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2020 Volume 37 Issue 1
2020, 37(1): 1-15
doi: 10.11944/j.issn.1000-0518.2020.01.190199
Abstract:
The catalytic performance of zeolite is mainly dependent on its acidic properties. The accurately and quantitatively distinguishing acid type, density, strength and site distribution of acid is significant to clarify the catalytic performance of zeolites. Here, we summarize the recent advances in the qualitative and quantitative analytic methods for acid site distribution, acid type and acid strengths.
The catalytic performance of zeolite is mainly dependent on its acidic properties. The accurately and quantitatively distinguishing acid type, density, strength and site distribution of acid is significant to clarify the catalytic performance of zeolites. Here, we summarize the recent advances in the qualitative and quantitative analytic methods for acid site distribution, acid type and acid strengths.
2020, 37(1): 16-23
doi: 10.11944/j.issn.1000-0518.2020.01.190150
Abstract:
An efficient green-yellow light iridium complex based on 2-(4-brominephenyl)-1-octyl-benzimidazole as cyclometalated ligand and 3-bromine-5-(pyridin-2-yl)-1H-1, 2, 4-triazole as ancillary ligand was synthesized. A series of novel star-shape phosphorescent polymers (P2.5, P5.0 and P10) was synthesized by employing the iridium complex as the core guest and the poly(fluorine-carbazole) as the arm host through Suzuki cross-coupling. The properties of the iridium complex and polymers were studied. The results showed that the iridium complex emitted green-yellow light with peaks at 490, 526 and 565 nm and its fluorescent quantum efficiency was 32.06%. Fluorescent lifetimes for the iridium complex and the polymers are in the microsecond regime (1.09~3.93 s). Such long-lived excited states clearly suggest that the emitting state has triplet phosphorescent emission. The yellow light intensity was enhanced with the increasing of iridium complex content, indicating that there exists partial energy transfer from host to guest, and the emission color of polymers shifts from blue to yellow by adjusting the proportion of the iridium complex. When the mole fraction of iridium complex reached to 2.5%, the white-light polymer (P2.5) was obtained, the CIE1931 chromaticity coordinate was (0.30, 0.32), the highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) energy levels were 5.49 and 2.43 eV respectively, fluorescent quantum efficiency was 14.3%, and fluorescent lifetime was 2.22 s. The polymer having good thermal stability can satisfy the requirements of luminescent materials.
An efficient green-yellow light iridium complex based on 2-(4-brominephenyl)-1-octyl-benzimidazole as cyclometalated ligand and 3-bromine-5-(pyridin-2-yl)-1H-1, 2, 4-triazole as ancillary ligand was synthesized. A series of novel star-shape phosphorescent polymers (P2.5, P5.0 and P10) was synthesized by employing the iridium complex as the core guest and the poly(fluorine-carbazole) as the arm host through Suzuki cross-coupling. The properties of the iridium complex and polymers were studied. The results showed that the iridium complex emitted green-yellow light with peaks at 490, 526 and 565 nm and its fluorescent quantum efficiency was 32.06%. Fluorescent lifetimes for the iridium complex and the polymers are in the microsecond regime (1.09~3.93 s). Such long-lived excited states clearly suggest that the emitting state has triplet phosphorescent emission. The yellow light intensity was enhanced with the increasing of iridium complex content, indicating that there exists partial energy transfer from host to guest, and the emission color of polymers shifts from blue to yellow by adjusting the proportion of the iridium complex. When the mole fraction of iridium complex reached to 2.5%, the white-light polymer (P2.5) was obtained, the CIE1931 chromaticity coordinate was (0.30, 0.32), the highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) energy levels were 5.49 and 2.43 eV respectively, fluorescent quantum efficiency was 14.3%, and fluorescent lifetime was 2.22 s. The polymer having good thermal stability can satisfy the requirements of luminescent materials.
2020, 37(1): 24-31
doi: 10.11944/j.issn.1000-0518.2020.01.190295
Abstract:
Non-fullerene small molecule acceptor (ITIC) is introduced into the binary polymer solar cells (PBTIBDTT:PCBM[70]) to build ternary polymer solar cells, which achieves power conversion efficiency (PCE) of 10.95% with more than 200 nm thickness of photoactive layers. The ternary polymer solar cells are further fabricated by spray coating method, and realize 9.06% of PCE. The high efficiency ternary polymer solar cells fabricated by spray coating are suitable for the roll-to-roll printing, exhibiting great application prospects.
