氧化钇粒度控制与测定

用氨水或碳酸氢铵与氯化钇溶液反应生成沉淀，煅烧沉淀制备了D50为0．45μmt 2-10μm的各种粒径的氧化钇粉末。分别采用Coulter MultisizerⅡ和90Plus粒度仪测定微米和亚微米级氧化钇粉体粒度，研究了分散剂，待测样品量，分散时间等因素对亚微米级氧化钇粉体粒度测量精度的影响。     

低温烧成YAG用前驱体碳酸钇铝铵的合成

以Al(NO_3)_3,Y(NO_3)_3为原料,NH_4HCO_3为沉淀剂,利用共沉淀法制备了能够在较低煅烧温度下形成纯YAG相的前驱体碳酸钇铝铵粉体。采用红外光谱、X射线衍射、扫描电镜等技术对不同沉淀条件下所得沉淀的组成和过滤性能以及烧成YAG粉体的相纯度和颗粒特征进行了表征。研究了温度、加料方式、陈化和搅拌时间等条件对过滤效率和颗粒表面电位的影响。结果表明:采用简单的将钇铝混合硝酸盐溶液加入到NH_4HCO_3溶液中的反向沉淀法,可以获得易于过滤的碳酸钇铝铵无定型沉淀。这种无定型碳酸钇铝铵前驱体在高温煅烧下形成纯YAG相所需的温度比陈化后的结晶碳酸钇铝前驱体要低200℃。在1100℃下煅烧2 h所得产物为直径在60 nm左右的类球形均匀颗粒。     

超细粉体制备Nd:Y2O3透明陶瓷

采用碳酸氢铵为沉淀剂合成了碱式碳酸钇沉淀前驱体,研究了的前躯体的煅烧工艺对氧化钇粉体性能及烧结氧化钇陶瓷组织、致密化行为以及透光率的影响。在1000℃煅烧6 h获得的超细粉体,经过在氢气介质中1750℃保温3 h烧结后,获得组织均匀,无残余气孔,透光率高的氧化钇陶瓷。     

制备工艺对超细氧化钇粉体形态与烧结性的影响

以碳酸氢铵为沉淀剂,研究了不同沉淀反应终点pH值、陈化时间,以及沉淀前驱体煅烧温度对超细氧化钇粉体的形态和烧结致密化的影响。沉淀反应终点pH=7.0和7.8时,随着陈化时间的增加,煅烧后的粉体颗粒均匀长大、形态近似于球形,烧结致密化程度较高。在pH=8.3时,陈化处理后粉体颗粒长大明显且呈不规则形状,而且随陈化时间增长,粉体的烧结活性降低。另外,沉淀前驱体在800℃煅烧得到的超细氧化钇粉体中残留较多的非晶相,造成粉体烧结致密化程度降低;在1000℃煅烧时可以完全消除粉体中的非晶体相,所得到的超细球形粉体颗粒的烧结温度低,致密化程度高。     

碳酸钇铵复盐结晶的形成及影响因素

对碳酸氢铵沉淀钇时碳酸钇铵复盐结晶的形成条件与ｐＨ变化特征进行了研究,发现其结晶过程与平衡溶液ｐＨ有对应关系。溶液ｐＨ由碳酸钇铵结晶化反应和碳酸氢铵的水解反应所控制。根据溶液ｐＨ的变化可以判断结晶反应是否发生或完成,以及结晶速度的快慢和结晶的程度。Ｘ－射线衍射及差热－热重分析结果表明,产物为复盐结晶２,加料方式对结晶的形成有很大影响。     

碳铵沉淀法制备纳米氧化钇过程中氯离子的行为

研究了碳酸氢铵沉淀法制备纳米氧化钇过程中氯离子的行为及去除方法,认为沉淀物的组成为Y(OH)0.1Cl0.1(CO3)1.4·2H2O。讨论了氯离子的存在形式,氯离子主要以氯化铵吸附或夹带和碳酸钇复合物的形式存在,其中碳酸钇复合物和颗粒内部夹带的氯离子是影响最终纳米氧化钇中氯含量的关键。通过实验研究证明采用洗涤和提高煅烧温度和延长保温时间可以有效减少氯离子的含量,制得了氯离子含量为0.054%的纳米氧化钇粉体。     

二氧化碳碳化法制备氧化镧粉体研究

对二氧化碳直接碳化制备氧化镧粉体进行了研究,以氯化镧溶液和二氧化碳为原料,通过调控反应体系pH值制备获得稀土碳酸盐,再经过焙烧得到粒径小、粒度分布窄的氧化镧粉体。研究表明:在不同反应温度和pH条件下,通过碳化法可以获得不同形貌的前驱体,其中控制反应温度为25℃,pH为5的条件下,可以获得片状碳酸镧前驱体;经XRD,FI-IR,TG-DSC分析表征,确定该前驱体化学组成为La2(CO3)3·3.2H2O;通过焙烧可获得中值粒径D50为4.75μm,粒度分布(D90-D10)/(2×D50)<1.00的氧化镧粉体。二氧化碳碳化法制备氧化镧粉体技术具有条件温和、产品粒径小、粒度分布窄、易规模化生产的优点,而且可以实现二氧化碳循环利用以减少温室效应。     

