The control of paracetamol particle size and surface morphology through crystallisation in a spray dryer

The parameters governing the crystallisation of paracetamol using various conventional techniques has been extensively studied, however the factors influencing the drug crystallisation using spray drying is not as well understood. The aim of this work was to investigate the crystallisation of an active pharmaceutical ingredient through evaporative crystallisation using a spray dryer to study the physicochemical properties of the drug and to use semi-empirical equations to gain insight into the morphology and particle size of the dried powder. Paracetamol solutions were spray dried at various inlet temperatures ranging from 60 °C to 120 °C and also from a series of inlet feed solvent compositions ranging from 50/50% v/v ethanol/water to 100% ethanol and solid-state characterisation was done. The size and morphology of the dried materials were altered with a change in spray drying parameters, with an increase in inlet temperature leading to an increase in particle Sauter mean diameter (from 3.0 to 4.4 µm) and a decrease in the particle size with an increase in ethanol concentration in the feed (from 4.6 to 4.4 µm) as a result of changes in particle density and atomised droplet size. The morphology of the dried particles consisted of agglomerates of individual crystallites bound together into larger semi-spherical agglomerates with a higher tendency for particles having crystalline ridges to form at higher ethanol concentrations of the feed.     

Lewis acid-oxygen vacancy interfacial synergistic catalysis over SO42−/Ce0.84Zr0.16O2–WO3–ZrO2 for N,N-diethylation of aniline with ethanol

Herein, a new mechanism involving Lewis acid-oxygen vacancy interfacial synergistic catalysis for aniline N,N-diethylation with ethanol was proposed, and the SO₄²⁻/Ce_0.84Zr_0.16O₂–WO₃–ZrO₂ catalyst (SCWZ) with both Lewis acid sites and oxygen vacancies was synthesized by the hydrothermal method, which shows better catalytic activity than the reported solid acidic catalysts. Besides, the SO₄²⁻/ZrO₂ (SZ) and SO₄²⁻/WO₃–ZrO₂ (SWZ) catalysts were also prepared and compared with SCWZ to investigate the synergistic effect of each component. The SO₄²⁻ and WO₃ mainly generate Lewis acid by bonding with ZrO₂, which is beneficial for the fracture of the N–H bond in aniline. The Ce_0.84Zr_0.16O₂ solid solution mainly plays a vital role in generating the oxygen vacancies as the interface active species, which can participate in stripping –OH from ethanol, then the carbocation will also be released, which only needs 1.3805 kcal/mol energy, calculated by density functional theory (DFT), to be input. In comparison, the traditional reaction mechanism needs the Brønsted acidic sites to promote the protonation of ethanol, then dehydration and subsequent formation of carbocation followed, and 108.6846 kcal/mol energy needs to be input, which is far higher than that of the new mechanism. The apparent activation energy (E_a) over SCWZ was measured by experiment to be 34.09 kJ/mol, which is much lower than that of SWZ (47.10 kJ/mol) and SZ (54.37 kJ/mol), illustrating comparatively preferable kinetics for SCWZ than that of SWZ and SZ. Besides, the conversion of aniline and selectivity to N,N-diethylaniline over SCWZ reach almost 100% and 73%, respectively. The SCWZ can be renewed for 4 times without rapid deactivation, and the longevity of SCWZ is longer than that of SWZ and SZ, as the loaded SO₄²⁻ and tetragonal ZrO₂ are stabilized by Ce_0.84Zr_0.16O₂ and WO₃, respectively.     

水射流表面改性对国产Zirlo锆合金包壳管加速腐蚀氧化膜形貌的影响

为进一步提高国产锆合金包壳管性能,提高反应堆安全性,对国产Zirlo锆合金进行水射流冲击强化,研究在高温高压水腐蚀条件下不同冲击压力对样品表面氧化膜的影响,并与未冲击样品进行对比。结果表明,样品表面在不同压力的冲击下耐蚀性差异较大,当冲击压力达到40 MPa时样品表面氧化膜状态较好,相比于未冲击样品氧化膜厚度减少4.3%,在10 MPa和20 MPa冲击下则出现腐蚀加速情况。     

