清脉颗粒醇沉工艺的正交优选

目的：优选清脉颗粒的醇沉工艺。方法：选取药液相对密度,醇沉浓度及醇沉时间为考察因素,以干浸膏得率,薯蓣皂苷元苷含量为考察指标,采用正交试验优选醇沉工艺。结果：优选的醇沉工艺为药液浓缩至相对密度1.13 - 1.18 g·;ml-1,加乙醇至乙醇体积分数为60%,醇沉24 h。结论：优选的工艺稳定可行,为清脉颗粒的临床应用提供试验依据。     

Correction: Hood,M.A., et al. Synthetic Strategies in the Preparation of Polymer/Inorganic Hybrid Nanoparticles. Materials 2014, 7, 4057–4087

This article reviews the recent advances and challenges in the preparation of polymer/inorganic hybrid nanoparticles. We mainly focus on synthetic strategies, basing our classification on whether the inorganic and the polymer components have been formed in situ or ex situ, of the hybrid material. Accordingly, four types of strategies are identified and described, referring to recent examples: (i) ex situ formation of the components and subsequent attachment or integration, either by covalent or noncovalent bonding; (ii) in situ polymerization in the presence of ex situ formed inorganic nanoparticles; (iii) in situ precipitation of the inorganic components on or in polymer structures; and (iv) strategies in which both polymer and inorganic component are simultaneously formed in situ.     

超临界CO2沉析HMX过程中过饱和度与颗粒尺寸的关系

用超临界CO2在丙酮溶液中沉析环四亚甲基硝胺(HMX)，研究了溶液过饱和度与沉析颗粒尺寸及粒径分布之间的关系。结果表明：用超临界CO2沉析HMX，可在短时间内产生很大的过饱和度。当温度33～50℃，压力5．5～12．0MPa时，在前几分钟内，溶质HMX的浓度快速下降从而在短时间内产生很大的过饱和度。依据吉普斯能传统结晶理论估算了在一定过饱和度下的成核速率。过饱和度愈大、成核速率愈大，沉析的HMX颗粒度愈细。当过饱和度在短时间内形成并导致大量成核快速消耗过饱和度时，可以得到粒度更细，分布更窄的HMX颗粒，如33℃、12．0MPa时，能得到粒径5．1～7．1μm窄分布的HMX细颗粒。     

泡沫分离,带溶剂萃取和沉淀法提取庆大霉素

研究了用文题法从水相中分离砂大霉素的各种操作因素对分离过程的影响。在最适条件下，种方法对庆大霉素配制液的收率分别为７２％，８８％，８７％，无机盐能使沉淀收率提高。将上述３法用于发酵液时，泡沫法和萃取法的收率均有显著降低，而沉淀法依然能达到很高的收率，ψ＝捍沉淀率约为１００％．     

Separation of bone matrix proteins by calcium-induced precipitation

Summary It was found that significant precipitation occurred immediately after calcium, at a concentration as low as 2 mM, was added to a desalted solution of EDTA extract of adult bovine femur. The maximal yield of the precipitates was observed at a calcium concentration of 30 mM. These precipitates were dissolved in 0.5 M EDTA, desalted, and characterized by Sepharose CL-6B gel filtration chromatography and high performance gelexclusion chromatography. Results revealed that the precipitates were enriched in a 40 K protein and a higher molecular weight fraction as compared with the original extract of bone proteins. The 40 K fraction was isolated and identified as osteonectin, as judged from amino acid analysis, electrophoresis, and immunodetection. The supernatant after calcium-induced precipitation predominantly contained osteocalcin and a 50 K protein that was tentatively identified as α2HS protein. Osteonectin was purified from the calcium-induced precipitates from the EDTA extract of bovine bone. By calcium titration using fluorescence spectrometry, the isolated osteonectin showed high affinity to calcium ions with an apparent dissociation constant (K_0.5) of 8×10⁻⁷ M. Thus, the use of calcium to separate bone proteins, especially osteonectin, was proved to be a useful technique. In addition, calcium-induced precipitation of osteonectin suggested a possiblein vivo mechanism via which osteonectin might interact with calcium ions and participate in the initial immobilization of calcium to induce the nucleation of calcification in bone tissue.     

