Preparation and properties of some transition metal phosphorus trisulfide compounds

Transition metal phosphorus trisulfide compounds with the general formula MPS₃, with M = Mn, Fe, Ni, have been prepared by chemical vapor transport, vapor sublimation, and direct combination of the elements. Chemical transport is accomplished by using 75 Torr of chlorine gas as a transport agent and a temperature gradient of 750° → 690°C or 700° → 640°C. The structure of these three compounds, which belongs to the monoclinic space group $\text{C2}\text{m}$, is related to that of CdCl₂ with a distorted cubic close-packing of the sulfur atoms. Metal atoms and phosphorus-phosphorus pairs occupy the trigonally distorted octahedral holes in a ratio of 2:1 and are ordered throughout the structure. Magnetic susceptibility measurements indicate that all three compounds are antiferromagnetic. The paramagnetic moments indicate that the metal ions in each case exist in the divalent high-spin state.     

纳米SiO_2亲和吸附剂的制备及性能

采用水热法一步合成了巯基纳米二氧化硅(SiO_2-SH),随后在其表面修饰亚氨基二乙酸基团(-IDA)得到了SiO_2-SH/IDA,利用-SH和-IDA双官能团更多的吸附溶液中的Ni~(2+),从而得到SiO_2-SH/IDA-Ni~(2+)纳米亲和吸附剂.制备的亲和吸附剂可直接用于六聚组氨酸为标签的(His-tagged)融合蛋白的分离纯化.利用TEM、FT-IR、TG、SDS-PAGE等大型仪器表征了样品的形貌、结构及亲和分离能力.结果表明制备的SiO_2-SH/IDANi~(2+)纳米亲和吸附剂平均粒径为60nm,对His-tagged蛋白具有较好的特异性和较低的检测限(约为1.9×10~(-5)mol/L),且该吸附剂再生能力较强,再生3次后对目标蛋白仍具有较好的分离效果.     

Preparation of some chitosan heavy metal complexes and study of its properties

The chitosan was prepared and mixed with some metal salts (FeCl₃, Co(OAc)₂ and NiCl₂) by different concentrations to form chitosan-metal complexes. The metal ions which strongly complexed to the amino groups of chitosan like Fe showed a smooth surface product, amorphous phase, thermally more stable and high electrical conductivity than other complexes, while the Co ions which the weakly complexed with chitosan showed a rough surface product, crystalline phase, thermally less stable and low electrical conductivity. The chitosan-metal complexes have a higher electrical conductivity than chitosan pure at room temperature.     

Preparation and properties of some cardopolyamides

Several polyamides that contained cardo units were prepared. Thus 9,9-bis(4-aminophenyl)fluorene and 9,9-bis(4-aminophenyl)anthrone were condensed with 2,5-dimethyl-1,4-benzenediacetyl chloride, 2,4-dimethyl-1,4-benzendiacetyl chloride, and 2,5-dimethoxy-1,4-benzediacetyl chloride. Lowtemperature solution polycondensation in dimethyl acetamide (DMAc) was used throughout. The polymers were obtained in 80–90% yield and possessed intrinisic viscosities in the range of 0.6–1.2. The polymers were characterized by infrared (IR) spectra and elemental analysis. The solubility, crystallinity, and thermal stability of the polyamides were also determined.     

Preparation and some properties of polyoxathiaferrocenophanes

Some sulfur analogs of a crown ether-like compound containing ferrocene as a ring member were prepared. Their complexing ability was poor with alkali metal cations but good with a silver cation.     

Preparation and properties of some peralkylpolygermanes

Summary The alkylation of trihalogenogermane etherates 2R₂O·GeCl₃ with Grignard reagents RMgBr forms, in addition to tetraalkylgermanes, polyalkylpolygermanes R(GeR₂)_nR having an exclusively linear structure.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 6, pp. 1395–1398, June, 1977.     

Thermoelectric properties of some metal borides

Polycrystalline AlMgB₁₄ and some hexaborides (CaB₆, SrB₆, YbB₆, SmB₆, and CeB₆) were synthesized to examine their thermoelectric properties. Single phase of orthorhombic AlMgB₁₄, which contains B₁₂ icosahedral clusters as building blocks, was obtained at sintering temperatures between 1573 and 1823 K. Seebeck coefficient (α) and electrical conductivity (σ) of the phase were about 500 μV/K and 10⁻¹ 1/Ω m at room temperature, respectively. These values are comparable to those of metal-doped β-rhombohedral boron. On the other hand, metal hexaborides with divalent cation possessed large negative α ranging from −100 to −270 μV/K at 1073 K. Calculated power factors of CaB₆ and SrB₆ exceeded 10⁻³ W/K² m within the entire range of temperature measured. As a result, they can be thought as promising candidates for n-type thermoelectric material.     

