Alkali-activation of marble sludge: Influence of curing conditions and waste glass addition

The use of marble sludge as precursor for new alkali activated materials was assessed studying three different curing conditions (air, humid and water immersion, respectively), after an initial curing at 60 °C for 24 h, and two glass powder fractions additions (2.5 and 5.0 vol%). Microstructural, physical (drying shrinkage, Fourier transform-infrared (FT-IR) spectroscopy, X-ray spectroscopy (XPS)), thermal (differential thermal analysis – thermogravimetric analysis, DTA-TGA) and mechanical (flexural and compressive strength) properties were investigated. Air curing was the most favourable atmosphere for mechanical properties development because it promotes Si-O-Si polymerization and gel densification, as demonstrated by FT-IR and FE-SEM observations, respectively. Satisfactory mechanical properties were achieved (18 MPa and 45 MPa, for flexural and compressive strength, respectively) in particular for glass containing mixtures. Moreover, glass powder addition significantly reduced drying shrinkage of air-cured samples because it operated as a rigid aggregate in the matrix and strengthened the formed gel.     

硫酸铵法利用中低品位锂瓷土矿制备碳酸锂技术研究

针对江西宜丰地区氧化锂质量分数<2.0%以下中低品位锂瓷土矿,研究了硫酸铵法提取碳酸锂技术路线。首先,利用二步焙烧工艺,有利于脱氟、提高锂浸出率,并且能够有效防止结窑现象发生。在浸出液除杂过程中,采用成矾除铝的方法将大量溶出的铝离子转变为KAl（SO₄）₂·12H₂O、NH₄Al（SO₄）₂·12H₂O等有价值复盐,规避了传统石膏法产生的大量固废,有70%的铝离子被转变为矾盐晶体,同时带出大量的结晶水,减轻后续浓缩压力,对比传统的石膏法产生大量固废而言,其优点是显而易见的。碳化反应产品的XRD以及氧化锂含量分析表明,碳酸锂的纯度达到99%以上,全程锂收率为50%~60%。作为提锂实验对比,采用宜春414矿锂质量分数为4.0%的锂云母,由于414矿样中铝的相对含量更低,导致相同的除杂难度下得到的414矿样中浸出液锂离子浓度更高,浓缩倍数更小,414矿样的锂回收率更高。实验结果表明,中低品位锂瓷土提锂的工艺规律,通过适当改变参数,能够应用于难度更低的高品位的锂云母提锂过程。     

Stable Organic Titanium Catalysts and Reactive Distillation Used for the Transesterification of Dimethyl Carbonate with Phenol

The transesterification of dimethyl carbonate with phenol to methyl phenyl carbonate (MPC) was investigated on novel catalysts such as titanium diisopropoxide bis(ethyl acetoacetate) and titanium dibutoxide bis(ethyl acetoacetate) in a closed batch reactor at 185–206 °C under high pressure. The produced methanol could be removed efficiently by reactive distillation in order to overcome the equilibrium. The prepared catalysts have higher resistance to water than titanium alkoxides. Phenol conversion as high as 86.4 % with an MPC selectivity of 99.4 % was achieved under optimal reaction conditions within 9 h. Most of the catalytic activity was retained after repeated use for ten times.     

Superior lithium storage performance of hierarchical N-doped carbon encapsulated NaTi2(PO4)3 microflower

Na-superionic conductor (NASICON) structured NaTi₂(PO₄)₃ (NTP) as anode shows broad prospect in aqueous lithium ion battery. However, inherent low electrical conductivity of NaTi₂(PO₄)₃ remains a pivotal issue to be resolved. Herein, we report N-doped carbon encapsulated NaTi₂(PO₄)₃ microflower (NTP-CN) as anode for aqueous lithium ion battery, which is prepared via solvothermal way. NTP-CN with unique structural feature displays superb electrochemical performances. It delivers the discharge capacities of 131.2, 110.1, and 84.3 mAh g⁻¹ at 0.2, 3.0, and 15 C, respectively, 38.8, 33.8, and 51.1 mAh g⁻¹ higher than these of pristine NTP. NTP-CN also shows remarkable cycling stability at 6 C after 1000 cycles (capacity retention: 88.8%), superior to NTP (70.7%). The outstanding properties of NTP-CN may be due to that microflower structure can increase touching area between electrolyte and electrode, and carbon coating for electrode improves stability in aqueous electrolyte and ameliorates electrical conductivity. Moreover, nitrogen doping can further enhance hydrophilicity and conductivity of the sample, and also form lots of defects on electrode surface, which is beneficial for the intercalation/deintercalation of Li ions. This work reveals that the combination of microflower structure and N-doped carbon layer offers a promising method to improve electrochemical performances of NaTi₂(PO₄)₃.     

