基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量...基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量白酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。实验对HS-SPME方法进行了优化,在酒精度12%vol、加NaCl 3 g、萃取温度70℃,萃取时间40 min的条件下,能够显著提高目标物的响应值。实验以D_(5)-氨基甲酸乙酯(D_(5)-EC)为内标,对不同浓度的样品溶液进行GC×GC-TOFMS定量分析。结果表明,EC在10~500μg/L范围内线性关系良好,回归系数(R^(2))>0.998,检出限为0.19μg/L,定量限为0.64μg/L,平均回收率为97.57%,精密度为8.66%。测定结果与国标方法相比无显著性差异(P>0.05)。该方法前处理简单,检测灵敏度更高,为白酒中EC自动化定量测定提供了新思路。展开更多
It was investigated that the reaction of 4,4′-diphenylmethanediamine(MDA)with CO2 and bromoethane to synthesize diethyl 4,4′-diphenylmethanedicarbamate(MDC)under the catalysis of Cs2CO3 cooperating with DBU in super...It was investigated that the reaction of 4,4′-diphenylmethanediamine(MDA)with CO2 and bromoethane to synthesize diethyl 4,4′-diphenylmethanedicarbamate(MDC)under the catalysis of Cs2CO3 cooperating with DBU in supercritical carbon dioixide.The optimum reaction conditions were MDA(10mmol),EtBr(30mmol),Cs2CO3(6mmol)as catalyst cooperating with DBU(30mmol),a temperature of 60 °C,a pressure of 8 MPa,and a reaction time of 4 hours.MDC was obtained in the yield of 88% under the optimum reaction condtions.展开更多
As a novel collector, O-isopropyl-N,N-diethyl thionocarbamate(IPDTC) was designed and synthesized for copper-sulfur flotation separation. Density functional theory calculations were performed to investigate the electr...As a novel collector, O-isopropyl-N,N-diethyl thionocarbamate(IPDTC) was designed and synthesized for copper-sulfur flotation separation. Density functional theory calculations were performed to investigate the electronic structures of IPDTC. The results showed that IPDTC had higher energy of the highest occupied molecular orbital but lower electronegativity than O-isopropyl-N-ethyl thionocarbamate(Z-200). It was predicted that IPDTC had strong collection ability according to the reaction energy criteria. Flotation results demonstrated that the collecting ability of IPDTC to chalcopyrite and pyrite was stronger than that of Z-200. Then, the flotation mechanism was analyzed by measurements of surface tension, adsorption capacity, XPS, FTIR and zeta potential. These results indicated that IPDTC could reduce the solution surface tension. The adsorption capacity of IPDTC on chalcopyrite was higher than that on pyrite, consistent with the results of the flotation tests. FTIR, zeta potential and XPS results also demonstrated that IPDTC was strongly absorbed on the chalcopyrite surface by formation of Cu—S—C bonds, but showed a weak affinity on the pyrite surface.展开更多
Tung oil-based polyols were synthesized by the esterification and transesterification between Tung oilbased anhydride and butanediol. The hydroxyl values of the polyols prepared were tested and discussed. Polyurethane...Tung oil-based polyols were synthesized by the esterification and transesterification between Tung oilbased anhydride and butanediol. The hydroxyl values of the polyols prepared were tested and discussed. Polyurethane was prepared by using Tung oil-based polyols and/or poly(propylene glycol) as polyols and by using isophorone diisocyanate as isocyanate. The effect of the ratio of Tung oil-based polyols to poly(propylene glycol) on the properties of polyurethane prepared was investigated by the water resistance, alcohol resistance and hardness tests. The results show that Tung oil-based polyols are effective to improve the hardness, water resistance and alcohol resistance of polyurethane.展开更多
Water-dispersed polyurethane (PU) adhesive is a novel and highly efficient adhesive with broad application potential. In this study, the key parameters affecting the synthesis and application of this adhesive were exa...Water-dispersed polyurethane (PU) adhesive is a novel and highly efficient adhesive with broad application potential. In this study, the key parameters affecting the synthesis and application of this adhesive were examined, and optimal conditions were identified. The water-dispersed PU adhesive was successfully synthesized, and applied in the fastness test of pigment printing on cotton fabric. The data demonstrated that all the fastnesses of PU adhesive were better than that of the conventional PA one.展开更多