Non-fullerene small molecule acceptor (ITIC) is introduced into the binary polymer solar cells (PBTIBDTT:PCBM[70]) to build ternary polymer solar cells, which achieves power conversion efficiency (PCE) of 10.95% with more than 200 nm thickness of photoactive layers. The ternary polymer solar cells are further fabricated by spray coating method, and realize 9.06% of PCE. The high efficiency ternary polymer solar cells fabricated by spray coating are suitable for the roll-to-roll printing, exhibiting great application prospects.
2020, 37(1): 32-39
doi: 10.11944/j.issn.1000-0518.2020.01.190152
Abstract:
In this paper, the curing kinetics of two-component addition silicone rubber on different polyvinyl chloride (PVC) skins was studied with rheological method. The components of PVC skins were analyzed to determine the mechanism of uncuring of two-component addition silicone rubber by using Fourier transform infrared spectrometer (FTIR), nuclear magnetic resonance (NMR), and inductively coupled plasma mass spectrometer (ICP-MS). The results show that phosphorus (P) is the main element in the PVC skin that causes the difficulty in curing of silicone rubber. At the fixed silicone rubber thickness of 1 mm, when the content(mass fraction) of P element in the PVC is below 3×10-3%, the two-component addition silicone rubber casted on the PVC skin can still be solidified completely; when the content of P in the PVC skin exceeds about 2.4×10-2%, although the intermediate layer of two-component addition silicone rubber can be cured, the layer contacting PVC skins fails to cure, and the thickness of the uncured layer increases with the content of P. Besides, reducing the thickness of silicone rubber to micron on the skin of PVC with P element content less than 3×10-3%, especially less than 2 μm, the silicone rubber can not cure completely. The consequences mentioned above indicate that the curing behavior of two-component addition silicone rubber on the surface of PVC skin containing P element is mainly influenced by the total content of platinum catalyst in silicone rubber and the content of P element in PVC skin, while the reaction rate of two-component addition silicone rubber and diffusion rates of platinum catalyst and P element in the silicone rubber have ffects as well.
In this paper, the curing kinetics of two-component addition silicone rubber on different polyvinyl chloride (PVC) skins was studied with rheological method. The components of PVC skins were analyzed to determine the mechanism of uncuring of two-component addition silicone rubber by using Fourier transform infrared spectrometer (FTIR), nuclear magnetic resonance (NMR), and inductively coupled plasma mass spectrometer (ICP-MS). The results show that phosphorus (P) is the main element in the PVC skin that causes the difficulty in curing of silicone rubber. At the fixed silicone rubber thickness of 1 mm, when the content(mass fraction) of P element in the PVC is below 3×10-3%, the two-component addition silicone rubber casted on the PVC skin can still be solidified completely; when the content of P in the PVC skin exceeds about 2.4×10-2%, although the intermediate layer of two-component addition silicone rubber can be cured, the layer contacting PVC skins fails to cure, and the thickness of the uncured layer increases with the content of P. Besides, reducing the thickness of silicone rubber to micron on the skin of PVC with P element content less than 3×10-3%, especially less than 2 μm, the silicone rubber can not cure completely. The consequences mentioned above indicate that the curing behavior of two-component addition silicone rubber on the surface of PVC skin containing P element is mainly influenced by the total content of platinum catalyst in silicone rubber and the content of P element in PVC skin, while the reaction rate of two-component addition silicone rubber and diffusion rates of platinum catalyst and P element in the silicone rubber have ffects as well.
2020, 37(1): 40-45
doi: 10.11944/j.issn.1000-0518.2020.01.190153
Abstract:
The effect of the mass fraction of super absorbent resin on the adhesion of wood board was studied. The concentration range of the gel formed by the sample was determined by the rheological method and inverted experiment. The maximum water absorption ratio of the superabsorbent polymer was measured and the water absorption saturation concentration was determined. Through the simulation of the fire engine spray gun to the scene of the fire scene, the sample was sprayed to determine the adhesion performance of the gel on the fixed area of the board. The results show that the adhesion performance of the superabsorbent resin is related to its mass fraction. As the concentration increases, the adhesion performance of the sample increases. When the mass fraction of the superabsorbent resin sample reaches its gel mass fraction, the adhesion performance is greatly improved. When the increase is continued, the adhesion performance is increased to a small extent, and the adhesion layer falls off in a monolith due to the gravity.
