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废锂离子电池石墨负极综合回收利用研究进展

矿冶工程 2024年第4期44卷 120-125页

作者：赵朝显肖劲诸向东仲奇凡中南大学冶金与环境学院湖南长沙410083 中南大学低碳有色冶金国家工程研究中心湖南长沙410083

综述了废锂离子电池石墨负极的综合回收利用技术,包括湿法、火法-湿法联合以及物理法回收工艺,并对各工艺的优缺点进行了深入分析。特别指出,尽管目前存在多种回收技术,但高效、环保的闭环回收工艺仍面临挑战。探讨了废石墨负极材料的... 详细信息

综述了废锂离子电池石墨负极的综合回收利用技术,包括湿法、火法-湿法联合以及物理法回收工艺,并对各工艺的优缺点进行了深入分析。特别指出,尽管目前存在多种回收技术,但高效、环保的闭环回收工艺仍面临挑战。探讨了废石墨负极材料的资源化再利用途径,如作为二次电池负极材料、制备石墨烯等,并对未来研究方向进行了展望,旨在为废锂离子电池石墨负极的高值化利用提供理论支持和技术支持。建议未来的研究关注开发简单、高效、清洁的闭环回收工艺,提高石墨负极材料的回收率和纯度,同时减少环境污染。未来研究的热点应包括石墨负极材料的晶格重构修复技术,以及探索石墨负极材料在储能材料、催化剂、吸附剂等领域的新应用。

关键词：废锂离子电池石墨负极综合回收资源化再利用环境效益

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煅烧温度对煅后石油焦微观结构演变的影响

中国有色冶金 2024年第1期53卷 8-16页

作者：犹子涵肖劲于谱生周宇甘小双仲奇凡中南大学冶金与坏境学院湖南长沙410083 济南澳海炭素有限公司山东济南250101

煅后石油焦是铝电解用炭阳极等冶金炭素材料的主要原料,现有研究缺乏对不同煅烧温度下煅后焦微观结构演变的深入探索,导致冶金炭素材料的制备难以智能调控,降耗困难。针对上述问题,本文利用一种基于高分辨适射电镜(HRTEM)检测的碳材料... 详细信息

煅后石油焦是铝电解用炭阳极等冶金炭素材料的主要原料,现有研究缺乏对不同煅烧温度下煅后焦微观结构演变的深入探索,导致冶金炭素材料的制备难以智能调控,降耗困难。针对上述问题,本文利用一种基于高分辨适射电镜(HRTEM)检测的碳材料晶格条纹智能提取技术,结合数学拟合对不同煅烧温度下煅后焦微观结构的演变规律进行了深入探究。结果表明,煅后焦的平均晶格条纹长度、堆叠占比和45°集中分布的特征值在600℃以下会随温度升高而轻微劣化,而在600~1 600℃的温度范围内,各项微观结构特征值的变化规律符合Sigmoid函数模型,随着温度升高先迅速提升后平缓增加;利用拟合曲线的推导公式求得煅后焦各项微观结构特征的有效升温区间,进一步得到煅后焦微观结构特征随温度变化而演变的优先级为晶格取向>晶格堆叠>晶格尺寸生长;通过拉曼光谱分析得到煅后焦的石墨化度R值在25~1 600℃的温度范围内由0.86变化到0.59,石墨化度在不同温度下的变化规律映证了上述各项微观结构特征演变分析的结果。

关键词：冶金炭素煅后焦晶格条纹微观结构演变铝电解炭阳极煅烧

Wet Desulfurization of High-Sulfur Petroleum Coke Improved via Pre-calcination,H_(2)O_(2) Treatment,and Ultrasound

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China Petroleum Processing & Petrochemical Technology 2022年第2期24卷 34-45页

作者： Wang Gang Mao Qiuyun Liu Wei Yu Zhou zhong qifan School of Metallurgy and Environment Central South UniversityChangsha 410083China Department of Educational Science Hunan First Normal UniversityChangsha 410205China

