been described without use of base and cosolvent under mild conditions.     

苯甲酸(苯并三唑基)苯酯类紫外光稳定剂的合成及表征

以邻硝基苯胺和间苯二酚为原料,经重氮化-偶合、环化、酯化合成了6个新型苯甲酸(苯并三唑基)苯酯类化合物:3-羟基-4-苯并三唑基-4′-硝基苯甲酸苯酯(58.6%)、3-羟基-4-苯并三唑基-2′-硝基苯甲酸苯酯(60.7%)、3-羟基-4-苯并三唑基-3′-硝基苯甲酸苯酯(55.7%)、3-羟基-4-苯并三唑基-3′,5′-二硝基苯甲酸苯酯(62.1%)、3-羟基-4-苯并三唑基-2′-羟基苯甲酸苯酯(48.6%)和3-羟基-4-苯并三唑基-2′-羟基-3′,5′-二硝基苯甲酸苯酯(52.2%)。通过1H-NMR、FT-IR和MS确定了这些化合物的分子结构,紫外光谱测试表明它们均具有较好的紫外吸收性能。     

Synthesis and Characterization of New Thiazolidin-4-one Derivatives

The synthesis of some new functionalized thiazolidin-4-one derivatives has been described. The N-substituted-thiosemicarbazides 3a-3i were obtained though the reaction of alkylamines 2a–2i , carbon disulfide, and hydrazine hydrate. The condensation reaction between 3a–3i and 4-amino-2-methanesulfanylpyrimidine-5-carboxaldehyde 1 afforded the thiosemicarbazones 4a–4i . The corresponding thiazolidin-4-ones 5a–5i were prepared by cyclization of 4a–4i with ethyl bromoacetate. The structures of the final products were confirmed by IR, ¹ H NMR, ¹³ C NMR, and HRMS.     

LaPO4纳米微粒的制备及表征

Surface-modified LaPO4 nanoparticales were synthesized in the mixture solvent of water-ethanol with the surface modification age of dialkylphosphate. The conditions of synthesis and characterization were discussed. The results indicated that nanoparticle core of LaPO4 and surface-modified layer were formed. The surface-modified nanoparticles of LaPO4 can be dispersed in organic solvent and has better lubricating properties.     

Synthesis and Characterization of a Novel Zeolite CJS-4

A novel zeolite, denoted as CJS-4, has been synthesized from nonalkaline medium by using 4,4'-trimethylenebis(1-methylpiperidine) or 1,4-diazoniabicyclo(2,2,2) octane as template agent, respectively. The precursors were characterized by means of powder X-ray diffraction, scanning electron microscopy, thermal analysis, gas adsorption and high resolution solid state NMR of 13C and 29Si.     

新试剂二溴对硝基苯基重氮氨基-4-苯基-2-噻唑的合成及其与钯显色反应的研究

报道了新试剂二溴对硝基苯基重氮氨基－４－苯基－２－噻唑的合成方法，并研究了在表面活性剂ＣＰＣ存在下，该试剂与钯（Ⅱ）的显色反应。结果表明，在ｐＨ６．４～７．８范围内，钯（Ⅱ）与该试剂可形成１∶２灰紫色的配合物，其最大吸收波长位于６５０ｎｍ，表观摩尔吸光系数为７．０２×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，钯量在０～２２μｇ／２５ｍＬ范围内符合比尔定律，该方法已用于Ｐｄ－Ｃ催化剂中微量钯的测定，结果满意。     

棒状LiZnPO4的低温合成与表征

LiZnPO₄的性能与其形貌密切相关,其合成常用的固相法和水热法均无控制其微观形貌的优势。 本文采用改进的沉淀法成功合成了具有棒状结构的LiZnPO₄。 利用热重-差热分析仪(TG-DSC)、X射线衍射仪(XRD)、傅里叶变换红外光谱(FTIR)以及场发射扫描电子显微镜(FE-SEM)等技术研究了LiZnPO₄形成过程、晶相组成、微观结构和形貌。 同时探究了合成方法、煅烧温度、煅烧时间、酸的种类对LiZnPO₄形貌的影响。 结果表明,相比较于固相法,以醋酸为原料的改进沉淀法不仅可以有效降低LiZnPO₄的合成温度至500 ℃,而且很容易控制棒状LiZnPO₄的形成。 在600 ℃下煅烧2 h后可以获得分散性良好、横截面为矩形、直径约为2 μm的规则棒状LiZnPO₄。 此外,对比颗粒状LiZnPO₄和棒状LiZnPO₄的光响应能力,发现棒状LiZnPO₄的光响应能力明显增强。     

1-苯基-3-甲基-4-苯甲酰基-5-吡唑啉酮(HPMBP)缩甘氨酸甲酯的合成、表征和晶体结构

合成了化合物1-苯基-3-甲基-4-苯甲酰基-5-吡唑啉酮(HPMBP)缩甘氨酸甲酯,用红外光谱、核磁共振谱和元素分析等方法进行了表征,用X射线衍射方法测定了其晶体结构.晶体学参数如下:三斜晶系,空间群为P1, a=0.9403(3) nm, b=0.9884(3) nm, c=1.0127(3) nm, α=86.666(7)°, β=89.827(6)°, γ=73.951(6)°, V=0.9029(5) nm3, Z=2, Dc=1.285 Mg·m-3, μ=0.088 mm-1, F(000)=368.最终偏离因子R1=0.0452, wR2=0.0889.     

