化学镀镍废水中磷处理的研究

化学镀镍技术,以其独特的优越性正被广泛应用。但是化学镀镍溶液因其自身的还原反应性质导致镀液不稳定、使用寿命短。产生的废液中含有大量的镍离子、亚磷酸盐、硫酸钠及一些有机物等。镍是一种致癌的重金属物质,也是一种短缺昂贵的金属资源,磷则是引起水体富营养化现象的主要污染因素之一。因此,如何有效地处理化学镀镍废液中的磷,减少对环境的污染及生态平衡的破坏,有着非常重要的现实意义。本文通过大量的试验对影响磷处理效果的氯化钙投加量、反应温度、反应时间、反应pH值等因素进行了优化。在试验的基础上,可根据实际操作所得出的温度与pH值对镀镍废水磷处理的影响的结论,设计出一套化学镀镍废液综合治理的工艺流程。因此,具有非常重要的现实意义。     

电解法降解化学镀镍废液COD的研究

采用电解法处理化学镀镍废液,考察了pH值、电流密度、温度、循环、电解时间等因素对镍离子回收率和COD去除率的影响,并重点研究了电解参数对化学镀镍废液中不同物质的COD降解效果的影响。结果表明,酸性条件有利于COD的降解,碱性条件有利于化学镀镍废液中镍的回收,当镍的回收率达到98.7%时,COD的去除率可达61.91%。     

Preparation and catalytic properties of ZrO2-Al2O3 composite oxide supported nickel catalysts for methane reforming with carbon dioxide

ZrO2-Al2O3 composite oxides and supported Ni catalysts were prepared, and characterized by N2 adsorption/desorption, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) techniques. The catalytic performance and carbon deposition was also investigated. This mesoporous composite oxide is shown to be a promising catalyst support. An increase in the catalytic activity and stability of methane and carbon dioxide reforming reaction was resulted from the zirconia addition, especially at 5wt% ZrO2 content. The Ni catalyst supported ZrO2-Al2O3 has a strong resistance to sintering and the carbon deposition in a relatively long-term reaction.     

C/C复合材料不同碳基体的纳米压痕行为研究

目的研究碳基体微观结构对材料整体性能的影响。方法用酚醛浸渍-碳化、中温煤沥青浸渍-碳化、甲烷为碳源前驱体,经化学气相沉积制备得到不同碳基体C/C复合材料。采用偏光显微镜对C/C复合材料不同碳基体的显微结构进行观察分析,采用XRD和Raman光谱对C/C复合材料的树脂碳基体、沥青碳基体和热解碳基体的微晶尺寸进行表征,以玻璃碳作为参比样品,通过纳米压痕测试不同碳基体试样的弹性模量和硬度。结果碳基体为热解碳和沥青碳的石墨微晶缺陷少,完整度较好,石墨化程度高。玻璃碳和树脂碳基体中石墨微晶排列紊乱,有序度低,石墨化程度低。酚醛浸渍-碳化得到的树脂碳的微晶尺寸Lc最小,为1.69 nm,弹性模量和硬度最大,分别为(23.17±0.54) GPa和(3.26±0.10) GPa;光滑层热解碳和粗糙层热解碳的弹性模量和硬度次之;沥青碳的微晶尺寸最大,Lc为9.36nm,而弹性模量和硬度最小,分别为(12.53±2.29) GPa和(0.72±0.14) GPa。结论不同碳基体的C/C复合材料中,碳基体的石墨化度越高,微晶尺寸越大,各向异性越显著,材料的弹性模量和硬度越低。     

Catalytic decomposition of low level ozone with gold nanoparticles supported on activated carbon

Highly dispersed gold nanoparticles were supported on coal-based activated carbon (AC) by a sol immobilization method and were used to investigate their catalytic activity for low-level ozone decomposition at ambient temperature. Nitrogen adsorption-desorption, scanning electron microscope (SEM), and X-ray photoelectron spectroscopy (XPS) were used to characterize the catalysts before and after ozone decomposition. The results showed that the supported gold nanoparticles prepared with microwave heating were much smaller and more uniformly dispersed on the activated carbon than those prepared with traditional conduction heating, exhibiting higher catalytic activity for ozone decomposition. The pH values of gold precursor solution significantly influenced the catalytic activity of supported gold for ozone decomposition, and the best pH value was 8. In the case of space velocity of 120000 h⁻¹, inlet ozone concentration of 50 mg/m³, and relative humidity of 45%, the Au/AC catalyst maintained the ozone removal ratio at 90.7% after 2500 min. After being used for ozone decomposition, the surface carbon of the catalyst was partly oxidized and the oxygen content increased accordingly, while its specific surface area and pore volume only decreased a little. Ozone was mainly catalytically decomposed by the gold nanoparticles supported on the activated carbon.     

