以冰醋酸为介质制备低硫可膨胀石墨

以冰醋酸为介质，用酸性高锰酸钾作氧化剂制备低硫可膨胀石墨，筛选出制备的最佳条件，采用ＵＶ－Ｖｉｓ，ＸＲＤ等手段对石墨层间化合物予以分析。     

制备无硫可膨胀石墨的研究

用硝酸（65％）和乙酸酐混合液、高锰酸钾和天然鳞片石墨反应制备无硫可膨胀石墨,最佳反应条件是：石墨、乙酸酐、硝酸、高锰酸钾的重量比为1：0．8：0．5：0．07,反应时间为40min,反应温度为30℃,可膨胀石墨的膨胀容积为280mL／g;不含硫,含氮量为1．27％,其终端产品柔性石墨不含氮．迄今为止,未见文献报道．     

膨胀石墨的制备和影响其膨胀体积的因素

以硝酸为氧化剂,冰醋酸、甲酸为插层剂,采用化学氧化的方法制备可膨胀石墨.通过正交试验确定最佳工艺参数:10g鱼鳞片石墨,V(冰醋酸):V(甲酸):V(硝酸)=2:3:4,反应温度为20℃,反应时间为45min,制得可膨胀石墨在600℃时的膨胀体积为260mL/g;通过XRD分析检测插层剂,SEM观察膨胀石墨的表面形貌,测试结果表明,插层剂已插入石墨层间,形成石墨层间化合物,且膨胀石墨的表面形貌为疏松多孔结构.     

混酸法制备低硫可膨胀石墨

用硫酸（９８％）、硝酸（６５％）和草酸的混合液与天然鳞片石墨反 制备低硫可膨石墨，最佳反应条件是：石墨、硫酸（８％）、硝酸（６５％）、草的重量比为１：２．３：１．７：０．０５，反庆时间为４５ｍｉｎ，反应温度为２５℃，可膨胀石墨的含硫量为１．６３％时，膨胀容积为２５０ｍＬ／ｇ。其终端产品柔性石墨的含硫量为７８０ｐｐｍ。     

无硫高倍膨胀石墨的制备及影响因素探讨

以鳞片石墨、硝酸、乙酸酐、高锰酸钾为原料，采用化学法经氧化酸化插层、水洗、干燥、高温膨胀过程制备膨胀石墨，利用正交试验方法确定最佳工艺条件，并对相关影响因素及插层机理作了初步探讨。结果表明：按鳞片石墨：硝酸：乙酸酐：高锰酸钾(质量比)=1：0．7：1．5：0．4，反应时间90min，反应温度30℃～40℃的条件可以制备出膨胀体积达478mL/g的高倍无硫膨胀石墨。相关影响因素的大小依次为：高锰酸钾、硝酸、乙酸酐、反应时间，其中高锰酸钾的影响程度远大于其他三个因素。     

混酸法制备无硫可膨胀石墨的研究

首次用浓硝酸、乙酸、高锰酸钾和天然鳞片石墨反应制备无硫可膨胀石墨. 筛选出制备的最佳条件, 采用质谱法对该种无硫可膨胀石墨进行了分析.     

制备低硫可膨胀石墨的新方法

研究了一种以冰醋酸为反应介质,在少量浓Ｈ２ＳＯ４存在下,以重铬酸钾作为氧化剂制备低硫可膨胀石墨的新方法。在最佳制备条件下,可膨胀石墨产品的含硫量仅为０．６８％,膨胀石墨产品的含硫量为０．０８％,膨胀容积２６０ｍＬ·ｇ－１,水分０．１０５％,挥发分５．５％,灰分０．７６％,ｐＨ值５,并采用紫外分光光度计对产品进行了分析。     

爆轰裂解可膨胀石墨制备石墨微粉

在不改变石墨原始结构与成分的基础上,利用冲击波对可膨胀石墨进行爆轰,收集爆轰灰,进行X射线衍射、SEM的测量分析以及BET法测定比表面积。结果表明,可膨胀石墨经过爆轰后,得到了颗粒大小为1μm～10μm的石墨粉,比表面积由8.096m^2/g增大至47.48m^2/g,并且孔隙变得更为均匀,常规研磨设备是无法达到这种效果的。为石墨的细化提供了一种更为简便快捷而又节省能源的方法。     

制备低硫可膨胀石墨的研究

研究了以过二硫酸铵作氧化剂低硫可膨胀石墨的制备，找到了在较低温度下，制备低硫可膨胀石墨的最佳条件。即过二硫酸铵和石墨的重量比为１５％；反应温度为５５℃；反应时间为４０ｍｉｎ；硫酸浓度为９８％；硫酸与石墨的重量比为４∶１，草酸和硝酸（浓度为６５％）的重量比为７．５％时，所制得的可膨胀石墨含硫量为０．６５％，膨胀容积为２００ｍＬ／ｇ可膨胀石墨。并且，其终端产品柔性石墨具有优良的力学性能和抗氧化性能。     