Increasing demand is fueling the booming polyurethane industry worldwide. An impeding issue for poly- urethane industry is how to handle the large quantity of hydrogen chloride byproduct generated from the synthesis o...Increasing demand is fueling the booming polyurethane industry worldwide. An impeding issue for poly- urethane industry is how to handle the large quantity of hydrogen chloride byproduct generated from the synthesis of intermediates, i.e., isocyanates. In the meantime, the traditional chloro-alkaline process sufibrs both from the high en- ergy intensity of electrolysis method and the disparity in the chlorine and caustic soda market. To solve these prob- lems, the state-of-the-art chlorine recycling technologies are reviewed and compared. Approaches for cost-effective utilization of chlorine in polyurethane industry are investigated. Chinese academies and enterprises＇ on-going effort on the development of a novel hydrogen chloride oxidation process for the synthesis of chlorine is presented. With this process, the closed loop recycling of chlorine can be realized. Tremendous economic, environmental and social bene- fits can be expected. A wide adoption of this technology will significantly advance the sustainable development of polyurethane industry.展开更多
During the ultra large scale integration （ULSI） process, the surface roughness of the polished silicon wafer plays an important role in the quality and rate of production of devices. In this work, the effects of oxi...During the ultra large scale integration （ULSI） process, the surface roughness of the polished silicon wafer plays an important role in the quality and rate of production of devices. In this work, the effects of oxidizer, surfactant, polyurethane pad and slurry additives on the surface roughness and topography of chemical-mechanical planarization （CMP） for silicon have been investigated. A standard atomic force microscopy （AFM） test method for the atomic scale smooth surface was proposed and used to measure the polished silicon surfaces. Finally, compared with the theoretical calculated Ra value of 0.0276 rim, a near-perfect silicon surface with the surface roughness at an atomic scale （0.5 4） was achieved based on an optimized CMP process.展开更多
A novel hyperbranched poly(urethane-tetrazole)(HPUTZ) was synthesized via the "A2+BB2' " approach using hexadiisocyanate(HDI) and 3-(bis-(2-hydroxyethyl)) aminopropyltetrazole(HAPTZ).The molecular struct...A novel hyperbranched poly(urethane-tetrazole)(HPUTZ) was synthesized via the "A2+BB2' " approach using hexadiisocyanate(HDI) and 3-(bis-(2-hydroxyethyl)) aminopropyltetrazole(HAPTZ).The molecular structure was characterized by FTIR and 1H NMR spectroscopy.The number average molecular weight was measured to be 1.05×104 g/mol with a polydispersity of 1.27 by GPC analysis.The HPUTZ was further cured by the semi-adduct(PEG-IPDI) from polyethylene glycol(PEG) reacting with isophorone diisocyanate(IPDI) to form the crosslinked HAPTZ-PU film in different ratio of HAPTZ to PEG-IPDI.The glass transition temperature of HAPTZ-PU increased from 44.9 to 56.4 ℃ as the HPUTZ content increased from 20% to 33% from the DSC analysis.The DMA results indicated that the HPUTZ-PU with 20% HPUTZ possessed the highest storage modulus and loss tangent.However,the storage modulus increased with the increasing of HPUTZ segment at higher temperature.The shape memory study showed that all the films presented the excellent shape memory function.Over 98% shape recovery could be obtained for the HAPTZ-PU with 20%-33% HAPTZ segment content within 60 s in the tension deformation test and within 40 s at 80 ℃ in the bend deformation test.展开更多
An efficient method for the synthesis of N-Cbz-β-aminoalkanesulfonamides was described.N-Cbz-β-aminoalkanesulfonamides were readily prepared in good yields from a variety of amino alcohols,including optically active...An efficient method for the synthesis of N-Cbz-β-aminoalkanesulfonamides was described.N-Cbz-β-aminoalkanesulfonamides were readily prepared in good yields from a variety of amino alcohols,including optically active ones,via N-Cbz protection with benzyl chloroformate,Mitsunobu esterification reaction with thiolacetic acid,N-chlorosuccinimide oxidation,and ammonolysis process.展开更多