介孔氮化碳对水中全氟辛烷磺酸的吸附去除研究

以SBA-15为模板、四氯化碳和乙二胺为前驱体,通过聚合反应制备了介孔氮化碳(Mesoporous Carbon Nitride,MCN).同时,采用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶红外光谱(FT-IR)、X射线光电子能谱(XPS)和元素分析等手段对MCN进行了表征分析,并考察了MCN对水中全氟辛烷磺酸(PFOS)的吸附性能.结果表明,MCN吸附PFOS的过程符合准二级动力学模型,其吸附行为遵循Langmuir等温线模型;MCN吸附去除PFOS的效率受溶液pH值、溶液温度及共存离子等因素的影响,其中,溶液pH值的影响最为显著,当溶液pH值分别为2.2和10.6时,MCN对PFOS的去除率分别为98.15%和5.59%;吸附PFOS饱和后的MCN可以用0.1 mol·L-1NaOH溶液进行解吸,经5次循环/再生后的MCN对PFOS的去除率仍在95%以上.与介孔碳(CMK-3)和活性炭(AC)相比,MCN对PFOS显示出更优越的吸附能力.     

硅铝比和NiO对ZSM-5协同低温等离子体降解甲苯的影响

研究了不同硅铝比的ZSM-5与Ni/ZSM-5分子筛协同低温等离子体技术对甲苯降解性能的影响.以Ni O(Nickel Oxide)为活性组分,采用浸渍法对ZSM-5分子筛进行改性,利用氮气吸附脱附(BET)、X射线衍射仪(XRD)、X射线光电子能谱分析(XPS)、H_2程序升温还原(H_2-TPR)、NH_3程序升温脱附(NH_3-TPD)、Toluene程序升温脱附(Toluene-TPD)等技术表征样品的物理化学性质.考察了硅铝比对ZSM-5与Ni/ZSM-5分子筛体系中甲苯的吸附性能,研究了不同放电电压下硅铝比对甲苯降解率、碳平衡及二氧化碳选择性的影响,并采用气相色谱-质谱联用仪(GC-MS)分析了催化剂表面的有机产物.结果表明:硅铝比不但影响分子筛本身的物理化学特性(比表面积、氧化还原性能、表面酸性、疏水性等),还会影响Ni的负载形态和方式,更高的硅铝比与Ni O的负载能促进甲苯深度氧化,减少副产物,提高碳平衡和二氧化碳选择性.     

化学镀镍老化液资源化处理工艺的研究

利用三步法综合处理化学镀镍老化液。以多孔性泡沫镍作为阴极、Ti RuO2 作为阳极 ,电解回收化学镀镍老化液中的金属镍离子 ,镍的回收率可以达到 97.5 % ,同时废液中总有机碳去除率达到 97.3 % ;再以 15 %石灰乳作沉淀剂 ,每克镍投加量为 6.5mL时进一步将溶液中的残余镍处理至排放标准以下 ;最后以Ca(ClO) 2 作为氧化沉淀剂 ,处理剩余溶液中的磷 ,排放水中总磷浓度达到 1.0 6mg L ,沉淀中镍的含量低于 1.4mg kg ,以P2 O5计的磷含量高达 67.3 % ,符合农用污泥污染物控制指标 ,可以作为农业肥料使用。实验结果表明 ,利用以上方法处理 ,可以有效地将老化液中的镍、磷处理至排放标准以下 ,同时溶液中的大量有机物得到去除 ,化学镀镍老化液中的有用资源得到回收利用     

活性炭负载Co3O4活化过一硫酸盐降解金橙G

通过浸渍煅烧法制备活性炭负载Co的活化剂(Co/AC),采用X射线衍射仪(XRD)、扫描电镜(SEM)及X射线能谱仪(EDS)技术对活化剂进行表征,发现Co主要以Co_3O_4的形式负载于活性炭表面,并利用Co/AC活化过一硫酸盐(PMS)产生硫酸根自由基(SO_4~-·)降解偶氮染料金橙G(OG),研究了活化反应机制及不同因素对OG降解的影响.结果表明,SO_4~-·在OG降解过程中起主要作用,并且随Co/AC用量、PMS浓度、温度的提高,OG降解效率明显增加.反应初始pH对降解OG有较大影响,当p H在4~8范围内,SO_4~-·均能有效降解OG,但在强酸碱条件下,则不利于OG降解.Cl~-对活化降解OG具有双重作用,低浓度时抑制降解,而在高浓度时促进降解.Co/AC在重复使用6次时仍具有较好活化性能.通过紫外可见光谱及气相色谱-质谱(GC/MS)对OG降解过程及中间产物进行了分析.     