The effect of the mass fraction of super absorbent resin on the adhesion of wood board was studied. The concentration range of the gel formed by the sample was determined by the rheological method and inverted experiment. The maximum water absorption ratio of the superabsorbent polymer was measured and the water absorption saturation concentration was determined. Through the simulation of the fire engine spray gun to the scene of the fire scene, the sample was sprayed to determine the adhesion performance of the gel on the fixed area of the board. The results show that the adhesion performance of the superabsorbent resin is related to its mass fraction. As the concentration increases, the adhesion performance of the sample increases. When the mass fraction of the superabsorbent resin sample reaches its gel mass fraction, the adhesion performance is greatly improved. When the increase is continued, the adhesion performance is increased to a small extent, and the adhesion layer falls off in a monolith due to the gravity.
2020, 37(1): 46-53
doi: 10.11944/j.issn.1000-0518.2020.01.190209
Abstract:
In this study, thermally conductive phase change composites materials was prepared based on polyethylene glycol (PEG) and inorganic fillers via the molten blending method. The microstructure, thermal conductivity and phase transition performance of the prepared composites were investigated by scanning electronic microscopy (SEM), thermal constant analyzer, differential scanning calorimetry (DSC), infrared thermal imaging and thermogravimetric analysis. The results show that, compared with calcium carbonate and alumina, boron nitride can more significantly improve the thermal conductivity of PEG at the same mass fraction. When the mass fraction of BN is 40%, the thermal conductivity of composites can reach 3.40 W/(m·K). Simultaneously, flake boron nitride can effectively limit the leakage of PEG and maintain the initially shapes well upon long time heating, and maintain the shape stability of the composite.
In this study, thermally conductive phase change composites materials was prepared based on polyethylene glycol (PEG) and inorganic fillers via the molten blending method. The microstructure, thermal conductivity and phase transition performance of the prepared composites were investigated by scanning electronic microscopy (SEM), thermal constant analyzer, differential scanning calorimetry (DSC), infrared thermal imaging and thermogravimetric analysis. The results show that, compared with calcium carbonate and alumina, boron nitride can more significantly improve the thermal conductivity of PEG at the same mass fraction. When the mass fraction of BN is 40%, the thermal conductivity of composites can reach 3.40 W/(m·K). Simultaneously, flake boron nitride can effectively limit the leakage of PEG and maintain the initially shapes well upon long time heating, and maintain the shape stability of the composite.
2020, 37(1): 54-60
doi: 10.11944/j.issn.1000-0518.2020.01.190131
Abstract:
Silver nanoclusters have special physical and chemical properties and wide potential applications. In this paper, a method of rapid preparation of stable silver nanoclusters with strong fluorescence characteristics and small particle size was developed by using chromotropic acid 2R as the stabilizer and pH regulation twice. Under the optimal experimental conditions, the maximum emission wavelength of silver nanoclusters prepared is 450 nm, the maximum excitation wavelength is 336 nm, and the average particle size is 1.74 nm. The main particles are distributed in the region of 0.68~2.99 nm, the lattice spacing of the silver nanocluster is 0.223 nm, and the lattice type is (102). The silver nanoclusters can be used as probes for the determination of trace heavy metal ions, non-metallic ions in solutions and small molecules, the detection of weak acid concentration, and cell imaging.
Silver nanoclusters have special physical and chemical properties and wide potential applications. In this paper, a method of rapid preparation of stable silver nanoclusters with strong fluorescence characteristics and small particle size was developed by using chromotropic acid 2R as the stabilizer and pH regulation twice. Under the optimal experimental conditions, the maximum emission wavelength of silver nanoclusters prepared is 450 nm, the maximum excitation wavelength is 336 nm, and the average particle size is 1.74 nm. The main particles are distributed in the region of 0.68~2.99 nm, the lattice spacing of the silver nanocluster is 0.223 nm, and the lattice type is (102). The silver nanoclusters can be used as probes for the determination of trace heavy metal ions, non-metallic ions in solutions and small molecules, the detection of weak acid concentration, and cell imaging.