Scaffolds play a crucial role in tissue engineering. Biodegradable polymers with great processing flexibility are the predominant scaffolding materials. Synthetic biodegradable polymers with well-defined structure and...Scaffolds play a crucial role in tissue engineering. Biodegradable polymers with great processing flexibility are the predominant scaffolding materials. Synthetic biodegradable polymers with well-defined structure and without immunological concerns associated with naturally derived polymers are widely used in tissue engineering. The synthetic biodegradable polymers that are widely used in tissue engineering, including polyesters, polyanhydrides, polyphosphazenes, polyurethane, and poly(glycerol sebacate) are summarized in this article. New developments in conducting polymers, photoresponsive polymers, amino-acid-based polymers, enzymatically degradable polymers, and peptide-activated polymers are also discussed. In addition to chemical functionalization, the scaffold designs that mimic the nano and micro features of the extracellular matrix(ECM) are presented as well, and composite and nanocomposite scaffolds are also reviewed.展开更多
文摘基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量白酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。实验对HS-SPME方法进行了优化,在酒精度12%vol、加NaCl 3 g、萃取温度70℃,萃取时间40 min的条件下,能够显著提高目标物的响应值。实验以D_(5)-氨基甲酸乙酯(D_(5)-EC)为内标,对不同浓度的样品溶液进行GC×GC-TOFMS定量分析。结果表明,EC在10~500μg/L范围内线性关系良好,回归系数(R^(2))>0.998,检出限为0.19μg/L,定量限为0.64μg/L,平均回收率为97.57%,精密度为8.66%。测定结果与国标方法相比无显著性差异(P>0.05)。该方法前处理简单,检测灵敏度更高,为白酒中EC自动化定量测定提供了新思路。
文摘It was investigated that the reaction of 4,4′-diphenylmethanediamine(MDA)with CO2 and bromoethane to synthesize diethyl 4,4′-diphenylmethanedicarbamate(MDC)under the catalysis of Cs2CO3 cooperating with DBU in supercritical carbon dioixide.The optimum reaction conditions were MDA(10mmol),EtBr(30mmol),Cs2CO3(6mmol)as catalyst cooperating with DBU(30mmol),a temperature of 60 °C,a pressure of 8 MPa,and a reaction time of 4 hours.MDC was obtained in the yield of 88% under the optimum reaction condtions.
基金financial supports from the Open Foundation of State Key Laboratory of Mineral Processing,China (Nos.BGRIMM-KJSKL-2019-06,BGRIMMKJSKL-2022-13)the Open Fund of State Key Laboratory of Comprehensive Utilization of Low-Grade,China (No.ZJKY2017(B)KFJJ003)。
文摘As a novel collector, O-isopropyl-N,N-diethyl thionocarbamate(IPDTC) was designed and synthesized for copper-sulfur flotation separation. Density functional theory calculations were performed to investigate the electronic structures of IPDTC. The results showed that IPDTC had higher energy of the highest occupied molecular orbital but lower electronegativity than O-isopropyl-N-ethyl thionocarbamate(Z-200). It was predicted that IPDTC had strong collection ability according to the reaction energy criteria. Flotation results demonstrated that the collecting ability of IPDTC to chalcopyrite and pyrite was stronger than that of Z-200. Then, the flotation mechanism was analyzed by measurements of surface tension, adsorption capacity, XPS, FTIR and zeta potential. These results indicated that IPDTC could reduce the solution surface tension. The adsorption capacity of IPDTC on chalcopyrite was higher than that on pyrite, consistent with the results of the flotation tests. FTIR, zeta potential and XPS results also demonstrated that IPDTC was strongly absorbed on the chalcopyrite surface by formation of Cu—S—C bonds, but showed a weak affinity on the pyrite surface.
文摘Tung oil-based polyols were synthesized by the esterification and transesterification between Tung oilbased anhydride and butanediol. The hydroxyl values of the polyols prepared were tested and discussed. Polyurethane was prepared by using Tung oil-based polyols and/or poly(propylene glycol) as polyols and by using isophorone diisocyanate as isocyanate. The effect of the ratio of Tung oil-based polyols to poly(propylene glycol) on the properties of polyurethane prepared was investigated by the water resistance, alcohol resistance and hardness tests. The results show that Tung oil-based polyols are effective to improve the hardness, water resistance and alcohol resistance of polyurethane.
文摘Water-dispersed polyurethane (PU) adhesive is a novel and highly efficient adhesive with broad application potential. In this study, the key parameters affecting the synthesis and application of this adhesive were examined, and optimal conditions were identified. The water-dispersed PU adhesive was successfully synthesized, and applied in the fastness test of pigment printing on cotton fabric. The data demonstrated that all the fastnesses of PU adhesive were better than that of the conventional PA one.
