Synthesis, characterization, and property test of crystalline polyferric sulfate adsorbent used in treatment of contaminated water with a high As(Ⅲ) content

A crystalline polyferric sulfate(PFS) adsorbent was synthesized by oxidizing and precipitating ferrous ions in air atmospheric conditions. The morphology, structure, specific surface area(SSA), and adsorptive efficacy of the adsorbent to As(Ⅲ) were characterized by scanning electron microscope(SEM) and transmission electron microscopy(TEM) images, X-ray diffraction(XRD) patterns, Fourier-transform infrared(FTIR) spectra, BET SSA analyses, and adsorption experiments. The adsorbent showed a near-spherical aggregate structure and had good crystallinity. A significant amount of α-goethite co-precipitated with PFS in the case of the initial ferrous concentration of 1 mol/L and increased SSA of the adsorbent. The stability region of ferric compounds in the process was drawn and applied to analyze the iron behavior during the synthesis. The adsorption of As(Ⅲ) in high As(Ⅲ)-containing solutions fitted the Langmuir isotherm model adequately. The absorbent with co-precipitation of α-goethite showed good adsorbability for As(Ⅲ) and good filtering performance in the high As(Ⅲ)-containing solution of 10–100 mg/L under acidic, neutral, and alkaline conditions(pH 2.09–9.01). After the adsorption process, the stability of the residues bearing As(Ⅲ) was evaluated by toxic characteristic leaching procedure(TCLP) tests. The results indicated that the residues were extremely stable, and the concentrations of arsenic in the leaching solutions were less than 0.01 mg/L.

Enantioseparation of Aminoglutethimide by High-speed Countercurrent Chromatography Using Carboxymethly-β-cyclodextrin as Chiral Selector

Enantioseparation of aminoglutethimide was performed by high-speed counter-current chromatography with a two-phase system composed of ethyl acetate： methanol： water = 10： 1： 9. The lower phase contained 20 mmol/L of carboxymethly-β-cyclodextrin as chiral selector. The enantiomers were separated in 1.2 h and identified by chiral HPLC. This method was very efficient for the chiral preparative separation.

SULFATE RESISTANCE MECHANISM OF HIGH- PERFORMANCE CONCRETE CONTAINING NCI

It is found that the incorporation of Nitrite Corrosion Inhibitor (NCI) greatly weakens the resistance of mixtures to sulfate attack. To study the mechanism of this phenomenon, in this paper, the influence of NCI addition on the cement paste and microstructure change of high performance concrete specimens is studied by means of quantitative XRD, SEM tests. The results demonstrate that the incorporation of NCI accelerates the formation of calcium hydroxide and ettringite crystals, and weakens the pore refinement effect caused by the secondary hydration reaction of fly ash and microsilica. At the age up to one year, the relative crystal quantity in mixture containing NCI is always higher than that in control mixture. The reasons for the degradation in sulfate resistance of mixtures may be attributed to the increase and stability of the calcium hydroxide and ettringite crystals formed and the weakening of secondary hydration reaction. Based on the results, conclusion can be drawn that NCI should be used cautiously in practical engineering where high resistance to sulfate attack is required. (Author abstract) 7 Refs.

Preparation of High Percentage α-Calcium Sulfate Hemihydrate via a Hydrothermal Method