2020, 37(1): 61-68
doi: 10.11944/j.issn.1000-0518.2020.01.190161
Abstract:
Firstly, Pd2+ ions are anchored on melamine-formaldehyde prepolymer by the coordination with N atoms on the prepolymer. Then the colloidal nanospheres grow on silica hydrogel via the simultaneous condensation reaction accelerated by 2, 4-diaminobenzenesulfonic acid. Finally, the carbon-supported highly dispersed palladiumPd@C catalyst is obtained after calcination in an atmosphere of 5%(molar fraction) H2 and 95%(molar fraction) N2 gases, followed by being treated with 5% HF solution. The prepared highly dispersed Pd nanoparticles with a loading amount of 1.37%(mass fraction) have an average diameter of (2.4±0.87) nm, and the catalytic performance of Pd@C has been further evaluated by Suzuki reaction. With the addition of molar ratio 1:100 catalyst, Pd@C performs both good catalytic activity with a yield of 99.3% achieved within 5 minutes, and excellent durability after 8 cycles.
Firstly, Pd2+ ions are anchored on melamine-formaldehyde prepolymer by the coordination with N atoms on the prepolymer. Then the colloidal nanospheres grow on silica hydrogel via the simultaneous condensation reaction accelerated by 2, 4-diaminobenzenesulfonic acid. Finally, the carbon-supported highly dispersed palladiumPd@C catalyst is obtained after calcination in an atmosphere of 5%(molar fraction) H2 and 95%(molar fraction) N2 gases, followed by being treated with 5% HF solution. The prepared highly dispersed Pd nanoparticles with a loading amount of 1.37%(mass fraction) have an average diameter of (2.4±0.87) nm, and the catalytic performance of Pd@C has been further evaluated by Suzuki reaction. With the addition of molar ratio 1:100 catalyst, Pd@C performs both good catalytic activity with a yield of 99.3% achieved within 5 minutes, and excellent durability after 8 cycles.
2020, 37(1): 69-79
doi: 10.11944/j.issn.1000-0518.2020.01.190121
Abstract:
Nanoparticle drug delivery system has played an important role in enhancing the efficacy of traditional chemotherapy drugs in recent years. However, the main challenges faced by conventional nanoparticle include poor biocompatibility, low specific targeting and slow drug release in target sites. In this work, we fabricated an efficient hepatocellular carcinoma-targeting liposome system functionalized with a redox-cleavable and homologous cell membrane(M)-targeting. The blank (P-ss-G/D@M) and drug-loaded (P-ss-G/D/Sf@M) nanoparticles coated with cell membrane were prepared by thin-film hydration method combined with electrostatic adsorption and membrane extrusion. The drug-loading amount of sorafenib was 7.2%, and the encapsulation efficiency was 79.9%. The results of in vitro drug release showed that P-ss-G/D/Sf@M accelerated drug release under reducing conditions, and the drug release rate was more than 65% at 48 hours, which was 25% higher than that under non-reducing conditions. In vitro study demonstrated that nanoparticles coated with hepatoma cell membrane were more easily taken into hepatoma cells, showing the targeting of hepatocellular carcinoma. At the same time, the disulfide bonds in the nanoparticles broke and drugs were rapidly released under the high concentration of glutathione (GSH) in the tumor cells. Compared with non-reducing sensitive drug-loaded nanoparticles, P-ss-G/D/Sf@M could significantly inhibit the growth of hepatoma cells (Hep-G2) and increase the apoptosis rate of hepatoma cells. Therefore, the homologous cell membrane-coated smart drug delivery carrier prepared herein is likely to be used to treat hepatocellular carcinoma in future.
Nanoparticle drug delivery system has played an important role in enhancing the efficacy of traditional chemotherapy drugs in recent years. However, the main challenges faced by conventional nanoparticle include poor biocompatibility, low specific targeting and slow drug release in target sites. In this work, we fabricated an efficient hepatocellular carcinoma-targeting liposome system functionalized with a redox-cleavable and homologous cell membrane(M)-targeting. The blank (P-ss-G/D@M) and drug-loaded (P-ss-G/D/Sf@M) nanoparticles coated with cell membrane were prepared by thin-film hydration method combined with electrostatic adsorption and membrane extrusion. The drug-loading amount of sorafenib was 7.2%, and the encapsulation efficiency was 79.9%. The results of in vitro drug release showed that P-ss-G/D/Sf@M accelerated drug release under reducing conditions, and the drug release rate was more than 65% at 48 hours, which was 25% higher than that under non-reducing conditions. In vitro study demonstrated that nanoparticles coated with hepatoma cell membrane were more easily taken into hepatoma cells, showing the targeting of hepatocellular carcinoma. At the same time, the disulfide bonds in the nanoparticles broke and drugs were rapidly released under the high concentration of glutathione (GSH) in the tumor cells. Compared with non-reducing sensitive drug-loaded nanoparticles, P-ss-G/D/Sf@M could significantly inhibit the growth of hepatoma cells (Hep-G2) and increase the apoptosis rate of hepatoma cells. Therefore, the homologous cell membrane-coated smart drug delivery carrier prepared herein is likely to be used to treat hepatocellular carcinoma in future.
