A basic ionic liquid, namely 1,1＇-（butane-1,4-diyl）bis（1,4-diazabicyclo [2.2.2]octan-1-ium） hydrox-ide, was prepared and characterized using Fourier-transform infrared spectroscopy, XH nuclear magnetic...A basic ionic liquid, namely 1,1＇-（butane-1,4-diyl）bis（1,4-diazabicyclo [2.2.2]octan-1-ium） hydrox-ide, was prepared and characterized using Fourier-transform infrared spectroscopy, XH nuclear magnetic resonance spectroscopy, and pH measurements. The ionic liquid was used for efficient promotion of the synthesis of pyrano[2,3-d]pyrimidinone and pyrido[2,3-d]pyrimidine derivatives at room temperature under grinding conditions. A simple procedure, short reaction time, high yields, non-column chromatographic separation, commercial availability of the starting materials, and recyclability of the catalyst are attractive features of this process.展开更多
In order to apply grinding method for degradation of pentachlorophenol(PCP) to an industrial scale,the proportion of different materials[CaO,SiO_2 and CO(NH_2)_2]and the size of grinding balls were examined.For saving...In order to apply grinding method for degradation of pentachlorophenol(PCP) to an industrial scale,the proportion of different materials[CaO,SiO_2 and CO(NH_2)_2]and the size of grinding balls were examined.For saving energy and increasing dechlorination efficiency,the rotation speed and grinding time were maintained at relatively low values.At a mass ratio of grinding balls to materials(40:1),PCP was added into a big steel jar(300 ml) with other materials to grind at 300 r ·min^(-1)for 5 h.The results indicated that when PCP was mixed with CaO and SiO_2in a molar ratio of 1:60:60,the best dechlorination of 58.4%was achieved.CO(NH_2)_2 could not be used as hydrogen donor in the dehalogenation by mechanochemical reaction,since it restrained the dechlorination process.The size of grinding balls has significant effect on the reaction.The experiment with 5 mm steel balls indicates that the weight is too light to provide appropriate energy for the reaction,while steel balls of 10 and 15 mm could give better dechlorination reaction.It indicates that dechlorination depends on the mass of balls and fill rate.展开更多
This paper reports a sustainable,water-assisted,solid-state method for synthesizing ammonium nickel molybdate（（NH4）HNi2（OH）2（MoO4）2,ANM）,a precursor for an unsupported hydrodesulfurization（HDS） catalyst.The ...This paper reports a sustainable,water-assisted,solid-state method for synthesizing ammonium nickel molybdate（（NH4）HNi2（OH）2（MoO4）2,ANM）,a precursor for an unsupported hydrodesulfurization（HDS） catalyst.The associated ANM formation mechanism is also discussed.The synthesis route consists of physical mixing of the raw materials,water-assisted grinding and heating.The formation mechanism involves replacement of a Mo atom by a Ni atom,generating the metastable intermediate（NH4）4（NiH6Mo6O（24））·5H2O.Heating of this intermediate at 120 ℃ removes the added water and produces ANM.Catalysts prepared by this method exhibit almost the same physicochemical properties and catalytic performance during the HDS of dibenzothiophene as materials made from ANM synthesized by a chemical precipitation procedure.Compared with traditional hydrothermal or chemical precipitation methods,this water-assisted,solid-state synthesis provides several significant advantages,including simplifying the synthetic procedure,reducing waste and energy costs and increasing product yields.These features will be highly important with regard to allowing the application of ANM in industrial-scale processes involving HDS reactions.This water-assisted,solid-state strategy can also be extended to the synthesis of isomorphous compounds such as ammonium cobalt（zinc and copper） molybdate.展开更多
Large size mechanical seals are one of the most important components used in reactor coolant pumps.However,the hydrodynamic seal rings with wavy face are difficult to machine due to their high hardness and high form a...Large size mechanical seals are one of the most important components used in reactor coolant pumps.However,the hydrodynamic seal rings with wavy face are difficult to machine due to their high hardness and high form accuracy demand.In order to solve this difficult problem,a novel four-axis linkage grinding method using a cup wheel to process the hydrodynamic seal rings by line contact was proposed.A preliminary study indicates that the form error of the ground seal ring surface is extremely sensitive to different linkage relations of the four axes.By taking the center height of the cup wheel and the laws of motion along the X-axis,Z-axis,B-axis and C-axis as control variables,their effects on the principle form error of the ground surface are evaluated.Six implementation strategies are proposed to reach lower principle form errors.It is found that the minimal principle form error is only 9.64 nm and hence its influence on the ground seal ring shape can be neglected in designing an ultra-precision grinding machine.In addition,the results indicate that the position accuracy of the X-axis at the microscale is acceptable no matter which implementation strategy is selected.This study is expected to serve as a theoretical basis for design and development of the four-axis ultra-precision grinding machine.展开更多
Under the high-speed vibration milling conditions,the solvent and catalyst-free azo-Michael addition of chalcone derivatives and amines was found to proceed efficiently in excellent yields at ambient temperature in sh...Under the high-speed vibration milling conditions,the solvent and catalyst-free azo-Michael addition of chalcone derivatives and amines was found to proceed efficiently in excellent yields at ambient temperature in short reaction time.In most cases,conventional side reactions were avoided and thus quantitative yields were achieved.The influences of the vibration frequency and reaction time on the azo-Michael addition were investigated.展开更多
基金the University of Guilan Research Council for the partial support of this work
文摘A basic ionic liquid, namely 1,1＇-（butane-1,4-diyl）bis（1,4-diazabicyclo [2.2.2]octan-1-ium） hydrox-ide, was prepared and characterized using Fourier-transform infrared spectroscopy, XH nuclear magnetic resonance spectroscopy, and pH measurements. The ionic liquid was used for efficient promotion of the synthesis of pyrano[2,3-d]pyrimidinone and pyrido[2,3-d]pyrimidine derivatives at room temperature under grinding conditions. A simple procedure, short reaction time, high yields, non-column chromatographic separation, commercial availability of the starting materials, and recyclability of the catalyst are attractive features of this process.