化学氧化法制备可膨胀石墨过程中的电位控制

以高锰酸钾、硫酸、天然鳞片石墨为原料,采用化学氧化法制备可膨胀石墨。通过调控体系初始氧化还原电位,并结合其膨胀容积值,探讨石墨氧化的最佳电位区间,采用扫描电镜及X射线衍射仪对样品进行表征。结果表明,当体系初始氧化还原电位为1340~1810mV时,能够获得平均膨胀容积大于230mL/g,最高300mL/g的可膨胀石墨,扫描电镜及X射线衍射结果证实了此区间的合理性。此法避免了传统化学氧化法通过复杂正交实验来确定最佳工艺的弊端,可为实现可膨胀石墨制备的自动化和工业化生产提供重要的理论依据。     

Lattice images of carbon fibres treated with intercalating agents

Carbon fibres were treated with nitrogen dioxide, bromine, and hydrazine to determine whether any changes in the arrangement of the carbon layer planes could be observed. A statistical analysis of lattice image photographs showed small increases in crystallite width (most notable with hydrazine) and also in the apparent length. This is consistent with previous suggestions that intercalation produces ordering by means of dislocation movement during changes in the graphite stacking mode.     

Preparation of high silica microporous zeolite SSZ-13 using solid waste silica fume as silica source

Silica fume (SF) is a kind of solid waste that produced in the process of industrial silicon smelting. The disposal of SF for environmental problem is of great urgency. Here, a facile and novel one-step approach of high silica microporous materials SSZ-13 (SF-SSZ-13) were hydrothermally synthesized using silica fume (SF) as silica source. This method requires significantly shorter reaction times (48?h) compared to conventional SSZ-13. The as-synthesized SF-SSZ-13 exhibited high purity structure, popcorn-like morphology, and a large BET surface area of 545.74?m²?g^?1. Additionally, on the basis of controlled growth under different hydrothermal times, the formation mechanism of the SF-SSZ-13 outlined for further extension to other materials. The results on time- and energy-efficient of SF-based preparation of SSZ-13 pave the way for the reducing the cost of production of raw materials and decreasing environment load of solid waste, and also extend the application of silica fume.     

Decontamination of liquid radioactive waste concentrates from 60Co using diethyldithiocarbamates

Oxidized bottom residue (BR) from installations for reprocessing trap waters of the Leningrad NPP were treated to remove ⁶⁰Co by coprecipitation with transition metal diethyldithiocarbamates (DDTC). Coprecipitation of ⁶⁰Co with manganese and cobalt diethyldithiocarbamates was examined in relation to pH of solution, temperature, amount of diethyldithiocarbamates, reagent ratio, and number of coprecipitation steps. The effect of diethyldithiocarbamates on the efficiency and conditions of the solution decontamination from ^134,137Cs on nickel potassium ferrocyanides was studied. Oxidative treatment of liquid radioactive waste concentrates to break down organic complexes is a necessary condition for ⁶⁰Co removal by coprecipitation with transition metal diethyldithiocarbamates. From a solution initially containing 56 kBq dm^{−3 60}Co, ⁶⁰Co can be removed to a residual content of 0.12–0.16 kBq dm⁻³ by two-step coprecipitation with Co(DDTC)₂. The coprecipitation with Co(DDTC)₂ does not affect the efficiency of the subsequent removal of Cs radionuclides on nickel potassium ferrocyanides.     

用柔性石墨制备低密度膨胀石墨块

通过在浓硫酸或浓硝酸中浸泡柔性石墨纸（板），然后在200℃～750℃膨化制备了低密度膨胀石墨块。研究了插层剂、插层时间和膨化温度对膨胀石墨块体积密度和外形完整程度的影响。结果表明：膨化温度越高，制得的膨胀石墨块密度越低，越难获得完整的外形。以浓硫酸或浓硝酸插层时，适宜的膨化温度分别约为550℃和650℃，插层时间应为3h以上。发现膨胀石墨块主要存在两种外观，一种为均匀膨胀，另一种为非均匀膨胀。     

Low-temperature immobilization of liquid radioactive waste using silica from concentrated hydrothermal solutions

Experiments on vitrification of simulated liquid radioactive waste (LRW) were performed. To obtain solid glass-like phases, LRW components were treated with aqueous-alcoholic hydrochloric acid solutions containing hydrolyzates of alkyl silicates and aqueous silica sols obtained by membrane concentration of a natural hydrothermal solution. The pH of the mixture was 1.5–4. The characteristics of the solid samples obtained were studied by X-ray phase analysis, thermogravimetry, and scanning electron microscopy. A procedure was developed for low-temperature (5–60°C) immobilizaiton of low-level LRW using aqueous silica sols.     