2020, 37(1): 80-87
doi: 10.11944/j.issn.1000-0518.2020.01.190165
Abstract:
Two novel anthracene-benzimidazolium based receptors 1 and 2 were synthesized. The anion (F-, Cl-, Br-, I-, AcO-, HSO4-, H2PO4-, ClO4-, NO3-) binding properties of receptors 1 and 2 were evaluated in acetonitrile by fluorescence spectroscopy. The receptors 1 and 2 display fluorescent quenching effect with H2PO4-, the quench percentage for receptor 1 is 13%, and for receptor 2 is as much as 94%. The results indicate that receptor 2 is more closely matched to H2PO4- in configuration, and receptor 2 can behave as a "turn-off" fluorescence sensor for H2PO4-. Job-plot shows that receptor 2 and H2PO4- form a 1:1 complex, the binding constant is (3.70±0.16)×104 L/mol, and the detection limit is 3.77×10-6 mol/L.
Two novel anthracene-benzimidazolium based receptors 1 and 2 were synthesized. The anion (F-, Cl-, Br-, I-, AcO-, HSO4-, H2PO4-, ClO4-, NO3-) binding properties of receptors 1 and 2 were evaluated in acetonitrile by fluorescence spectroscopy. The receptors 1 and 2 display fluorescent quenching effect with H2PO4-, the quench percentage for receptor 1 is 13%, and for receptor 2 is as much as 94%. The results indicate that receptor 2 is more closely matched to H2PO4- in configuration, and receptor 2 can behave as a "turn-off" fluorescence sensor for H2PO4-. Job-plot shows that receptor 2 and H2PO4- form a 1:1 complex, the binding constant is (3.70±0.16)×104 L/mol, and the detection limit is 3.77×10-6 mol/L.
2020, 37(1): 88-95
doi: 10.11944/j.issn.1000-0518.2020.01.190180
Abstract:
A simple fluorescence probe based on benzoindole (H) was designed and synthesized. The recognition performance of the probe for metal cations was studied by ultraviolet-visible absorption spectrophotometry (UV-Vis) and fluorescence emission spectra. The results show that probe H in the mixed system of ethanol (EtOH) and 4-(2-hydroxyethyl)piperazine-1-ethanesulfonic acid(HEPES)(pH=7.4)(volume ratio 1:1) has specific recognition of Al3+ and is not impacted by other metal cations. The complex ratio of probe H and Al3+ is 1:1, the association constant Ka is 0.52×102 mol/L and the detection limit is 1.75 μmol/L. The quantitative detection of Al3+ in water and food samples proves that the probe has potential applications.
A simple fluorescence probe based on benzoindole (H) was designed and synthesized. The recognition performance of the probe for metal cations was studied by ultraviolet-visible absorption spectrophotometry (UV-Vis) and fluorescence emission spectra. The results show that probe H in the mixed system of ethanol (EtOH) and 4-(2-hydroxyethyl)piperazine-1-ethanesulfonic acid(HEPES)(pH=7.4)(volume ratio 1:1) has specific recognition of Al3+ and is not impacted by other metal cations. The complex ratio of probe H and Al3+ is 1:1, the association constant Ka is 0.52×102 mol/L and the detection limit is 1.75 μmol/L. The quantitative detection of Al3+ in water and food samples proves that the probe has potential applications.
2020, 37(1): 96-102
doi: 10.11944/j.issn.1000-0518.2020.01.190136
Abstract:
Based on luminol chemiluminescence system, a self-developed online ozone concentration detector was used to establish a real-time online method for detecting ozone concentration for the determination of ozone gas at trace level. The effects of luminol, potassium hydroxide, alcohols and surfactants on the chemiluminescence intensity were investigated. The results showed that ethylene glycol (volume fraction 1.5%), methanol (volume fraction 1.5%), ethanol (volume fraction 1.0%), and glycerol (volume fraction 3.0%) were added to luminol (0.005 mol/L) and potassium hydroxide (0.05 mol/L) can significantly enhance the luminescence signal of O3 in the luminol system, and formaldehyde (volume fraction 3.0%) can effectively inhibit the interference of NO2 signal. At the same time, the detection limit of ozone was 1.26 μg/m3, the relative standard deviation was 0.32%, and the relative error was 0.75%. This ozone determination system has the advantages of stable signal, good precision, high accuracy and low detection limit. It is suitable for online continuous detection of trace O3 in the atmosphere.