α-calcium sulfate hemihydrate (α-HH) is known to be suitable for application as bone void filler. High percentage of α-HH is obviously needed for medical applications, especially for implantation. Three commercially available calcium sulfate dihydrates (DH, CaSO4·2H2O) with different sizes and surface morphologies were used as starting materials to synthesize high percentage α-HH via a hydrothermal method. The median particle sizes of the three types of DH were 946.7 μm, 162.4 μm and 62.4 μm, respectively. They were named as DH-L, DH-M and DH-S in this paper. The particle size distribution, morphology and phase composition of the raw materials were evaluated before synthesis. SEM results revealed that DH-L consisted of irregular large particles, while DH-M and DH-S were composed of plate-like particles with some small ones. High percentage HH can be obtained with proper synthesis parameters by hydrothermal method, specifically, 105 °C/90 min for DH-L (achieving 98.8% HH), 105°C/30 min for DH-M (achieving 96.7% HH) and 100°C/45 min for DH-S (achieving 98.4% HH). All the synthesized HH were hexagonal columns, demonstrating that they were α-phase HH. The particle size and morphology of starting material (DH) have significant influences on not only the rate of phase transition but also the morphology of the synthesized α-HH. Calcium sulfate dihydrate cements were prepared by the synthesized α-HH. The highest compressive strength of calcium sulfate dihydrate cement was 17.2 MPa. The results show that the preparation of high percentage α-HH is feasible via a hydrothermal method and the process can be further scaled up to industrial scale production.

Research on Preparation and Influencing Fctors of High Calcium High Sulfate Ash to Autoclaved Aerated Concrete

In this paper, a high calcium high sulfate ash as the main material, adding fly ash, lime, cement, gypsum and some modifiers to prepare autoclaved aerated concrete. The products complies with the technical requirements of GB/T11968-2006. This paper also studies the influence of the physical methods and water ratio on autoclaved aerated concrete by high calcium high sulfate ash aerated concrete. The best ratio of water and Grinding time were found in practice study.

Preparation and Application of Polymer Silicate Phosphate Ferric Sulfate Used in High-Viscosity Oil Refining Wastewater Treatment

A new kind of flocculants, named Polymer Silicate Phosphate Ferric Sulfate(PSPFS), was synthesized by ferrous sulfate used as the main material and activated silicic acid as additive. In this paper, High-Viscosity Oil Refining wastewater from Liaohe Petrochemical Corporation was the treatment object. Overall, the in-fluencing factors and synthesis technology conditions of PSPFS were determined by experiments. First of all, the conditions of influencing factors were showed as follows: the mass percent concentration of ferrous sulfate 55%,concentration of sodium silicate 15% , the molar ratio of ferrous sulfate and hydrogen peroxide 1.2:1, oxidation temperature 40 degree Celsius, oxidation time 4 hours, polymerization temperature 60 de-gree Celsius and polymerization time 2 hours. Secondly, the optimal ratios of components were determined by uniform design method. The molar ratio of Fe/Si is 5.0:1, Fe/H2SO4 is 3.2:1, and Fe/P is 18.0:1. At last, the optimal experimental condition was determined as follows: the dosing quantity 200mg/L, pH value 5.5~9, temperature 25~45℃, stirring time 2 min, and standing time 3 min, according to the result of floc-culation experiments with PSPFS. Besides, the result of the comparative experiments showed that the effi-ciency of PSPFS was much better than the reference flocculants.

Development of a High Early Strength Non-fuorine and Non-alkaline Flash Setting Admixture and Flash Mechanism

To solve the problems of high rebound rate and strength reversion of shotcrete,a non-fluorine and non-alkaline liquid flash setting admixture(FSN)with low rebound and high early strength was synthesized under 60-65℃water bath environment through orthogonal test design and taking setting time and compressive strength as indicators.The experimental results show that the optimum mass ratio of FSN is aluminum sulfate:diethanolamine:triethanolamine:pseudo-boehmite:lithium carbonate:water=57%:8%:0.05%:2%:2%:31%.When FSN is added with 7%of the mass of portland cement,the cement paste can be initially set in 3 min and finally set in 5 min.The compressive strength of mortar is 1.2 MPa at 6 h,18.0 MPa at 1 d,and more than 100%at 28 days;The microscopic analysis shows that the rapid release of Li^(+),NH^(4+),and CO_(3)^(2-)ions by FSN in the paste solution effectively shortens the induction period of high C_(3)S content in Portland cement,directly forms early coagulation AFt crystals in FSN and CH dominated by Al_(2)(SO_(4))_(3),and forms a large number of C-S-H gels in the later stage,so that the cement can quickly coagulate and harden,and the strength in the later stage is not retracted.