Electro-oxidation of Ni (II)-citrate complexes at BDD electrode and simultaneous recovery of metallic nickel by electrodeposition

The simultaneous electro-oxidation of Ni (II)-citrate and electrodeposition recovery of nickel metal were attempted in a combined electro-oxidation-electrodeposition reactor with a boron-doped diamond (BDD) anode and a polished titanium cathode. Effects of initial nickel citrate concentration, current density, initial pH, electrode spacing, electrolyte type, and initial electrolyte dosage on electrochemical performance were examined. The efficiencies of Ni (II)-citrate removal and nickel metal recovery were determined to be 100% and over 72%, respectively, under the optimized conditions (10 mA/cm², pH 4.09, 80 mmol/L Na₂SO₄, initial Ni (II)-citrate concentration of 75 mg/L, electrode spacing of 1 cm, and 180 min of electrolysis). Energy consumption increased with increased current density, and the energy consumption was 0.032 kWh/L at a current density of 10 mA/cm² (pH 6.58). The deposits at the cathode were characterized by scanning electron microscopy (SEM), energy-dispersive spectrometry (EDS), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). These characterization results indicated that the purity of metallic nickel in cathodic deposition was over 95%. The electrochemical system exhibited a prospective approach to oxidize metal complexes and recover metallic nickel.     

Pd/CMK-3的合成、表征及对甲酸的电催化氧化性能研究

以中孔硅SBA-15为硬模板、蔗糖为炭源,合成了有序中孔炭CMK-3,并以此CMK-3为载体,采用络合还原法制备了负载量为20%的催化剂Pd/CMK-3.X射线衍射(XRD)和透射电镜(TEM)的结果表明,CMK-3孔结构高度有序,呈现二维六方结构,Pd/CMK-3和Pd/AC(活性炭)催化剂中Pd纳米颗粒分散均匀,平均粒径分别为4.2 nm和4.5 nm;拉曼光谱测试表明,CMK-3比活性炭的石墨化程度更高,导电性更强;N2吸附/脱附实验表明,CMK-3具有典型的中孔结构,CMK-3的最可几孔径为4.5 nm,显著大于活性炭的0.54 nm,CMK-3的BET比表面积为1 114 m2.g-1,大于活性炭的871 m2.g-1.在对甲酸电催化氧化的循环伏安(CV)和计时电流(CA)测试中,Pd/CMK-3的初始催化活性显著高于Pd/AC,而两者在100 s后的计时电流稳定性则基本相当.     

负载型纳米铁吸附剂去除饮用水中As(Ⅴ)的研究

以活性炭为载体制备了一种负载型纳米铁吸附剂.纳米铁在活性炭孔内为针状,其直径为30～500 nm,长度为1 000～3 000 nm,载入量[m(Fe)/m(炭)]为82.1 mg/g.用1.5 g/L该吸附剂对pH 6.5、 (25±2)℃、 2 mg/L的As(Ⅴ)进行吸附其去除率为99.5%,在平衡浓度1.0 mg/L时,该吸附剂对As(Ⅴ)的吸附容量为15.4 mg/g;吸附速度较快,12 h可达91.4%,72 h达到吸附平衡.吸附过程可由孔内扩散模型较好地说明.除PO_4~(3-)、SiO_4~(2-)外其它常见阴阳离子均对As(Ⅴ)的去除影响不大.吸附剂可以用0.1 mol/L NaOH溶液再生,再生效率较高.实验室初步实验数据表明,该吸附剂对饮用水砷去除具有较好的应用前景.     

