BNKT BZT陶瓷的制备和性能研究

采用传统固相法制备了Bi0.5(Na0.825K0.175)0.5TiO3-Ba(TiyZr1-y)O3 (BNKT-BZT)无铅压电陶瓷.运用XRD、SEM等技术表征了陶瓷的晶体结构、形貌、介电和压电性能.研究结果表明,在所研究的结构范围内,所有陶瓷样品都形成钙钛矿固溶体.陶瓷晶粒的尺寸随x、y适当的增大而增大,压电性能随x、y的增大先增大后减小,在x=0.05,y=0.2(摩尔比)时,压电常数d33=157 pC/N,介电常数εr=1 510.     

Structural Effect of Potassium Sulfamate on Synthesis of Ammonium Dinitramide

Potassium sulfamate (PS) is an efficient starting material for the nitration reaction used in the synthesis of ammonium dinitramide (ADN), which is an environmentally friendly high-energy oxidizer for propellants that does not release chlorine-based compounds. PS is a core structure to form dinitramide, -N(NO₂)₂, by taking NO₂^? from nitric acid. In this work, five test batches of PS were prepared using a few solvents including ethanol, methanol, acetone, isopropanol, and their mixtures. The lab-made PSs matched well with the commercial PS in terms of the chemical structure. The use of acetone led to a high recovery of PS up to 97 w/w% and ultimately contributed to the formation of high-purity and (99.2%) and a high yield (57.3%) that are greater than those for commercial PS (87.3% purity and 31.3% yield). Therefore, we proved that the crystallinity and homogeneity of PS influenced the properties of ADN and the synthesis efficiency.     

甲酸盐加重瓜胶压裂液体系

为解决深层破裂压力高、常规压裂液难以压开的难题,开展了加重压裂液体系研究。由于压裂液需要进入到储层深部,因此要求加重剂具有良好的水溶性,而瓜胶压裂液需要在弱碱性环境中交联,因此强酸弱碱盐类加重剂,如氯化钙、氯化锌等不适用,溴酸盐（溴化钾、溴化钙等）虽可用但成本较高,难以应用,因此选择甲酸盐,该加重压裂液密度在1.0~1.5g/cm3范围内可调。受电性、分子量和分散性的影响,助排剂和黏土稳定剂可能与甲酸盐发生化学反应或物理作用,出现絮凝、析出或沉淀现象,通过实验优选出ME-1微乳助排剂和FP-2黏土稳定剂,结合流变性、滤失和破胶等实验,优选了与其配伍的有机硼交联剂等相关助剂,形成综合性能良好的加重压裂液体系。董8井压裂层段5 353.70~5 364.45 m,地层温度为120℃,优化加重压裂液（密度为1.2 g/cm3）现场配制工艺,成功地进行了现场应用;压后破胶液黏度小于5 mPa·s,返排率达100%。该加重压裂液技术为下一步的高闭合应力油藏的压裂改造提供了经验。      

钻井液用页岩防塌剂中磺化度测定方法的改进

磺化沥青中磺酸钠基含量为衡量其质量好坏的重要指标,其含量越高,性能越好。采用离子色谱与元素分析仪相结合,建立了1种快捷地测定磺化沥青中磺酸钠基含量的方法。此方法测定每个样品结果的相对标准偏差（RSD）均小于1%（n=5）,表明该方法具有良好重复性。经实验表明,此方法简单快速可靠,可便捷地应用于磺化沥青中磺酸钠基含量的测定。      

Minerals in vitro bioaccessibility and changes in textural and structural characteristics of uncooked pre-germinated brown rice influenced by ultra-high pressure

Ultra-high pressure (UHP) is considered as an effective processing method to enhance micronutrients utilization efficiency in germinated brown rice (GBR), but there is little information available for the effects of UHP treatments on mineral bioaccessibility and related structural characteristics. Therefore, this work examined the changes induced by UHP in the in vitro bioaccessibility of selected minerals and structural and textural properties at pressures, as well as their potential relationship. UHP treatments were applied at 100, 300 and 500 MPa for 10 min, and 0.1 MPa as control. Proximate analysis showed that free fatty acids (FFA) and moisture in GBR greatly increased after UHP treatment. Three representative minerals with different levels were chosen to assess the bioaccessibility, including phosphorus (P), magnesium (Mg) and manganese (Mn). The results demonstrated that the minerals bioaccessibility, measured by percentage solubility, were the highest when at 300 MPa whereas it decreased at 500 MPa. Correspondingly, microstructure imaging by scanning electron microscope (SEM) showed that the gelatinization of starch granule occurred at 300 MPa and it became more obvious when increased to 500 MPa. Starch gelatinization significantly lowered the hardness of GBR grains, simultaneously accompanied with the decrease of cohesiveness, gumminess and resilience through texture profile analysis (TPA). Multivariate analysis by principal component analysis and canonical correspondence analysis indicated a highly intra-associated (p < 0.01) TPA parameters and a close correlation between the bioaccessibility and hardness, chewiness and springiness. These results provide information on minerals bioaccessibility and structural properties of uncooked GBR after UHP treatment, which could lay the foundation for further elucidating the correlation between structure and micronutrients bioaccessibility.     