On the enhanced properties of composite asphalt via adding surface modified calcium sulfate whisker-SBR

With the aim of improving the durability and safety,erosion time,and cost-effective of asphalt road,a composite of modified calcium sulfate whisker-styrene butadiene rubber modified asphalt(MCSWSBRMA)was prepared via thermal doping.Firstly,stearic acid and titanate coupling agent(NDZ-201)were used as a modifier to transform calcium sulfate whisker(CSW)into MCSW via wet modification method at 60℃and anhydrous ethanol as a dispersant.What is more,the optimum loading of modifier(a mixture of 25%stearic acid+75%NDZ-201)was found to be at 2%to prepare MCSW.Subsequently,a composite of MCSW-SBRMA was prepared with different loading of MCSW(i.e.2%to 8%)to enhance the softening point of asphalt.In this study,it was found that 4%of modifiers was the best composition to improve the MCSW-SBRMA properties as elucidated in the orthogonal experiment table L_(16)(42).The effects of MCSW and SBR addition on several properties of asphalt were studied by multiple routine tests including penetration,segregation test,and so on.The results show that:2%to 8%MCSW can increase the softening point of SBR modified asphalt(SBRMA)by 7%to 8%.4%MCSW increased the PG of SBRMA from 64 to 70,which greatly improved the high temperature characteristics of asphalt.The 5℃ductility of MCSW-SBRMA is greater than 100 cm,which greatly improves the low temperature performance of asphalt.Through the application of fluorescence microscopy(FM),Fourier transform infrared spectroscopy(FTIR),Scanning electron microscopy(SEM),and energy dispersive spectroscopy(SEM-EDS),it has been demonstrated that MCSW-SBR effectively alters asphalt in a highly uniform manner,with some MCSW still retaining large cross sections,thereby facilitating the dispersion of shear stress and enhancing the durability of asphalt.

Formulating for Innovative Self-Compacting Concrete with Low Energy Super-Sulfated Cement Used for Sustainability Development

This study proposed a new way to formulate a low energy super-sulfated cement (SSC) which can be used to produce self-compacting concrete (SCC) with high compressive strength and durability in terms of chloride penetration resistance. This innovative SSC, different from the traditional SSC, was purely produced with a ternary mixture of three industrial by-products of ground granulated blast furnace slag, low calcium Class F fly ash and circulating fluidized bed combustion (CFBC) fly ash and was denoted as SFC-SSC (super-sulfated cement made by mixture of slag, Class F fly ash and CFBC fly ash). Experimental results showed that the combination of a fixed amount of 15 wt.% of CFBC fly ash with various ratios of Class F fly ash to slag could be used to produce the hardened SCCs with high 28-day compressive strengths (41.8 - 65.6 MPa). Addition of Class F fly ash led to the resulting SCCs with lowered price and preferable engineering properties, and thus it was considered as state-of-the-art method to drive such type of concrete towards sustainable construction materials.

Dry Mix Slag—High-Calcium Fly Ash Binder. Part Two: Durability

This work investigates durability of cement-free mortars with a binder comprised of ground granulated blast furnace slag (GGBFS) activated by high-calcium fly ash (HCFA) and sodium carbonate (Na2CO3): the soundness, sulfate resistance, alkali-silica reactivity and efflorescence factors are considered. Results of tests show that such mortars are resistant to alkali-silica expansion. Mortars are also sulfate-resistant when the amount of HCFA in the complex binder is within a limit of 10 wt%. The fineness of fly ash determines its’ ability to activate GGBFS hydration, and influence soundness of the binder, early strength development, sulfate resistance and efflorescence behavior. The present article is a continuation of authors’ work, previously published in MSA, Vol. 14, 240-254.

