Direct Electrochemical Preparation of Nickel Complexes

采用金属镍为“牺牲”阳极 ,首次在无隔膜电解槽中 ,电化学溶解金属镍一步制备了纳米NiO前驱体Ni(OEt) 2 ,Ni(OBu) 2 ,Ni(OEt) 2 (acac) 2 ,Ni(OBu) 2 (acac) 2 [acac为乙酰丙酮基 ].产物通过红外光谱 (FT IR)、拉曼光谱 (Ramanspectrum)进行表征 .同时讨论了影响电合成镍醇盐及其配合物的关键因素 .实验表明 ,防止阳极钝化 ,温度控制在30～ 40℃ ,采用有机胺溴化物为导电盐 ,可以提高电合成效率Nickel complexes were directly prepared by electrochemical dissolution of nickel in non-aqueous media. The products were characterized by FT-IR spectrum and Raman spectrum. The influence of temperature and conductive additives on product yield was also investigated. The experiments at the temperature under 30～40 ℃ with R 4NBr as a conductive additive gave improve yields. The study showed that the direct electrochemical preparation of nickel complexes had high current efficiency and electrolysis yield. These nickel complexes had high purity and could be directly used as precursor of nanometer oxides.国家自然科学基金 (No .2 98730 39);; 安徽省自然科学基金 (No.0 0 0 46 112 );; 安徽省教育委员会自然科学基金资助项

Electrochemical synthesis of zinc complexes and preparation of nano-sized ZnO

Zinc complexes were directly prepared by using zinc metal as sacrificing anode in a cell without separating the cathode and anode spaces. The products were characterized by using FT-IR, NMR and Raman spectroscopy. The influence of temperature and conductive additives on product yield was also investigated. The study shows that direct electrochemical preparation of zinc complexes such as Zn(acac)(2), Zn(OEt)(2) (acac)(2) and Zn(OBu)(2)(acac)(2) has high current efficiency and electrolysis yield than that of Zn(OR)(2). Furthermore, these zinc complexes have high purity and can be directly used as sol-gel precursor for preparation of nanometer ZnO. Experimental results show that controlling temperature in the range of 50 similar to 60 degreesC, selecting R4NBr as conductive additives and preventing zinc anode from being covered by electrochemical products can improve product yield. The study also shows that nano-sized ZnO prepared by this method has monoclinic structure with a narrow size distribution of 5-10 nm

基于展成法的蜗轮数控铣削加工工艺研究

为实现蜗轮的展成法加工，在经过数控改造的普通铣床上使用蜗轮滚刀，通过扩展应用螺纹指令和锥螺纹指令的功能，实现了蜗轮滚刀转1转对应蜗轮工件转1齿的运动比例关系；通过将允许的蜗轮齿距累积误差均匀地分布在蜗轮节圆的几段圆弧上，大大提高了蜗轮的齿距精度和传动精度，从而提高了其传动的平稳性。实践表明，该方法不仅得到了较高的蜗轮加工精度，而且扩展了数控改造的应用范围

非水体系中电解镍中间产物制备纳米NiO

采用纯镍为阳极,乙酰丙酮和乙醇的混合溶液中加入少量有机胺导电盐为电解液,施加一定电流使镍溶解,然后将电解液直接水解,控制一定的水解条件,制备得到纳米NiO粉体.采用拉曼光谱、红外光谱、元素分析、XRD和TEM分别对电解得到的纳米NiO前驱体和纳米NiO进行了分析与表征,并探讨了电化学溶解镍金属法制备纳米NiO反应的影响因素.电化学溶解镍金属得到的前驱体为Ni(OEt)2(acac)2,这种不溶性镍醇盐配合物升温至40～50℃即可溶解于乙醇溶液中,可直接应用于溶胶-凝胶(Sol-gel)过程.水解后的纳米NiO呈无定形结构,350℃煅烧后形成立方晶型NaCl结构,纳米NiO经600℃煅烧后粒径分布在5～10nm.该方法理论上为二价不溶性金属醇盐经溶胶凝胶工艺制备纳米氧化物材料提供了一条新的途

电合成系列锌配合物及纳米ZnO的制备

采用锌金属为“牺牲”阳极 ,首次在无隔膜电解槽中 ,电化学一步法制备了纳米ZnO前驱体锌配合物Zn(OEt) 2 ,Zn(OBu) 2 ,Zn(acac) 2 ,Zn(OEt) 2 (acac) 2 ,Zn(OBu) 2 (acac) 2 (acac为乙酰丙酮基 ) ,产物通过红外光谱 (FT IR)、拉曼光谱和核磁共振进行表征 .同时采用含Zn(OEt) 2 (acac) 2 的电解液直接水解制备纳米ZnO粉体 ,纳米ZnO通过拉曼光谱、X射线粉末衍射 (XRD)和透射电子显微镜 (TEM)进行表征 .实验表明电解时防止阳极钝化 ,控制温度在 5 0～ 6 0℃之间 ,采用有机胺溴化物为导电盐 ,可以提高电合成效率 ;电解合成Zn(acac) 2 ,Zn(OEt) 2 (acac) 2 ,Zn(OBu) 2 (acac) 2 的电流效率比Zn(OEt) 2 ,Zn(OBu) 2 高 ,其中Zn(OEt) 2 (acac) 2 适宜作为溶胶 -凝胶法制备纳米ZnO的原料 ,制备得到的纳米ZnO经 6 0 0℃煅烧后呈球形单分散结构 ,平均粒径在 5～ 10nm左右