活性炭催化双氧水氧化处理分散橙结晶废母液

采用Fe2+/H2O2、活性炭(AC)/H2O2和AC/H2O2/Fe2+三种氧化体系对高浓度、高酸度和高盐分的分散橙结晶废母液进行处理,探讨了H2O2投加量、n(H2O2)/n(Fe2+)比值和初始pH对TOC去除率影响,比较三种氧化体系对TOC和色度的去除效果。结果表明:AC/H2O2/Fe2+氧化体系对TOC去除率最高,AC/H2O2氧化体系对色度去除率最高。即使在强酸环境中下,AC对H2O2仍然具有较高的催化活性,并可多次重复利用。AC/H2O2氧化体系为分散橙结晶废母液处理及资源化利用提供了新途径。     

Activated carbon supported TiO2-photocatalysis doped with Fe ions for continuous treatment of dye wastewater in a dynamic reactor

Fe-doped TiO2 coated on activated carbon (Fe-TiO2/AC, FTA) composites were prepared by an improved sol-gel method and characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, X-ray di ractometry, inductively coupled plasma mass spectrometry and BET surface area analysis. Obtained FTA composites were applied to the continuous treatment of dye wastewater in a dynamic reactor. The e ects of Fe ion content, catalyst content, UV-lamp power and flowrate of the continuous treatment of dye wastewater on degradation e ciency were analyzed to determine the optimum operating conditions of dye wastewater degradation. Continuous photocatalytic experiments provided interesting results that FTA had a high chemical oxygen demand (COD) removal rate compared with TiO2, Fe doped TiO2 (FT) and TiO2 coated on activated carbon (TA). In particular, when using the FTA catalyst with a Fe ion content of 0.33%, the kinetic content (k = 0.0376) of COD removal was more than the sum of both TA (0.0205) and 0.33% FT (0.0166). FTA showed a high photoactivity because of a synergistic e ect between Fe ions and AC on TiO2, which is higher than the individual e ects of AC or Fe ions on TiO2. Additionally, for the photocatalytic degradation of dye wastewater, the optimum Fe ion content, catalyst content, UV-lamp power and flowrate were 0.33%, 6 g/L, 60 W (two lamps) and 300 mL/hr, respectively. An investigation of catalyst reuse revealed that the 0.33% FTA showed almost no deactivation in photocatalytic degradation of naturally treated wastewater.     

Fe-Ni-TiO2/AC粒子电极的制备及可见光光电催化协同降解RhB

制备Fe-Ni-TiO2/AC粒子电极,应用于可见光助三维电极/电Fenton(Vis-3D/EF)光电催化体系中,以RhB为目标污染物,研究了可见光光电催化对RhB的协同降解.实验优化了Fe-Ni-TiO2/AC粒子电极的制备条件,并与活性炭粒子电极、活性炭负载TiO2粒子电极在Vis-3D/EF体系中的光电催化性能进行对比,结果表明:TiO2浸渍液浓度为2g/L,Fe-Ni掺杂比为5:5,Fe:Ni:TiO2物质的量比为0.5:0.5:100的条件下制备的粒子电极在Vis-3D/EF体系中表现出最优的光电催化性能,60min对RhB的去除率达92.58%,优于活性炭粒子电极和活性炭负载TiO2粒子电极.自制粒子电极在Vis-3D/EF体系比在3D/EF体系对RhB的去除率提高29.46%,表现出明显的光催化和三维电极/电Fenton协同处理效果,协同指数为1.18,说明了自制粒子电极应用在Vis-3D/EF组合技术中,实现对RhB的可见光光电协同降解是可行的.     

Zero-valent iron doped carbons readily developed from sewage sludge for lead removal from aqueous solution

Low-cost but high-efficiency composites of iron-containing porous carbons were prepared using sewage sludge and ferric salts as raw materials. Unlike previous time- and energy-consuming manufacturing procedures, this study shows that pyrolyzing a mixture of sludge and ferric salt can produce suitable composites for lead adsorption. The specific surface area, the total pore volume and the average pore width of the optimal composite were 321 m²/g, 0.25 cm³/g, and 3.17 nm, respectively. X-ray diffraction analysis indicated that ferric salt favored the formation of metallic iron, while Fourier transform infrared spectroscopy revealed the formation of hydroxyl and carboxylic groups. The result of batch tests indicated that the adsorption capacity of carbons activated with ferric salt could be as high as 128.9 mg/g, while that of carbons without activation was 79.1 mg/g. The new manufacturing procedure used in this study could save at least 19.5 kJ of energy per gram of activated carbon.     