Extraction of valuable metals from Ti-bearing blast furnace slag using ammonium sulfate pressurized pyrolysis−acid leaching processes

A novel method of extracting valuable metals from Ti-bearing blast furnace slag(TBBF slag)via pressure pyrolysis of recyclable ammonium sulfate(AS)−acid leaching process was proposed.The results show that when pressurized roasting at an AS-to-slag mass ratio 3:1 and 370℃for 90 min,the extraction rates of titanium,aluminum and magnesium reached 94.5%,91.9%and 97.4%,respectively.The acid leaching solution was subjected to re-crystallization in a boiling state to obtain a titanium product having a TiO2 content of 94.1%.The above crystallization mother liquor was adjusted to pH=6 and pH≥12.2,respectively,and then qualified Al2O3 and MgO products were obtained.The analysis through XRD and SEM−EDS proves that the main phases in roasted samples were NH4AlSO4,CaSO4 and TiOSO4.The thermodynamic analysis presents that the main minerals of perovskite,spinel and diopside in raw ore could spontaneously react with the intermediate produced by AS under optimal conditions.

Enantiomeric separation of phenylsuccinic acid by cyclodextrin-modified reversed phase high-performance liquid chromatography

The chiral separation of phenylsuccinic acid(PSA)was studied by reversed phase high-performance liquid chromatography(RP-HPLC)with cyclodextrins(CDs)as chiral mobile phase additives.The effects of types of CDs,concentration of hydroxypropyl-β-cyclodextrin(HP-β-CD),percentage of organic modifier,pH value and column temperature on enantioselective separation were investigated.The quantification property of the developed RP-HPLC method was examined.The chiral recognition mechanism of PSA was also discussed.The results show that a baseline separation of PSA enantiomers is achieved on a Lichrospher C18 column(4.6 mm(inner diameter)×250 mm,5μm)with HP-β-CD as chiral mobile phase additive.The capacity factors of R-PSA and S-PSA are 3.94 and 4.80,respectively.The separation factor and resolution are respectively 1.22 and 8.03.The mobile phase is a mixture of acetonitrile and deionized water(20-80,volume ratio)containing 10 mmol/L HP-β-CD and 0.05% trifluoroacetic acid(pH 2.5,adjusted with triethylamine)with a flow rate of 1.0 mL/min.The ultraviolet(UV)detector is set at 254 nm.The likely roles are inclusion interaction,induction and hydrogen bonding between HP-β-CD and PSA enantiomers.

Deterioration Mechanisms of Sulfate Attack on Concrete under Alternate Action

By micro- and macro-observations, the deterioration mechanisms of concrete under alternate action between repeated sub-high temperature/cooling by water and sodium sulfate solution attack （TW-SA） were studied; meanwhile, the single sodium sulfate solution attack （SA） was also done as comparison. Micro-observations included the analysis of attack products by thermal analysis method and the determination of sulfate-ion content from surface to interior by chemical titrating method （modified barium sulfate gravimetric method）. Macro-observations mainly included the mechanical behaviors such as compressive strength, splitting strength. The experimental results indicate, in both cases, the main attack product is ettringite, only in the first layer of case SA some gypsum is checked; in case SA, the sulfate ions mainly concentrate in the surface layer, so the attack is relatively mild; but in case TW-SA, the repeated sub-high temperature/cooling by water promotes the sulfate ions diffusing inwards, which leads to obvious strength degradation.

Geochemical Characterization and Origin of High-Sulfur,Heavy Oils in Jiyang Sub-Basin,East China