文摘Increasing demand is fueling the booming polyurethane industry worldwide. An impeding issue for poly- urethane industry is how to handle the large quantity of hydrogen chloride byproduct generated from the synthesis of intermediates, i.e., isocyanates. In the meantime, the traditional chloro-alkaline process sufibrs both from the high en- ergy intensity of electrolysis method and the disparity in the chlorine and caustic soda market. To solve these prob- lems, the state-of-the-art chlorine recycling technologies are reviewed and compared. Approaches for cost-effective utilization of chlorine in polyurethane industry are investigated. Chinese academies and enterprises＇ on-going effort on the development of a novel hydrogen chloride oxidation process for the synthesis of chlorine is presented. With this process, the closed loop recycling of chlorine can be realized. Tremendous economic, environmental and social bene- fits can be expected. A wide adoption of this technology will significantly advance the sustainable development of polyurethane industry.
基金supported by the Science Fund for Creative Research Groups(Grant No.51021064)the National Natural Science Foundation of China(Grant No.51205226)
文摘During the ultra large scale integration （ULSI） process, the surface roughness of the polished silicon wafer plays an important role in the quality and rate of production of devices. In this work, the effects of oxidizer, surfactant, polyurethane pad and slurry additives on the surface roughness and topography of chemical-mechanical planarization （CMP） for silicon have been investigated. A standard atomic force microscopy （AFM） test method for the atomic scale smooth surface was proposed and used to measure the polished silicon surfaces. Finally, compared with the theoretical calculated Ra value of 0.0276 rim, a near-perfect silicon surface with the surface roughness at an atomic scale （0.5 4） was achieved based on an optimized CMP process.
基金support of the National Natural Science Foundation of China (50633010) is gratefully acknowledged
文摘A novel hyperbranched poly(urethane-tetrazole)(HPUTZ) was synthesized via the "A2+BB2' " approach using hexadiisocyanate(HDI) and 3-(bis-(2-hydroxyethyl)) aminopropyltetrazole(HAPTZ).The molecular structure was characterized by FTIR and 1H NMR spectroscopy.The number average molecular weight was measured to be 1.05×104 g/mol with a polydispersity of 1.27 by GPC analysis.The HPUTZ was further cured by the semi-adduct(PEG-IPDI) from polyethylene glycol(PEG) reacting with isophorone diisocyanate(IPDI) to form the crosslinked HAPTZ-PU film in different ratio of HAPTZ to PEG-IPDI.The glass transition temperature of HAPTZ-PU increased from 44.9 to 56.4 ℃ as the HPUTZ content increased from 20% to 33% from the DSC analysis.The DMA results indicated that the HPUTZ-PU with 20% HPUTZ possessed the highest storage modulus and loss tangent.However,the storage modulus increased with the increasing of HPUTZ segment at higher temperature.The shape memory study showed that all the films presented the excellent shape memory function.Over 98% shape recovery could be obtained for the HAPTZ-PU with 20%-33% HAPTZ segment content within 60 s in the tension deformation test and within 40 s at 80 ℃ in the bend deformation test.
基金the support from the National Natural Science Foundation of China(20973013)Beijing Natural Science Foundation(2092022)
文摘An efficient method for the synthesis of N-Cbz-β-aminoalkanesulfonamides was described.N-Cbz-β-aminoalkanesulfonamides were readily prepared in good yields from a variety of amino alcohols,including optically active ones,via N-Cbz protection with benzyl chloroformate,Mitsunobu esterification reaction with thiolacetic acid,N-chlorosuccinimide oxidation,and ammonolysis process.
基金the financial support of the US National Institutes of Health(NIDCR DE015384,DE017689,DE022327)DOD(W81XWH-12-2-0008)+1 种基金the National Science Foundation of the United States(DMR-1206575)the National Natural Science Foundation of China(21304073)
文摘Scaffolds play a crucial role in tissue engineering. Biodegradable polymers with great processing flexibility are the predominant scaffolding materials. Synthetic biodegradable polymers with well-defined structure and without immunological concerns associated with naturally derived polymers are widely used in tissue engineering. The synthetic biodegradable polymers that are widely used in tissue engineering, including polyesters, polyanhydrides, polyphosphazenes, polyurethane, and poly(glycerol sebacate) are summarized in this article. New developments in conducting polymers, photoresponsive polymers, amino-acid-based polymers, enzymatically degradable polymers, and peptide-activated polymers are also discussed. In addition to chemical functionalization, the scaffold designs that mimic the nano and micro features of the extracellular matrix(ECM) are presented as well, and composite and nanocomposite scaffolds are also reviewed.