This work reports an improved method for the wet desulfurization of high-sulfur petroleum coke(petcoke)powder based on the combination of pre-calcination,H_(2)O_(2),and *** results demonstrated that over 45%of the sulfur atoms were efficiently removed from Tianjin coke and Qilu coke(particle size<0.1 mm)by pre-calcination at 800℃ for 6 h followed by desulfurization with HNO3(8 mol/L)and H_(2)O_(2)(2 mol/L)solution at a reaction temperature of 60℃,a reaction time of 6 h,a liquid-to-solid ratio of 10 mL/g,and a 40 kHz ultrasonic power of 400 *** addition,the specific surface area of the petcoke particles increased from 0.7 to 301.49 m^(2)/*** desulfurization,the pore size distribution of the petcoke particles was more concentrated on micropores compared with the samples prior to petcoke *** force field molecular dynamics simulation results indicated that HNO_(3) continuously oxidized the carbon atoms adjacent to sulfur atoms in the petcoke macromolecules and promoted sulfur removal from petcoke via the cleavage of C-S *** sulfur transformation mechanism can be summarized as follows:thiophene sulfur→branched chain carbon sulfur→CO_(2)S→C_(2)O_(2)S→C_(2)O_(3)NS→C_(2)O_(4)S→CO_(2)S.

关键词： sulfur removal ultrasonic petcoke thiophene ReaxFF

Desulfurization of Petroleum Coke by Calcination in Ammonia Atmosphere below 1000℃

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China Petroleum Processing & Petrochemical Technology 2016年第4期18卷 41-50页

作者： zhong qifan Xiao Jin Huang Jindi Yuan Jie Yu Bailie school of metallurgy and environment central south universityChangsha410083 national engineering laboratory of efficient utilization of refractory nonferrous metal resources central south universityChangsha410083

The desulfurization efficiency and mechanism of the calcination of petroleum coke in ammonia atmosphere at lower than 1000 ℃ were investigated through a series of conditional experiments and comparison with other gases such as H_2. The topics of efficiency and reaction mechanism are usually discussed through investigation by means of the Fourier transform infrared spectroscopy(FT-IR), the Brunauer-Emmett-Teller(BET) technique, and the thermogravimetry coupled with the mass spectrometry(TG-MS). Results showed that in addition to H_2, ammonia not only could retain a high desulfurization rate but could also reduce coke loss during the desulfurization process of petroleum coke. The best desulfurization conditions covered a petroleum coke particle size of less than 0.1 mm, a calcination temperature of 800 ℃ in ammonia atmosphere with a flow rate of 10 L/h, and a heating duration of more than 120 min. Ammonia decomposition, H_2 generation, decline in the activation energy of the carbon–sulfur bonds, and petroleum coke with a largest specific surface area at 800 ℃ are the key goals of desulfurization studied thereby. As proved by TG-MS analysis, given a large quantity of H_2, ammonia can be decomposed at the same temperature to completely come into contact with the sulfur species in petroleum coke to generate H_2S.

关键词： desulfurization petroleum coke ammonia calcination TG-MS

Integrated UV-based photo microreactor-distillation technology toward process intensification of continuous ultra-high-purity electronic-grade silicon tetrachloride manufacture

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Chinese Journal of Chemical Engineering 2020年第9期28卷 2248-2255页

作者： Ye Wan Wenhui Guo Jin Xiao Dazhou Yan Xiong Zhao Shuhu Guo Jianhua Liu qifan zhong Tao Yang Yu Zhao Xin Chang Xin Gao School of Metallurgy and Environment Central South UniversityChangsha 410083China China ENFI Engineering Co. Ltd.Beijing 100038China National Engineering Laboratory of Polysilicon Materials Preparation Technology Luoyang 471023China National Engineering Laboratory of Efficient Utilization of Refractory Nonferrous Metal Resources Central South UniversityChangsha 410083China School of Chemical Engineering and Technology Tianjin UniversityTianjin 300072China

Ultra-high-purity silicon tetrachloride(SiCl4)is demanded as an electronic-grade chemical to meet the stringent requirements of the rapidly developing semiconductor *** high requirement for ultra-high-purity SiCl4 has created the need for a high-efficient process for reducing energy consumption as well as satisfying product *** this paper,a mass of production technology of ultra-high-purity SiCl4 was successfully developed through chlorination reaction in the ultraviolet(UV)-based photo microreactor coupled with the distillation *** influences of key operational parameters,including temperature,pressure,UV wavelength and light intensity on the product quality,especially for hydrogen-containing impurities,were quantified by the infrared transmittance of Fourier transform infrared spectroscopy(FT-IR)at 2185 cm^-1and 2160 cm^-1indicating that chara cteristic vib rational modes of Si-H bonds,as well as the operating conditions of distillation were also investigated as key factors for metal impurities *** advanced intensification of SiCl4 manufactured by the integration of photo microreactor and distillation achieves the products with superior specifications higher than the standard commercial products.