复合沉淀剂制备高质量碳酸镧及氧化镧的研究

为满足稀土工业生产对环保、经济的沉淀剂及沉淀技术的需求,以氯化镧料液为原料,碳酸氢钠和碳酸钠为复合沉淀剂制备了碳酸镧和氧化镧。研究了加料方式、复合沉淀剂配比、反应温度、料液浓度、料液及沉淀剂的流量、沉淀过程pH值范围、添加晶种等因素对碳酸镧形貌、粒度及氧化镧中Cl~-,Na₂O含量和稀土总量(REO)等理化性能的影响,运用SEM、粒度分析、XRD等手段对碳酸镧或对应氧化镧形貌、粒度进行了表征。结果表明,控制复合沉淀剂中碳酸氢钠和碳酸钠摩尔比为1∶4,反应温度30℃,料液浓度为110g·L^-1,料液流量为6.0mL·min^-1,沉淀过程pH值为4.0～4.5,在添加适量碳酸镧晶种和并流加料的条件下,可获得易沉降,粒度D50为23.46μm,形貌为片状堆叠成的类球形La₂(CO₃)₃·8H₂O晶体;灼烧后氧化镧产品稀土总量为99.62%,Cl~-和Na₂O含量分别为0.01%和0.001%,达到国家标准GB/T415...     

Na_2CO_3沉淀制备超细Y_2O_3粉体的研究

超细Y_2O_3具有尺寸效应和稀土元素的双重特性,广泛应用于MLCC,超耐热合金等高新材料。在前期获得晶型Y_2(CO_3)_3的基础上,对Na_2CO_3沉淀制备超细Y_2O_3粉体进行了深入研究,结果表明:与温度、浓度等条件相比,搅拌陈化过程对Y_2(CO_3)_3粒度的影响较大,可以使针状和片状聚集的类球形Y_2(CO_3)_3粉体逐渐分散转化成粒度更小的颗粒;实验最终在并流加料、反应温度40℃, pH 5.5～6.5, YCl_3浓度1.0 mol·L~(-1),加料速度10 mL·min~(-1),搅拌转速600 r·min~(-1), 40℃搅拌陈化48 h的条件下可得到D_(50)=3.77μm,(D_(90)-D_(10))/2D_(50)=0.70的Y_2(CO_3)_3;在550℃较低温度下焙烧2 h后,得到了D_(50)=2.69μm,(D_(90)-D_(10))/2D_(50)=0.97的超细氧化钇粉体。研究为Na_2CO_3沉淀制备超细Y_2O_3工艺提供基础和可能,对提高Y_2O_3产品附加值和减少普通Y_2O_3积压具有重要意义。     

稀土铝酸盐蓝色荧光粉前驱体的制备及其应用

以硫酸铝铵和碳酸氢铵为原料，制备了结晶碳酸铝铵，用IR，XRD，DTA－TG等手段研究了结晶碳酸铝铵在煅烧过程中的相变和热分解机理，并考察了煅烧过程中的粒度和比表面变化以及煅烧产物的外观形貌，结果表明：在煅烧过程中结晶碳酸铝铵首先分解为无定型氧化铝，并依次从无定型Al2O3-γ-Al2O3-κ-Al2O3,δ-Al2O3,τ-Al2O3-α-Al2O3,τ-Al2O3-α-Al2O3转变，比表面在600℃之前是随温度升高而增大，600摄氏度之后则下降，而粒度变化在900摄氏度之前随温度升高而降低，900摄氏度之后则增大，煅烧产物为粒度在2-3um的片状结晶氧化铝，用该氧化铝所合成的稀土铝酸盐蓝粉，晶相纯，发光强度高，且粒度小，可以满足不球磨蓝色荧光粉的基本要求。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

化学计量中不确定度评定研究进展

测量不确定度是表征合理地赋予被测量之值的分散性的参数。本文针对化学计量不确定度评定基础模型仅适用于线性模型、概率分布为正态分布或缩放位移t分布等局限,介绍了近年来不确定度评定的研究热点:蒙特卡罗方法(Monte Carlo Method,MCM),不确定度评定的来源、评定概念、评估方法及其发展过程,扩大了测量不确定度评定与表示的适用范围。     

微量钙的测定方法研究进展

介绍了1995-2006年期间测定微量和痕量钙的方法,如电感耦合等离子体-原子发射光谱法、原子吸收光谱法以及离子色谱法等的工作原理和特点,并说明了其测定微量钙的应用领域。并对微量钙的测定技术进行了展望(引用文献55篇)。