改性氧化钛对羟乙基乙二胺水溶液解吸CO2的强化

羟乙基乙二胺（AEE）水溶液的CO₂循环吸收量高（1.2molCO₂/molAEE），吸收速度快，稳定性好，但解吸速度慢、解吸量少（0.8mol CO₂/mol AEE）是限制该技术广泛应用的主要原因。本文通过向AEE水溶液中添加质量分数为0.05%～0.20%的改性氧化钛（TiO₂-MWCNT和TiO₂-OH）强化AEE的解吸能力。CO₂循环吸收（40℃）-解吸（120℃）实验结果表明改性氧化钛的添加比氧化钛强化CO₂解吸效果更好，强化顺序为TiO₂-MWCNT＞TiO₂-OH；其对应的最大解吸速率分别为0.093L/min（质量分数0.15%）和0.083L/min（质量分数0.20%），相对于AEE水溶液，分别提高了32.9%和18.6%；其对应的最大解吸量分别为0.92molCO₂/molAEE（质量分数0.15%）和0.88molCO₂/molAEE（质量分数0.20%），分别提高了12.2%和9.7%；其对应的CO₂循环吸收量分别是0.95molCO₂/molAEE（质量分数0.15%）和0.89molCO₂/molAEE（质量分数0.15%），分别提高了18.75%和11.25%；5次循环吸收解吸实验结果表明改性氧化钛强化CO₂解吸效果稳定，具有较强的化学稳定性。对反应后的改性氧化钛进行XRD、BET、FTIR和SEM表征，结果表明改性氧化钛具有较强的结构稳定性。TiO₂-MWCNT和TiO₂-OH在促进有机胺溶液解吸CO₂方面具有一定的工业应用潜力。     

紫金山东南矿段成矿期次、阶段浅析

通过对紫金山东南矿段铜钼(金)矿床地质矿化特征分析,指出铜钼矿化带主要赋存于花岗闪长斑岩的内外接触带,处于似斑状花岗闪长斑岩的上部,金矿化带赋存在表生氧化带的英安玢岩、隐爆角砾岩中。经过对矿石的组构特征、矿物生成顺序等特征分析,将矿床的成矿演化过程分为斑岩热液期、高硫化浅成低温热液期、表生氧化期三个主要矿化期次,进一步将斑岩热液期分为黑云母-钾长石化阶段、石英-绢云母化阶段、碳酸盐化阶段三个阶段;高硫化浅成低温热液期分为地开石化阶段、明矾石化阶段、硅化阶段三个阶段。研究结果为进一步研究矿床成因提供了依据。     

水平衡法与高温转化法在矿泉水氢氧稳定同位素测定中的应用

为了鉴别不同品牌矿泉水标注水源地信息真伪,对11种不同品牌饮用水的氢氧稳定同位素(δD和δ18 O)进行测定。结果表明,水平衡法(GasBench-IRMS)和高温转化法(TC/EA-IRMS)的测定结果一致性较好,两种方法测定6种不同饮用水的δD和δ18 O的平均差异分别为(0.6±1.59)‰和(0.02±0.13)‰。水平衡法需要较长的制备和测定时间,但δD和δ18 O的测定精度明显优于高温转化法。11种饮用水δD和δ18 O变化范围较大,其δD和δ18 O受不同品牌饮用水的水源地降水影响形成明显的地域性。虽然无法区分矿泉水是否由其他类别饮用水伪造,但δD和δ18 O可以为特定区域(如高海拔与沿海地区)以及产地相近的矿泉水水源地鉴别提供依据。     

镓锗铜萃余液综合利用研究与应用

本文针对镓锗铜综合回收系统产出的萃余液,设计通过中和氧化除杂、锌粉置换除铜镉、有机试剂除钴镍、纯碱法生产碱式碳酸锌、高温煅烧生产活性氧化锌和一步法生产元明粉的生产工艺流程,有效的将镓锗铜萃余液分类分离富集,产出具有价值的富集渣和工业产品,进一步提升综合回收经济效益。     

[学科发展]机构学中机构重构的理论难点与研究进展——变胞机构演变内涵、分岔机理、设计综合及其应用

生产力发展与工程技术革新要求机构具备可自重组与可重构及“一机多用”的功能，以满足复杂工况需求。可重构机构具有可变活动度和可变构态，可以满足多任务、多工况与多功能的要求，然而，决定其设计方法的演变内涵与分岔机理的研究目前仍不为学者们充分了解。从变胞机构的演变与分岔机理的角度，以旋量理论、李群与李代数及微分流形为主要工具，揭示了机构演变内涵及运动与约束空间的内在关联关系；探究了机构演变中的分岔机理与可控奇异位形，回顾了变胞机构与折纸及折展机构的历史渊源，综述了变胞机构的构型设计、性能综合与新型设计理念及其创新应用。     

[可靠性建模及试验技术]重型机床液压元件油液污染退化量分布剖面可靠性建模

针对重型机床液压系统故障频繁且多与油液中的固态颗粒污染物相关的问题，进行了油液污染趋势变化试验。通过时域分析获得了油样颗粒数的有量纲和量纲一参数，通过Q-Q图和K-S检验分析有量纲参数，污染颗粒数是退化量服从正态分布的退化数据。进行了油液污染与环境相关性分析试验，采用相关系数法分析得到，颗粒数变化量与一定范围内的温度、流量、压力的相关性小；将液压元件分为管路、阀、过滤器三类，用直径5 μm左右的颗粒和直径大于15 μm的颗粒分别研究管路及阀件的堵塞和磨损情况，以过滤器过滤精度大小的颗粒研究过滤器的堵塞情况，设定ISO4406标准20/17级对应的颗粒数为阈值，利用退化量分布建立了液压元件单一故障模式的可靠性模型；利用竞争失效模型将上述模型融合为多故障模式下的可靠性模型。