单斜BiV04的离子液体辅助水热合成及表征

在离子液体[BMIM]Br辅助的水热条件下,合成了斜钒铋矿(Clinobisvanite,m-BiVO4)片状多面体微米晶.采用XRD,XPS,IR和SEM等对产物物相、结构和形貌进行了表征.结果表明,m-BiVO4产物为单斜晶系,I2/b空间群,片状多面体长宽为8～12 m,厚度为2-5 μm,晶型较完整,且具有良好...     

纳米级LiFePO_4材料的水热模板法合成及其性能研究

采用水热模板法合成纳米级LiFePO4材料,改变水热反应中表面活性剂(十六烷基三甲基溴化铵)的比例控制样品颗粒生成的大小.SEM测试表明,合成的LiFePO4晶粒尺寸与表面活性剂的配比密切相关,范围在几十到几百nm之间.充放电试验表明,合成的纳米级LiFePO4材料电极具有优良的电化学性能,其0.1C放电最高比容量可达150 mAh/g,而1C和2C放电比容量也分别有140 mAh/g和126 mAh/g.     

Synthesis and Characterization of New Soluble Polyamides from 9,9-Bis[4-(chloroformylphenoxy)phenyl]xanthene and Various Aromatic Diamines

9,9‐Bis(4‐hydroxyphenyl)xanthene (BHPX) was synthesized in 82% yield from xanthenone in a one‐pot, two‐step synthetic procedure. A new diacyl chloride monomer, 9,9‐bis[4‐(chloroformylphenoxy)phenyl]xanthene (BCPX), was synthesized in three steps from the nucleophilic fluorodisplacement of 4‐fluorobenzonitrile with the dipotassium bisphenolate of BHPX, followed by alkaline hydrolysis of the intermediate bis(ether nitrile), and then chlorination with thionyl chloride. Several novel aromatic polyamides containing ether and bulky xanthene groups with the inherent viscosities (0.72–0.98 dL/g) were prepared by the low temperature polycondensation of BCPX with various aromatic diamines in N,N‐dimethylacetamide (DMAc) solution containing pyridine (Py). All new polyamides were amorphous and readily soluble in various polar solvents such as DMAc, N,N‐dimethylformamide (DMF), N‐methyl‐2‐pyrrolidone (NMP) and Py. These polymers showed relatively high glass transition temperatures between 236 and 298°C, decomposition temperatures at 10% weight loss ranging from 490 to 535°C and 483 to 515°C in nitrogen and air, respectively, and char yields at 700°C in nitrogen higher than 50%. Transparent, flexible, and tough films of these polymers cast from DMAc solutions exhibited tensile strengths ranging from 82 to 106 MPa, elongations at break from 10% to 25%, and initial moduli from 2.0 to 2.8 GPa.     

Li3PO4包覆LiMn2O4正极材料的结构表征和电化学性能

采用共沉淀法在尖晶石LiMn2O4颗粒表面包覆Li3PO4.XRD、SEM研究结果表明,包覆后的材料仍为尖晶石结构,粒径均匀.电化学性能测试表明,Li3PO4包覆层的存在,减少了正极材料与电解液的直接接触,抑制了高温下电解液对LiMn2O4材料的侵蚀,从而有效改善了高温下材料的循环性能.在40℃时,包覆样品的比容量衰减率都低于未包覆样品,其中包覆1%Li3PO4的样品的初始比容量为110.4mAh/g,50次循环后比容量为84.1mAh/g.     

Synthesis and characterization of new organosoluble polyamides derived from bis[4‐(4‐carboxyphenoxy) phenyl]diphenylmethane

A new dicarboxylic acid containing a diphenylmethylene linkage, bis[4‐(4‐carboxyphenoxy)phenyl]diphenylmethane (BCAPD), was prepared from bis(4‐hydroxphenyl)diphenylmethane and p‐fluorobenzonitrile via an aromatic nucleophilic substitution reaction followed by hydrolysis. A series of novel polyamides were prepared by the direct polycondensation of BCAPD and various aromatic diamines. The polymers were produced with moderate to high inherent viscosities of 0.80–0.85 dL g^?1. Nearly all the polymers were readily soluble in polar solvents such as N‐methyl‐2‐pyrrolidinone, N,N‐dimethylacetamide, N,N‐dimethylformamide, and dimethyl sulfoxide, in less polar solvents such as pyridine and cyclohexanone, and in tetrahydrofuran. All the polymers were amorphous, and the polyamide films had a tensile strength and a tensile modulus greater than 80 MPa and 2.0 GPa, respectively. These polyamides had glass‐transition temperatures between 249 and 274 °C, and their temperatures at a 10% weight loss were 477–538 and 483–540 °C in nitrogen and air atmospheres, respectively. © 2001 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 39: 1156–1161, 2001     

Synthesis and Characterization of Benzylidene Bis-Dithiobenzoate

Benzal chloride reacts with sodium sulfide in alcoholic solution to yield three main products: benzyl disulfide, benzyl dithiobenzoate, and a new interesting compound 5 , C ₂₁ H ₁₆ S ₄ , which was isolated and characterized as benzylidene bis-dithiobenzoate. The intermediates obtained from the autoxidation-reduction of the unisolable thiobenzaldehyde are implied in subsequent nucleophilic addition and substitution processes. NMR spectra and X-Ray structure analysis of 5 are discussed.