活性炭粒子电极改性及其电催化性能

针对粒子电极电催化性能低、电能消耗大等问题,以柱状活性炭（AC）为载体,采用浸渍法制备负载金属的活性炭粒子电极,通过正交试验探究其最优制备条件,并应用Bohem返滴定法和SEM对改性活性炭进行表征。正交试验表明:粒子电极电催化性能受浸渍时间的影响比受浸渍浓度、焙烧时间、焙烧温度的影响更大。不同制备条件下的粒子电极形貌差异很大。在0.1 mol/L的浸渍液中浸渍12 h,400 ℃条件下焙烧4 h得到的粒子电极用于三维电极反应器中降解活性艳红X-3B,染料去除率达到85.97%,COD去除率达到65.61%,对比AC,染料去除率提高了5.29百分点,COD去除率提高了10.12百分点,能耗降低了13%。表明Ni/AC粒子电极可提高其电催化性能,降低能耗。     

载银活性炭活化过硫酸钠降解酸性橙7

采用硝酸氧化的颗粒活性炭浸渍制备Ag/GAC活化剂,利用N₂吸附、 SEM、 FT-IR及XRD对Ag/GAC进行表征,得出Ag成功负载于颗粒活性炭上,并以Ag/GAC在常温常压下活化过硫酸钠(PS)产生硫酸根自由基(SO^－4 ·)降解偶氮染料酸性橙7(AO7). 考察了Ag负载量、 PS浓度、 Ag/GAC投加量、 初始pH对AO7降解效果的影响. 结果表明,当Ag负载量为12.7 mg ·g^-1、 n(PS) :n(AO7)为120 :1、 Ag/GAC投加量为1.0 g ·L^-1,降解180 min后AO7降解率达95.0%以上. 初始pH对Ag/GAC活化PS降解AO7有较大影响,pH为5.0时降解效果最优. 通过紫外可见光谱、 气相色谱-质谱(GC/MS)对AO7降解过程进行了探讨,在降解过程中AO7的偶氮键和萘环结构均被破坏,并检测出主要降解产物有邻苯二甲酸和乙酰苯.     

生物炭负载纳米零价铁对污染土壤中铜钴镍铬的协同去除

合成了一种低成本、高效生物炭负载纳米零价铁的复合材料(ZVI-SM)并应用于铜、钴、镍、铬污染土壤的修复。采用X射线衍射(XRD)、X射线光电子能谱(XPS)和金属吸附实验等方法,考察了不同碳化温度下制备的生物炭前驱体和生物炭复合材料对复合重金属污染修复的影响及去除作用机制。其中,吸附-还原后形成的FeCr₂O₄极大地降低了铬的毒性,同时提高了铜、钴、镍的去除率。Fe0的引入既提高了生物炭对重金属的吸附量,又解决了Cr(Ⅵ)毒性的问题;XPS的结果进一步阐明了生物炭可以作为电子传递介质,通过表面官能团得失电子与Fe0间形成强相互作用,增强了复合材料对多重金属离子的去除效果。除ZVI-SM500外,ZVI-SM100、300、400、700 4种材料对于铜、钴、镍、铬的去除率要远高于商用纳米Fe0和单纯的生物炭材料,表现为对铬和铜有较强的亲和力和反应性,均能在5 min内完全去除铜和铬,钴和镍也能在180 min内达到80%以上的去除率。在反应过程中存在显著的离子竞争效应:铬≥铜>钴>镍,这与金属离子的标准还原电位大小的趋势一致。土壤修复实验表明:ZNI-SM300用于污染土壤的修复,15 d后,Cr(Ⅵ)含量从480 mg/kg降至0.52 mg/kg,水溶态Cr总量从500 mg/kg降至1.2 mg/kg,两者的固定化效率均达到99%以上,并能达到完全去除水溶态的铜、钴、镍、Cr(Ⅵ)的效果。因此,以SM300为载体的纳米零价铁可作为复合重金属污染土壤修复的理想材料。     

醋酸银真空浸渍制备杀菌功能载银活性炭及其表征

通过醋酸银真空浸渍法制备了银缓释杀菌功能载银活性炭(Ag/AC),研究了其对大肠杆菌(E.coil)的杀灭性能和抗银流失性能.以气体吸附仪测定活性炭的比表面积和孔结构,以扫描电子显微镜(SEM)观察Ag/AC表面形貌,以X射线衍射(XRD)考察Ag/AC晶体结构.结果表明,单质银均匀负载在活性炭表面.随着CH3COOA...