络合沉淀法制备BaTiO_3超细粉末

在分析ＢａＴｉＯ_３前驱体形成机理的基础上，提出了以草酸作为络合剂，用络合沉淀法制备超细ＢａＴｉＯ_３新工艺。用化学分析法测定产物Ｂａ／Ｔｉ比，用ＸＲＤ、ＴＥＭ、ＢＩ－９０激光散射粒度仪对产物的晶型、粒度及形貌进行表征。结果表明：采用该法合成的前驱体，微观组分确定，粒径小，粒度分布窄，近似球形，煅烧后为高纯超细ＢａＴｉＯ_３粉末。     

Characterization of the hard anodizing layers formed on 2014-T3 Al alloy,in sulphuric acid electrolyte containing sodium lignin sulphonate

The properties of hard anodizing layers formed on 2014 Al alloy in sulphuric acid electrolyte containing sodium lignin sulphonate were investigated. The corrosion behavior of 2014 Al alloy has been studied using potentiodynamic polarization technique. Anodic layers morphology and composition were examined by scanning electron microscope, energy dispersion X-ray (EDX), X-ray diffraction (XRD) and Fourier infrared spectroscopy (FTIR). The results showed that the corrosion resistance has been enhanced after hard anodizing of 2014 Al alloy. Addition of lignin sulphonate to the sulphuric acid electrolyte significantly improved the corrosion resistance of the anodized 2014 aluminum alloy by adsorption on copper-intermetallic phases. Adsorption of sodium lignin sulphonate on oxide surface has been confirmed by SEM, EDX, and FTIR. Phenolic and carboxylic groups in sodium lignin sulphonate are functional groups, which are responsible of complex formation on oxide surface. The morphology of the hard anodizing layer is non-homogenous due to the high copper content of 2014 Al alloy. Addition of sodium lignin sulphonate resulted in the formation of anodic layers with more homogeneity and fewer cracks.     

丙烯酰胺与2-甲基丙烯酰氧乙基三甲基氯化铵在柠檬酸钾溶液中的沉淀聚合

以(NH4)2S2O8-Na2SO3为氧化还原引发剂,通过非离子单体丙烯酰胺(AM)与阳离子单体2-甲基丙烯酰氧乙基三甲基氯化铵(DMC)在柠檬酸钾溶液中的沉淀聚合,制备了阳离子聚电解质聚(2-甲基丙烯酰氧乙基三甲基氯化铵-丙烯酰胺)[P(DMC-AM)]。利用溶解度参数原理,得知聚合物[P(DMC-AM)]在柠檬酸钾溶液中的溶解量远小于单体的溶解量,同时探讨了聚合物[P(DMC-AM)]在柠檬酸钾溶液中沉淀分离的机理。通过考察单体总转化率的影响因素,得到最佳的反应条件:柠檬酸钾质量分数57%,m((NH4)2S2O8)∶m(Na2SO3)=1∶1,引发剂总质量分数0.10%,单体总质量分数3%,单体配比m(DMC)∶m(AM)=3∶1,反应温度50℃,反应时间2h。在此条件下,DMC和AM的总转化率为86.4%。通过红外光谱分析验证,所得聚合物为[P(DMC-AM)]。     

KOAc/NaY催化合成邻甲基苯甲醚

以KOA c/NaY为催化剂,在连续流动固定床反应器内,邻甲基苯酚(OC)与碳酸二甲酯(DMC)经过气固相催化反应合成了邻甲基苯甲醚(OM)。考察了内、外扩散对KOA c/NaY催化剂活性的影响。实验结果表明,当气流线速度大于30cm/m in时可消除外扩散对合成反应的影响;当KOA c/NaY催化剂的平均粒径在0.30~0.75mm(20~80目的颗粒)时能消除内扩散对合成反应的影响。在消除内、外扩散效应后,还考察了反应温度、原料配比、空速对合成反应的影响,得到较佳的反应条件:催化剂5mL,反应温度548K,反应压力0.6M Pa,空速0.6h-1,n(DMC)∶n(OC)=1,在线评价时间7h。在此条件下,OC的转化率高达85.7%,OM的选择性大于99%。     

离子液体中K_2CO_3/CH_3I直接催化合成碳酸二甲酯

利用高压间歇反应釜,考察了K2CO3/CH3I催化CO2与甲醇直接合成碳酸二甲酯(DMC)的反应规律,得到最佳的反应条件:反应温度363K、反应压力3.6M Pa、反应时间8h、m(甲醇)∶m(CH3I)∶m(K2CO3)=12∶2.3∶1。液相产物中DMC含量随K2CO3用量的增加几乎呈直线增加,因此可以在较低的反应压力下获得较高的DMC收率。另外,利用离子液体溴代1-乙基-3-甲基咪唑盐[Em im]B r对CO2的溶解特性,研究了离子液体[Em im]B r对K2CO3/CH3I催化CO2与甲醇直接合成DMC反应规律的影响。实验结果表明,在反应温度低于393K、反应压力高于4.0MPa的条件下,离子液体[Em im]B r可以加快反应速率,对反应具有一定的促进作用,但不能改变反应的最佳条件和整体规律性。甲醇、CH3I、[Em im]B r、K2CO3的最佳质量比为12∶2.3∶1.6∶1。