ELECTROCHEMICAL SYNTHESIS OF METAL ALKOXIDES USING SACRIFICING ANODE

采用金属为“牺牲”阳极 ,在无隔膜电解槽中 ,一步法制备金属醇盐 :Ti(OEt) 4、Ti(OPr -i) 4、Ti(OMe) 4(acac)、Cu(OEt) 2 、Cu(OBu) 2 、Ni(OEt) 2 和Mg(OEt) ,产物通过元素分析、红外光谱进行表征 .实验表明电极表面粗糙化处理 ,防止阳极纯化 ,温度控制在 5 0 - 60℃之间 ,采用有机溴化胺电导盐 ,可以提高电合成收率 .采用合金电极 ,可以有效克服不溶性金属醇盐在阳极的吸附问题 ,并同时合成几种金属醇盐 ,从而提高反应的电流效率 .Metal alkoxides were directly prepared using pure metal as sacrificing anode in absolute alcohol. Metal alkoxides were characterized by FTIR spectra and element analysis. The effects of temperature,conductive additives,trace water on product yield were also investigated. The results showed that the direct electrochemical preparation of metal alkoxides had high current efficiency and electrolysis yield. These metal alkoxides have high purity and can be directly used as precursor of nanometer oxides prepared by Sol-gel method. The experiments showed that controlling temperature under 50-60℃, selecting R 4NBr as conductive additives and preventing titanium anode from being passiviated can improve product yield. Using alloy as anode may be recommended as a technique for the synthesis of alkoxides, this process can run in sufficiently high current efficiency and high reaction activity.安徽省教育厅科研基金 ( 99JL0 0 75 ) ;; 安徽省自然科学基金 ( 0 0 0 46112

电化学溶解钛金属直接水解法制备纳米TiO_2

Metallic titanium was electrochemically dissoluted in absolute ethanol in the presence of Et4N· Br(as electro conductive additive),The electrolyte solution was then directly hydrolysized to obtain nanocrystalline TiO2.The powder obtained was calcined at 720℃ for 1 h.FT IR,Raman spectra,XRD and TEM were used to investigate the structure and particle size of the powder.Studies showed that the nanocrystalline TiO2 prepared by this method was of monocline structure with high textural stability and narrow size distribution of 10－ 20 nm,and its Raman spectra showed a shift of about 25 cm－ 1.The experiments also showed that the product yield could be improved by controlling the temperature under 50－ 60℃ ,selecting R4N· Br as conductive additive and preventing titanium anode from being passivated.The electrochemical dissolution of metal anode may be recommanded as a promising technique for the synthesis of nanomaterials

Electrochemical Synthesis of Metal Alkoxides Using Sacrificial Anode

采用金属为“牺牲”阳极 ,在无隔膜电解槽中 ,一步法制备了纳米材料前驱体金属醇盐 :Ti(OEt) 4、Ti(OPr i) 4、Ti(OBu t) 4、Ti(OMe) 2 (acac)、Cu(OEt) 2 、Cu(OBu) 2 、Ni(OEt) 2 和Mg(OEt) 2 ,产物通过元素分析、红外光谱 (FTIR)进行了表征。讨论了影响电合成钛醇盐的关键因素 ,实验表明电极表面粗糙化处理 ,防止阳极钝化 ,温度控制在 5 0～ 6 0℃ ,采用有机季铵溴化物为导电盐 ,可以提高电合成收率。采用合金电极 ,可以有效克服不溶性金属醇盐在阳极的吸附问题 ,并同时合成几种金属醇盐。Metal alkoxides were directly prepared with pure metal as sacrificial anode in absolute alcohol.The products were characterized by FTIR spectra and elementary analysis.The effects of temperature,conductive additives and trace water on the yield of product were also investigated.The results showed that direct electrochemical preparation of titanium alkoxides had high current efficiency and electrolysis yield.These titanium alkoxides have high purity and can be used directly as precursor of nanometer oxides prepared by Solgel method.The experiments showed that by controlling temperature under 50-60 ℃,selecting R\-4NBr as conductive additives and preventing titanium anode from being passiviated,yield of the product was increased.The use of alloy as anode may be recommended as a technique for the synthesis of alkoxides.This process can run with high current efficiency and high reaction activity.安徽省教育委员会基金资助课题 !(99j10 0 75