关键词： SiCl4 Process intensification Photochlorination Microreactor Distillation

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酸碱脱灰对煤结构及其热解特性的影响

中南大学学报（自然科学版） 2016年第1期47卷 14-19页

作者：肖劲李发闯邓松云仲奇凡赖延清李劼中南大学冶金与环境学院湖南长沙410083

通过酸碱脱灰制备超纯煤,运用X线衍射(XRD)、拉曼光谱(Raman)、红外光谱(FTIR)和热重(TG/DTG)等分析技术研究酸碱脱灰对煤结构和热解特性的影响。研究结果表明:酸碱脱灰达到很好的脱灰效果,煤样灰分质量分数降低到0.5%以下;脱灰处理破... 详细信息

通过酸碱脱灰制备超纯煤,运用X线衍射(XRD)、拉曼光谱(Raman)、红外光谱(FTIR)和热重(TG/DTG)等分析技术研究酸碱脱灰对煤结构和热解特性的影响。研究结果表明:酸碱脱灰达到很好的脱灰效果,煤样灰分质量分数降低到0.5%以下;脱灰处理破坏煤中碳微晶结构,使煤中分子结构有序性减弱;脱灰煤中羟基和甲基、亚甲基脂肪烃类官能团含量减少,Si—O—Si和Si—O基团消失,酚、醚类含氧官能团含量显著增加;脱灰对低阶煤的分子结构影响较大;在热解过程中,脱灰煤的初始分解温度(ts)和最大质量损失温度(tmax)均向低温区推移;灰分脱除降低传质传热的势垒,有助于促进热解反应。

关键词：脱灰结构含氧基团热解特性

硫对焦空气反应性的影响及钙硫的相互抑制作用与机理

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中南大学学报（自然科学版） 2015年第10期46卷 3603-3610页

作者：肖劲仲奇凡邓松云赖延清李劼刘业翔中南大学冶金与环境学院湖南长沙410083

以二苯并噻吩、硫酸铵和稀硫酸为硫添加剂,以多种含钙化合物为钙添加剂对低杂质沥青进行掺杂,在550℃和1 100℃下制备含Ca,S杂质的半焦前驱体和沥青焦,研究空气反应中S对焦反应性的影响以及Ca与S之间的相互作用关系,并结合扫描电镜(SEM... 详细信息

以二苯并噻吩、硫酸铵和稀硫酸为硫添加剂,以多种含钙化合物为钙添加剂对低杂质沥青进行掺杂,在550℃和1 100℃下制备含Ca,S杂质的半焦前驱体和沥青焦,研究空气反应中S对焦反应性的影响以及Ca与S之间的相互作用关系,并结合扫描电镜(SEM)和能谱(EDS)对其中的机理进行了探讨。研究结果表明:有机S对焦的空气反应性具有比Ca更强的催化作用,但当S和Ca同时存在于沥青焦中时,它们却会对彼此的催化作用表现出一种很强的相互抑制效果;S的催化机理极有可能是因为它在焦的表面上形成一个可直接增加焦的消耗并具有放热特性的循环反应体系;Ca与S之所以能够相互抑制很可能是因为它们生成相对稳定的Ca SO4并通过其引发的一系列反应破坏了S的催化性循环反应体系平衡。

关键词：焦空气反应性硫杂质钙杂质作用机理

Fabrication and characterization of 3D printed biocomposite scaffolds based on PCL and zirconia nanoparticles

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Bio-Design and Manufacturing 2021年第1期4卷 60-71页