High-sulfur,heavy petroleum is widely occurring in the Tertiary lacustrine Jiyang sub-basin, Bohai Bay Basin.They are differentiated into two families based on the bulk properties and biomarker compositions.Family 1 is characterized by high resins（40%-71%）and sulfur（2%-4%）,and low wax （l%-6%）,with n-alkanes removed by biodegradation,whereas family 2 is characterized by extremely abundant sulfur（3%-10%）,and high asphaltenes（7%-31%）and wax（2%-19%）,with no evidence of microbial attack.The oils of family 1 are distributed in the reservoir,lower than 1500 m throughout the sub-basin.Biomarker assemblages,such as low pristane/phytane ratios（1 Pr/Ph）and a high abundance of carotane,gammacerane,and dinosterane,suggest that they are derived from the calcareous mudstones and shales among the stratified,saline Es_4~u unit,in addition to the in situ biodegradation-concentrated sulfur content.However,the oils of family 2 are identified only in the western Zhanhua and eastern Chezhen depressions,with a depth deeper than 1700 m.Physical properties,together with biomarker ratios,including even-numbered n-alkanes,1 Pr/Ph,trace diasteranes,higher C35 homohopanes,and abundant dibenzothiophene series,with1 dibenzothiophene/phenanthrene,indicate an origin from carbonate source rocks.The X-ray diffraction analysis showed that the carbonate source rock is limited in the Es_4~u unit of the Bonan sag,which is different from most other source rocks in the same horizon.It is suggested that the high-sulfur,heavy oils are generated at the early stage of the oil window.Bacterial sulfate reduction might be responsible for the occurrence of sulfur species in the high-sulfur,heavy oils,while heavy biodegradation will enhance sulfur concentrations.

High-speed countercurrent chromatography for purification of single-walled carbon nanotubes

A new chromatographic purification of single-walled carbon nanotubes using high-speed countercurrent chromatography is reported. The purification was accomplished on the basis of experiment that dispersed the single-walled carbon nanotubes with sodium dodecyl sulfate, and the result mixture was separated using the two phase system composed of n-butanol/water = 1/1 （v/v）. The sizes of SWNTs separated were observed by scanning electron microscopy. The results demonstrated that the high-speed countercurrent chromatography possessed a good efficency for purification of single-walled carbon nanotubes.

硫酸多黏菌素B在两种溶媒中的含量稳定性

目的考察硫酸多黏菌素B在成品输液及高浓度储备液中的含量稳定性,为临床给药提供依据。方法建立测定硫酸多黏菌素B含量的高效液相色谱方法,将硫酸多黏菌素B分别溶于0.9%氯化钠注射液及5%葡萄糖注射液,配成0.5、1 mg·mL^(-1)成品输液及5 mg·mL^(-1)储备液,并在4和25℃储存条件下于0、2、4、6、8、12、16、20及24 h测定多黏菌素B含量。结果4和25℃储存条件下,0.5、1 mg·mL^(-1)硫酸多黏菌素B成品输液和5 mg·mL^(-1)硫酸多黏菌素B储备液均稳定,多黏菌素B1和多黏菌素B2含量和0 h(以100%计)比较,分别在97.23%~102.63%和97.30%~102.63%范围内。结论硫酸多黏菌素B溶于0.9%氯化钠注射液及5%葡萄糖注射液,0.5、1和5 mg·mL^(-1)溶液在4和25℃储存,24 h内稳定性良好。

全球高含硫天然气藏资源分布、地质特征与勘探开发进展

随着勘探开发技术的进步和成本的降低,全球高含硫天然气藏的勘探开发取得了显著进展,但目前针对全球高含硫天然气藏的资源分布和共性地质特征的相关研究较少。为此,在对全球高含硫气藏调研分析的基础上,系统总结了其储量分布特点、天然气地球化学特征、油气成藏条件与富集规律,分析了全球高含硫天然气藏勘探开发历程和关键技术,指出了高含硫天然气资源的安全高效利用的重要意义。研究结果表明:①高含硫天然气藏主要分布在特提斯域中段与前陆相关的叠合盆地三叠系、侏罗系、石炭系和二叠系4个层系,其中石灰岩和白云岩发现的储量超过90%;②高含硫天然气藏一般具有高甲烷、中CO_(2)、低N_(2)含量和硫同位素分馏小的特点;③大型高含硫天然气藏具有优越烃源岩条件,发育优质碳酸盐岩储层与封闭条件良好的膏盐岩盖层,其形成往往经历了高温高能环境并经过多期次调整成藏;④全球高含硫天然气藏经历了2个储量快速增长阶段,主要产量集中在卡塔尔、哈萨克斯坦、俄罗斯、中国和阿曼等5个国家;⑤形成了元素硫溶解和沉积伤害评价、高含硫气井井下节流器、高含硫气藏防腐以及天然气净化等关键开发技术,并建立了高含硫天然气藏安全开发标准和制度、管理与决策体系。结论认为,高含硫天然气田在区域构造位置、储层地质层位和岩性等方面分布极不均衡,大型气藏分布相对集中,天然气地球化学特征明显,气藏形成需要特殊的地质条件,形成的系列适用的勘探开发理论技术为全球高含硫天然气资源的安全高效利用提供了重要的参考和指导。