Mapping of the atomic lattice orientation of a graphite flake using macroscopic liquid crystal texture

The electronic properties of graphene depend critically on its lattice orientation and edge type. However, it is very difficult to identify them, and they are accessible only using sophisticated tools. In this paper, we show an easy and reliable way to reveal the lattice orientation and edge type of graphene and graphite flakes, i.e.?multi-layered graphene. Nematic liquid crystals have the potential to align themselves into three symmetric and equivalent orientations on crystalline graphite. The director of macroscopic texture due to the elasticity indicates the lattice orientation of the top graphite layer. By analyzing the director orientation using a polarizing optical microscope, we were able to show the lattice orientation, chiral angle and edge type of graphene and graphite flakes on the macroscopic scale. As liquid crystals are soft and easily removable, our technique has little chance of influencing the following processes for graphene manipulation.     

Preparation and properties of polystyrene nanocomposites with graphite oxide and graphene as flame retardants

In this study, graphite oxides (GOs) with different oxidation degrees and graphene nanosheets were prepared by a modified Hummers method and thermal exfoliation of the prepared GO, respectively. Polystyrene (PS)/GO and PS/graphene nanocomposites were prepared via melt blending. X-ray diffraction results showed that GOs and graphene were exfoliated in the PS composites. It could be observed from the scanning electron microscope images that GOs and graphene were well dispersed throughout the matrix without obvious aggregates. Dynamic mechanical thermal analysis suggested that the storage modulus for the PS/GO1 and PS/graphene nanocomposites was efficiently improved due to the low oxygen content of GO1 and the elimination of the oxygen groups from GO. The flammability of nanocomposites was evaluated by thermal gravimetric analysis and cone calorimetry. The results suggested that both the thermal stability and the reduction in peak heat release rate (PHRR) decreased with the increasing of the oxygen groups in GOs or graphene. The optimal flammability was obtained with the graphene (5 wt%), in which case the reduction in the PHRR is almost 50 % as compared to PS.     

Preparation and characterization of low-temperature expandable graphite

The low-temperature expandable graphite was successfully prepared with perchloric acid, phosphoric acid and KMnO₄ by chemical process. The optimum weight ratio of perchloric acid to phosphoric acid in mixed acid was 1:0.2, and the weight ratio of the mixed acid, KMnO₄ and natural flake graphite was preferably 1.5:0.1:1. The expanded volume can reach 260 mL/g at a relatively low temperature of 300 °C. Meanwhile, the prepared samples were characterized by means of Fourier transform infrared, thermogravimetry-differential scanning calorimetry and X-ray diffraction.     

Heavy metal stabilization in municipal solid waste incineration flyash using heavy metal chelating agents

Heavy metal chemical stabilization with synthesized heavy metal chelating agent was assessed for flyash from municipal solid waste incinerator. Flyash can contain heavy metals (e.g. Pb, Cd) which can leach. A new kind of heavy metal chelating agent showed more attractive competition than inorganic chemicals in stabilizing flyash. The synthesizing method of this kind of heavy metal chelating agent was explained in this paper, and the technology process and treatment efficiency of the chelating agent in treating flyash were experimentally studied, which was compared with the results of inorganic chemical agents such as sodium sulfide and lime. The heavy metals in flyash were stabilized more effectively by using heavy metal chelating agents than by using sodium sulfide and lime, furthermore, the stabilized products using the chelating agents can meet the landfill disposal controlling standards for heavy metal waste. pH-dependent leaching experiment showed the stabilized flyash by treatment with heavy metal chelating agent could keep long-term stabilization within a broad range of pH value. Thus, the risk of secondary pollution for the stabilized products was reduced dramatically when the environment condition changes during its disposal period.     

Removal of U(VI) from simulated liquid waste using synthetic organic resin

Poly(acrylic acid–dimethylaminoethyl methacrylate) was prepared by γ-radiation-induced copolymerization at a radiation dose of 60 kGy and a dose rate of 1.25 kGy h^–1. The resin obtained was used to remove U(VI) from simulated solution of the waste from the Fuel Manufacturing Pilot Plant (FMPP). A preliminary test of U(VI) adsorption onto the resin showed high affinity of this resin for U(VI) ions. The adsorption behavior toward the U(VI) ions was studied in relation to the contact time, pH, temperature, resin dosage, and initial concentration of metal ions. The adsorption isotherms of uranium onto the resin were described using the Langmuir and Freundlich models, with the Langmuir model being more adequate to the experimental equilibrium data. Without foreign ions, the maximum adsorption capacity of the resin for U(VI) was 105.7 mg g^–1. X-ray fluorescence was used to evaluate the amount of U(VI) ions on the resin sample before and after the adsorption.