具有吸附作用的酸液缓速外加剂FL-1的研制

针对目前常规酸液缓速外加剂普遍存在泵入地层困难,二次伤害大等问题,从分子结构出发,合成了一种具有吸附作用的酸液缓速外加剂。采用CO2气体采集装置对外加剂延缓酸岩反应性能和缓速酸液的黏度进行了评价。结果表明,外加剂质量分数为0.5%时,缓速时间为140 min,酸液初始黏度为4.5 m Pa·s;酸岩反应过程中随着盐质量浓度和转子转速的逐渐增大,酸液缓速外加剂仍具有较好的缓速效果,并且外加剂与其他处理剂配伍性良好。     

多喷嘴气化工艺中灰水结垢分析及处理措施

针对安徽华谊化工公司气化炉灰水系统生产运行中存在的结垢问题,分析了不同位置灰垢的物理化学性质、主要成分及形成灰垢的灰水成分。根据不同位置的灰水结垢现象,推断出不同位置的结垢机理,据此采取:增加分散剂加药点、调整工艺操作、降低系统氨氮含量、定期射流清洗等处理措施,起到了良好的阻垢效果。     

离子液体体系卤水提锂的洗涤工艺研究

溶剂萃取法是盐湖提锂的重要工艺方法。采用磷酸三丁酯（TBP）/1-丁基-3-甲基咪唑双三氟甲基磺酰亚胺盐（[C₄mim][NTf₂]）离子液体体系对高镁锂比盐湖卤水中的锂进行萃取分离提取实验,对负载有机相的洗涤和反萃过程进行了研究。萃取实验：在TBP与[C₄mim][NTf₂]体积比为9∶1、相比（有机相与水相的体积比）为2∶1条件下,锂离子与其他离子的分离系数分别为β（锂/钠）=94.70、β（锂/钾）=148.85、β（锂/镁）=131.81。洗涤实验：系统考察了洗涤剂种类及浓度、相比、洗涤次数等因素对杂质离子洗脱率的影响,结果发现氯化锂和盐酸的混合溶液是从负载有机相中洗涤除去杂质离子的有效洗涤剂。洗涤过程适宜条件：洗涤剂中氯化锂浓度为4 mol/L、盐酸浓度为0.5 mol/L,相比为5∶1,洗涤次数为2次。反萃实验：用稀盐酸（1.0 mol/L）对负载有机相进行反萃取,在相比为1∶1条件下,单级反萃率达到97.81%。研究表明,离子液体体系作为一种新型萃取体系,在高镁锂比盐湖卤水中提取锂具有较好的应用前景。     

改性纳米碳酸钙用于硅酮胶挤出性研究

采用碳化法合成纳米碳酸钙,在反应过程中,调整反应起始温度合成不同晶型大小的纳米碳酸钙。通过透射电镜（TEM）、激光粒度仪对碳酸钙的物相、形貌、粒度进行分析,将改性纳米碳酸钙应用于硅酮胶基料制备及挤出性研究,分析改性纳米碳酸钙的颗粒大小、分散性、流变性能及表面改性剂对挤出性的影响。结果表明：粒径介于50~90 nm,屈服值介于66.4~148.9 Pa,黏度介于0.5~0.75 mPa·s,硬脂酸钠与LH-2、LH-3两种包覆剂进行复配改性的纳米碳酸钙用于硅酮胶基料具有较好的挤出性能。     

废旧锂电池正极材料回收技术研究进展

介绍了当前国内外三种车用锂电池正极材料的回收技术,包括火法冶金技术、湿法冶金技术和生物冶金技术。经过比较,以酸浸出—沉淀/萃取法为工艺流程的湿法技术对设备和能耗要求低、浸出效率高,是工业上方便引入的一种优异技术。     

锂离子在三维骨架复合锂金属负极中的沉积规律

锂金属具有极高的理论比容量和极低的氧化还原电极电势，成为了新一代高比能二次电池最理想的负极材料。然而，锂金属负极其走向大规模应用仍存在诸多问题与挑战。三维骨架复合负极可以控制金属锂均匀形核，低电流密度下均匀沉积，有望推动锂金属负极的实用化。为了更高效地指导锂金属负极设计和优化，采用相场理论，对三维骨架锂金属负极中比表面积对金属锂沉积过程的作用机制进行了定量分析和探究，发现了比表面积调控金属锂沉积的两阶段作用机理，并提出了基于比表面积参数的三维骨架负极设计与优化方向，从而最大程度发挥三维骨架在调控稳定金属锂负极上的积极作用。