活血养阴颗粒提取纯化工艺研究

目的研究活血养阴颗粒制备工艺,优选最佳提取、纯化工艺条件。方法以葛根素含量、含固量为检测指标,用正交试验考察了3种因素(加水量、煎煮时间、煎煮次数)对其水煎煮工艺的影响;然后比较了不同的醇沉浓度的去杂效果。结果活血养阴颗粒最佳水提工艺条件为先加12倍量水,煎煮1.5 h,再加10倍量水,煎煮1 h,煎煮2次;去杂工艺以60%乙醇沉为佳。结论制备工艺合理。     

Analysis of Hydrometallurgical Methods for Obtaining Vanadium Concentrates from the Waste by Chemical Production of Vanadium Pentoxide

The paper describes hydrometallurgical methods to recycle wastes of vanadium pentoxide chemical fabrication. Sludges containing a significant amount of V₂O₅ can be considered as an additional source of raw materials for vanadium production. We studied the one-stage leaching method using various iron-based reductants for converting V⁵⁺ to V⁴⁺ in a solution allowing to precipitate V when its concentration in the solution is low. As a result of the reduction leaching with further precipitation, we obtained concentrates with V₂O₅ content of 22–26% and a high amount of harmful impurities. Multistage counterflow leaching can be used to fabricate solutions with vanadium pentoxide concentration suitable for vanadium precipitation by hydrolysis and adding ammonium salts. The solutions with V₂O₅ content of ≈15 g/L can be obtained from the initial sludge by three-stage counterflow vanadium leaching. A concentrate with a content of 78 wt% V₂O₅ can be precipitated from these solutions at pH = 2.4 by adding ammonium chloride. Additionally, concentrate with V₂O₅ content of ≈94 wt% was precipitated from the solution with a concentration of >20 g/L V₂O₅ obtained from the roasted sludge. The concentrates were purified for increasing the vanadium content to 5–7%. The consumption and technological parameters of the considered processes are presented in the paper.     

Influence of Cold Deformation on Carbide Precipitation Kinetics in a Fe-22Mn-0.45C TWIP Steel

The carbide precipitation kinetics in a Fe-22Mn-0.45C TWIP steel subjected to three different cold-deformation levels, annealed at various temperatures, were studied. The studied carbides included chemical compositions, morphology, precipitation sites, volume fraction, and size. Manganese carbides were precipitated in a temperature range between 525 and 650 °C. Volume fraction increased with cold-deformation and decreased with annealing temperature. Carbide size increased with cold-deformation and annealing temperatures up to 625 °C, suffering a notable reduction at 650 °C. Precipitation kinetics were described by means of precipitation curves for 0.1% (vol.) of Fe-Mn-carbides. A kinetic model was used, and two stages were found. Complementarily, austenite grain size and microhardness were also measured. With increases in annealing time, microhardness decreased until it reached a nearly constant value, indicating that recrystallization was complete, while, with increases in annealing temperature, grain size increased.     

The Effect of the Pre-Existing VC on the Evolution of Precipitate and Mechanical Properties in the H13 Steel

To further improve the mechanical properties of H13 steel at room and high temperatures, its precipitates were regulated based on the Thermo-Calc results. Scanning electron microscope (SEM), electron backscattering diffraction (EBSD), transmission electron microscope (TEM), and X-ray diffraction (XRD) Rietveld refinement were used to study the effect of the intercritical annealing on the microstructure and mechanical properties of H13 steel. The results show that the intercritical annealing at 850~95 °C increased the VC volume fraction from 2.23 to 3.03~3.48%. Increasing the VC volume fraction could inhibit the M₇C₃ precipitation from 10.01 to 6.63~5.72% during tempering. A large amount of VC also promoted the M₂₃C₆ precipitation during tempering at higher dislocation densities. The intercortical annealing simultaneously increased the elongation of H13 steel. An excellent combination (room temperature: ultimate tensile strength (UTS) of 898 MPa and total elongation (TEL) of 19.35%, 650 °C: UTS of 439 MPa, and TEL of 27.80%) could be obtained when intercritical annealing is performed at 900 °C. Meanwhile, after aging at 650 °C for 128 h, the room temperature UTS and TEL decreased by only 31 MPa and 0.52%, respectively.     

均匀纺锤形α-Fe2O3的制备及其等电性研究

以硝酸铁为原料，尿素为均匀沉淀剂，磷酸二氢钠为结晶助剂，用动态开放回流系统的均匀沉淀法制备了纺锤形α-Fe2O3粒子。并用XRD、TEM等进行了表征。当Fe(NO3)3、NaH2PO4、CO(NH2)2的浓度分别为0．20、0．0015、0．10mol／L，反应温度为117℃，陈化时间为13h时，制备的粒子轴比可达3．3，且分散性较好，粒径分布窄，陈化时间短，产率较高。对反应机理、结晶助剂NaH2PO4的作用等作了初步研究。并测量了不同pH值时粒子的Zeta电位值，找出了粒子的等电点，与理论估算值接近。