文摘In order to apply grinding method for degradation of pentachlorophenol(PCP) to an industrial scale,the proportion of different materials[CaO,SiO_2 and CO(NH_2)_2]and the size of grinding balls were examined.For saving energy and increasing dechlorination efficiency,the rotation speed and grinding time were maintained at relatively low values.At a mass ratio of grinding balls to materials(40:1),PCP was added into a big steel jar(300 ml) with other materials to grind at 300 r ·min^(-1)for 5 h.The results indicated that when PCP was mixed with CaO and SiO_2in a molar ratio of 1:60:60,the best dechlorination of 58.4%was achieved.CO(NH_2)_2 could not be used as hydrogen donor in the dehalogenation by mechanochemical reaction,since it restrained the dechlorination process.The size of grinding balls has significant effect on the reaction.The experiment with 5 mm steel balls indicates that the weight is too light to provide appropriate energy for the reaction,while steel balls of 10 and 15 mm could give better dechlorination reaction.It indicates that dechlorination depends on the mass of balls and fill rate.
基金supported by the National Natural Science Fundation of China(U1162203,21106185)the Fundamental Research Funds for the Central Universities(15CX02023A,15CX06051A)Financial support from Petro China Corporation Limited~~
文摘This paper reports a sustainable,water-assisted,solid-state method for synthesizing ammonium nickel molybdate（（NH4）HNi2（OH）2（MoO4）2,ANM）,a precursor for an unsupported hydrodesulfurization（HDS） catalyst.The associated ANM formation mechanism is also discussed.The synthesis route consists of physical mixing of the raw materials,water-assisted grinding and heating.The formation mechanism involves replacement of a Mo atom by a Ni atom,generating the metastable intermediate（NH4）4（NiH6Mo6O（24））·5H2O.Heating of this intermediate at 120 ℃ removes the added water and produces ANM.Catalysts prepared by this method exhibit almost the same physicochemical properties and catalytic performance during the HDS of dibenzothiophene as materials made from ANM synthesized by a chemical precipitation procedure.Compared with traditional hydrothermal or chemical precipitation methods,this water-assisted,solid-state synthesis provides several significant advantages,including simplifying the synthetic procedure,reducing waste and energy costs and increasing product yields.These features will be highly important with regard to allowing the application of ANM in industrial-scale processes involving HDS reactions.This water-assisted,solid-state strategy can also be extended to the synthesis of isomorphous compounds such as ammonium cobalt（zinc and copper） molybdate.
基金supported by the National Basic Research and Development Program(Grant No.2009CB724306)
文摘Large size mechanical seals are one of the most important components used in reactor coolant pumps.However,the hydrodynamic seal rings with wavy face are difficult to machine due to their high hardness and high form accuracy demand.In order to solve this difficult problem,a novel four-axis linkage grinding method using a cup wheel to process the hydrodynamic seal rings by line contact was proposed.A preliminary study indicates that the form error of the ground seal ring surface is extremely sensitive to different linkage relations of the four axes.By taking the center height of the cup wheel and the laws of motion along the X-axis,Z-axis,B-axis and C-axis as control variables,their effects on the principle form error of the ground surface are evaluated.Six implementation strategies are proposed to reach lower principle form errors.It is found that the minimal principle form error is only 9.64 nm and hence its influence on the ground seal ring shape can be neglected in designing an ultra-precision grinding machine.In addition,the results indicate that the position accuracy of the X-axis at the microscale is acceptable no matter which implementation strategy is selected.This study is expected to serve as a theoretical basis for design and development of the four-axis ultra-precision grinding machine.
基金supported by the National Natural Science Foundation of China (20876148)the Natural Science Foundation of Zhejiang (Y407306)
文摘Under the high-speed vibration milling conditions,the solvent and catalyst-free azo-Michael addition of chalcone derivatives and amines was found to proceed efficiently in excellent yields at ambient temperature in short reaction time.In most cases,conventional side reactions were avoided and thus quantitative yields were achieved.The influences of the vibration frequency and reaction time on the azo-Michael addition were investigated.