二苯并噻吩分子印迹功能化MOF199吸附剂的制备及性能

结合分子印迹技术,MOF199为基体,以二苯并噻吩(DBT)为模板分子,甲基丙烯酸(MAA)为功能单体,制备了新型表面分子印迹聚合物材料MOF@SMIP。采用SEM、BET、FT-IR等对其结构和形貌进行表征,在模拟油样中进行吸附评测,吸附平衡时间为1.5 h。MOF@SMIP对DBT吸附量为130.73 mg/g较MOF199吸附量37.79 mg/g有很大提升,同时MOF@SMIP吸附量对比MOF@NIP吸附量(57.13 mg/g)优势明显,印记因子f_(imp)为2.29。吸附行为遵循伪一阶动力学模型说明吸附主要为物理过程。选择性吸附实验表明,MOF@SMIP对目标分子DBT表现出比对结构类似物苯并噻吩(BT)和联苯更高的亲和力,吸附DBT对干扰物BT和联苯的相对选择系数k'分别达到2.55和2.14。     

Preparation and some properties of nylon 46

Nylon 46 was synthesized from the salt of 1,4-diaminobutane and adipic acid. High molecular weight polymers could be obtained by reaction for 1 hr at 215°C in a closed system and at least for 1 hr in vacuo at a temperature in the range 290–305°C. The reactions at 290°C were found to have taken place in the solid state and those at 305°C in the melt. The highest molecular weights (M?_w ca. 45,000) were obtained by reaction at 290°C with a nylon salt with a pH of 7.8–8.0. The molecular weight characteristics were studied with end-group analysis, viscometry, light scattering, and ultracentrifugation. The polymers were found to be gel-free and monodisperse (M?_w/M?_n ～ 1.15). Films could be cast from formic acid. From x-ray diffraction patterns, measured on such films, spacings of 3.74 and 4.30 Å were calculated, whereas a long period of 66 Å was also found. The infrared spectra showed all the usual amide bands of even–even polyamides. The melting temperature was found to vary between 283 and 319°C, depending on the thermal history of the sample. Water absorption measured on a cast film showed this to be very hygroscopic (7.5% at 65% RH), while a highly crystalline sample absorbed only little water (1.6% at 65% RH).     

Preparation and some properties of porcine chymotrypsinogen

Summary A homogeneous preparation of chymotrypsinogen has been obtained by the fractional salting out of an acid extract of porcine pancreas and subsequent chromatography on a column of CM-cellulose. The isoelectric point of the enzyme has been found to be pH 8.8 and the optimum value of the pH for activation with trypsin 7.6. The enzyme is most stable in solutions with pH 3.0.     

Preparation and some properties of nylon-4,2

An attempt was made to produce a new short-chain alphatic polyamide nylon-4,2. This polyoxamide can be prepared by polycondensation of tetramethylene diamine and diethyl oxalate. A high molecular weight polymer (η_inh = 1.9 from 0.5% solutions in 96% sulphuric acid) has been obtained by employing a two-step polycondensation method; the precondensation was carried out in solution at low temperatures (20–140°C) and the postcondensation in the solid state at high temperatures (250–300°C). The effect of solvent composition and reaction temperature on the prepolymerization and the effect of reaction time and temperature on the postcondensation was studied. We also investigated the influence of moisture during washing, storing, and the solid-state reaction on the polymerizability by the postcondensation. Nylon-4,2 is soluble only in highly polar solvents such as trifluoroacetic acid (TFA), dichloroacetic acid, and 96% sulphuric acid. Films were cast from TFA. With these films we studied the IR spectrum, WAXS pattern, water absorption, and melting behavior. Nylon-4,2 was found to melt at 388–392°C, has a crystallinity of 70%, and a low water absorption (3.1% at 50% RH). The glass transition temperature of the dry sample was found to be at ～120°C and for the wet sample at ?15°C.     

Preparation of some metal carbonyl cluster formyl compounds

The reduction of H₂Os₃(CO)₁₀S or HOs₃(CO)₁₀(O₂CMe) with KBH(OPr-i)₃ at low temperatures yields unstable formyl complexes which have been identified by ¹H NMR spectroscopy; at higher temperatures conversion into stable hydridoanions is observed.     

Preparation and properties of some stable arsonium ylides

Stable crystalline arsonium ylides have been prepared by thermal decomposition of diazo compounds in the presence of triphenylarsine, and by condensation reactions of reactive methylene compounds with triphenylarsine oxide. The spectra of these ylides, and their reactions with benzaldehydes are discussed. Like other stabilised arsonium ylides they give alkenes rather than epoxides in Wittig reactions. They are generally more polar than their phosphonium analogues and also are more reactive in the Wittig reaction. With diphenylcyclopropenone some more reactive arsonium ylides form α-pyrones.     

Preparation and some properties of pyrimidine 1,3-dioxides

Oxidation of 1-hydroxy-1,2,5,6-tetrahydropyrimidine 3-oxides with active manganese dioxide leads to pyrimidine 1,3-dioxides. Depending on the conditions, pyrimidines or isomeric pyrimidine N-monoxides are formed by deoxygenation of pyrimidine 1,3-dioxides with triethyl phosphite.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 259–261, February, 1977.     

Preparation and some physicochemical properties of benzylammonium sulfates

New method of preparation of multisubstituted benzylammonium cations via interaction in the SO₂-L-H₂O systems (L is benzylamine, α-phenylethylamine, N,N-dimethylbenzylamine, or dibenzylamine) has been developed. The products have been studied by X-ray diffraction, IR, Raman spectroscopy, and mass spectrometry.     

Preparation and properties of zeolite coating on metal surface

Crystals of mordenite were grown on metallic Cr surface by the vapor phase method. The material of zeolite coating on metal surface has been characterized by X-ray powder diffraction and microprobe. It is shown by the results that this material possesses good catalytic properties.

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