作者： qifan Wang Zhiyong Ma Ying Wang Linna zhong Wenjia Xie College of Mechanical Engineering and Mechanics Ningbo UniversityNingbo 315211ZhejiangPeople’s Republic of China School of Engineering Huzhou UniversityHuzhou 313000ZhejiangPeople’s Republic of China Huzhou Aixiante Electronic Technology co. LTD.Huzhou 313000ZhejiangPeople’s Republic of China Department of Prosthodontics West China Hospital of StomatologySichuan UniversityChengdu 610000SichuanPeople’s Republic of China

The application of three-dimensional printed polymer scaffolds in repairing bone defects is a promising *** them,polycaprolactone(PCL)scaffolds are widely studied due to their good processability and controlled degradation ***,as an alternative graft for repairing bone defects,PCL materials have poor hydrophilicity,which is not conducive to cell adhesion and *** addition,the poor mechanical properties of PCL materials cannot meet the strength required to repair bone *** this paper,nano-zirconium dioxide(ZrO2)powder is embedded in PCL material through a meltmixing process,and a regular grid scaffold is constructed by 3D *** embedding of nanometer zirconium dioxide powder improves the hydrophilicity and water absorption of the composite scaffold,which is conducive to cell adhesion,proliferation and growth and is beneficial to the exchange of ***,the PCL/ZrO2 composite scaffold showed better biological activity in *** the same time,the PCL/ZrO2 composite material system significantly improves the mechanical properties of the *** them,compared with the pure PCL scaffold,the Young’s modulus is increased by about 0.4 times,and the compressive strength is increased by about 0.5 *** addition,the osteogenic differentiation results also showed that the PCL/ZrO2 composite scaffold group showed better ALP activity and more effective bone mineralization than the pure PCL *** believe that the 3D printed PCL/ZrO2 composite scaffold has certain application prospects in repairing bone defects.

关键词： 3D printing Bone tissue engineering Biocomposite scaffold Zirconium dioxide Hydrophilicity

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电子特气六氯乙硅烷产品金属杂质检测方法

中南大学学报（自然科学版） 2020年第12期51卷 3341-3348页

作者：万烨肖劲严大洲张园园仲奇凡刘芳洋中南大学冶金与环境学院湖南长沙410083 中国恩菲工程技术有限公司北京100038 多晶硅材料制备技术国家工程实验室河南洛阳471023 难冶有色金属资源高效利用国家工程实验室湖南长沙410083

六氯乙硅烷作为高品质氮化硅和氧化硅薄膜的硅源前驱体,主要用于DRAM和NAND Flash存储器的制造以及特征尺寸28 nm以下逻辑芯片的制备,在半导体制造中已被广泛应用。目前国内采用六氯乙硅烷生产技术已制备集成电路,但其十亿分之一量级的... 详细信息

六氯乙硅烷作为高品质氮化硅和氧化硅薄膜的硅源前驱体,主要用于DRAM和NAND Flash存储器的制造以及特征尺寸28 nm以下逻辑芯片的制备,在半导体制造中已被广泛应用。目前国内采用六氯乙硅烷生产技术已制备集成电路,但其十亿分之一量级的超痕量金属杂质检测是国内的检测技术瓶颈,也是国外技术封锁的项目之一。为此,研究六氯乙硅烷的水解过程产生的微颗粒吸附固化金属杂质的机理,采用氢氟酸消解产生的SiF4的强挥发性,以消除硅基效应导致的基体干扰。在此基础上,建立六氯乙硅烷中Li,Na,Mg,Al,K,Ca,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,As和Pb共18种金属杂质的电感耦合等离子体质谱(ICP-MS)检测方法,并确定质谱激发模式和最优仪器参数。研究结果表明:采用这种消解方法可以获得较好的检测效果:标准曲线线性相关系数大于0.999,各元素检出限低于0.10 ng/g,加标回收率为80%~110%,方法精密度小于10%。对比酸雾消解法和直接消解法对硅基体的消解效果,发现酸雾消解法作为样品前处理方式更加安全、洁净、准确和高效。精密度和准确度符合超痕量杂质检测方法的规定,再现性满足用户要求,适用于六氯乙硅烷中金属杂质的检测,其他高纯度氯硅烷的杂质测试亦可参照使用。

关键词：六氯乙硅烷 ICP-MS 金属杂质酸雾消解