硫酸镁侵蚀作用下高流态水泥砂浆的早期强度劣化特征

高流态早强(HFES)水泥砂浆被广泛应用于土木工程的各个领域。在复杂的工程环境下,HFES水泥砂浆的硫酸盐侵蚀不容忽视。尽管硫酸盐对水泥基材料性能的影响已有一些研究,但HFES水泥砂浆与传统水泥基材料相比有明显不同,其在硫酸盐侵蚀情况下的劣化机制尚不明确。本文研究了不同硫酸镁溶液浓度和侵蚀时间下HFES水泥砂浆的早期抗折和抗压强度,通过扫描电镜(SEM)、X射线衍射(XRD)和差示扫描量热仪(DSC)测试,分析了硫酸镁溶液浓度和侵蚀次数对HFES水泥砂浆微观结构和水化产物的影响,揭示了硫酸镁对HFES水泥砂浆早期强度形成的影响机制。

PCNF絮凝剂处理高藻水缓解超滤膜污染特性分析

本文以自制纳米Fe_(3)O_(4)为凝聚核心,羧甲基纤维素钠(CMC-Na)为粘合剂,搭配聚合硫酸铁(PFS)制备了新型复合絮凝剂(PCNF)。研究结果表明,纳米Fe_(3)O_(4)和PFS的质量比是决定新型絮凝剂PCNF絮凝效果的关键因素,当纳米Fe_(3)O_(4)和PFS的质量比为1:3时,Zeta电位为-1.5 mV,吸附电中和作用下对藻类物质去除效果较好。表面带有负电荷且具有松散结构的絮体,在超滤膜表面形成易于冲洗的滤饼层,且与超滤膜表面形成较强的静电斥力,超滤过程中比通量下降至0.69,相对污染总值0.33且不可逆污染占比仅仅34.65%,均优于传统絮凝剂PACl。通过微界面机制分析认为,新型PCNF絮凝剂与藻类物质形成的絮体结构,对缓解高藻水体引起的超滤膜污染有重要作用。

硫酸钙晶须/SBS复合改性沥青性能研究

为分析硫酸钙晶须(Calcium Sulfate Whisker,CSW)与苯乙烯-丁二烯-苯乙烯嵌段共聚物(Styrene⁃buta⁃diene⁃styrene Block Copolymer,SBS)复合改性沥青的常规物理性能和高低温流变性,采用沥青三大指标、动态剪切流变(Dynamic Shear Rheology,DSR)和弯曲梁流变(Bending Beam Rheology,BBR)试验,研究了不同CSW掺量对复合改性沥青基本性能和高低温流变性能的影响,并设置CSW改性沥青为对照组。研究结果表明:随着CSW掺量增加,CSW改性沥青的温度敏感性和高温性能提高而低温性能下降;掺量10%CSW改性沥青的针入度指数PI为-0.83,车辙因子G^(*)/sinδ为27.70 kPa,蠕变劲度模量S为368 MPa,蠕变速率m为0.271;CSW/SBS复合改性沥青的温度敏感性和高低温流变性能较CSW改性沥青均明显提高,其中,PI、G^(*)/sinδ和m分别提升了147.0%、82.3%和7.4%,S降低了19.5%。同时,掺量8%CSW/SBS复合改性沥青的高温、低温PG等级分别为82℃和-18℃,比CSW改性沥青的高低温等级分别升了两级和一级。因此,CSW可明显改善沥青的高温性能和温度敏感性,但对沥青低温性能稍微不利,若将其与SBS进行复合改性,可保证沥青的低温性能。