Based on luminol chemiluminescence system, a self-developed online ozone concentration detector was used to establish a real-time online method for detecting ozone concentration for the determination of ozone gas at trace level. The effects of luminol, potassium hydroxide, alcohols and surfactants on the chemiluminescence intensity were investigated. The results showed that ethylene glycol (volume fraction 1.5%), methanol (volume fraction 1.5%), ethanol (volume fraction 1.0%), and glycerol (volume fraction 3.0%) were added to luminol (0.005 mol/L) and potassium hydroxide (0.05 mol/L) can significantly enhance the luminescence signal of O3 in the luminol system, and formaldehyde (volume fraction 3.0%) can effectively inhibit the interference of NO2 signal. At the same time, the detection limit of ozone was 1.26 μg/m3, the relative standard deviation was 0.32%, and the relative error was 0.75%. This ozone determination system has the advantages of stable signal, good precision, high accuracy and low detection limit. It is suitable for online continuous detection of trace O3 in the atmosphere.
2020, 37(1): 103-108
doi: 10.11944/j.issn.1000-0518.2020.01.190185
Abstract:
An organic salt of etodolac and piperazine was prepared and the crystal structure was obtained. Structural analysis indicated that a hydrogen proton transferred from etodolac carboxyl group to piperazine nitrogen atom. The N-H…O hydrogen bond was the main intermolecular interaction to maintain structural stability. The intrinsic dissolution rate and equilibrium solubility of the newly synthesized salt were increased by 2.1 times and 4.8 times, respectively, compared with the original etodolac. In addition, the newly synthesized salt has good hydration stability without phase transition for 4 weeks at 25℃ and 95% relative humidity. As the first organic salt of etodolac, the etodolac-piperazine salt is a promising new solid form of etodolac.
An organic salt of etodolac and piperazine was prepared and the crystal structure was obtained. Structural analysis indicated that a hydrogen proton transferred from etodolac carboxyl group to piperazine nitrogen atom. The N-H…O hydrogen bond was the main intermolecular interaction to maintain structural stability. The intrinsic dissolution rate and equilibrium solubility of the newly synthesized salt were increased by 2.1 times and 4.8 times, respectively, compared with the original etodolac. In addition, the newly synthesized salt has good hydration stability without phase transition for 4 weeks at 25℃ and 95% relative humidity. As the first organic salt of etodolac, the etodolac-piperazine salt is a promising new solid form of etodolac.
2020, 37(1): 109-116
doi: 10.11944/j.issn.1000-0518.2020.01.190200
Abstract:
Silica coated bismuth-based yellow pigments with better acid resistance and temperature stability were successfully prepared by hydrolysis method using Bi0.82V0.45Mo0.55O4 and Na0.5Bi0.5(MoO4) prepared by precipitation method. The as-obtained pigments were characterized by X-ray diffraction(XRD), transmission electron microscopy(TEM), X-ray fluorescence spectrometer(XRF) and Fourier transform infrared spectroscopy(FT-IR). The results showed that compact and uniform amorphous SiO2·xH2O coating layers with the thickness of around 100 nm were obtained under the volume ratio of H2O to TEOS was 18, the ratio of n(Si)/n(Bi) was 4, Tb was 45℃, and vd ≤ 0.3 mL/min. The coated pigments showed the nature of bright yellow, and the values of L*, a* and b* were 78.85, -6.85 and 71.63, respectively. Compared with the uncoated pigments, the acid mass loss of coated pigments under the most optimized condition, after half an hour immersion in 1 mol/L hydrochloric acid, declined from 100% to 28.25% and the tolerable temperature was improved from 600℃ to 860℃.
Silica coated bismuth-based yellow pigments with better acid resistance and temperature stability were successfully prepared by hydrolysis method using Bi0.82V0.45Mo0.55O4 and Na0.5Bi0.5(MoO4) prepared by precipitation method. The as-obtained pigments were characterized by X-ray diffraction(XRD), transmission electron microscopy(TEM), X-ray fluorescence spectrometer(XRF) and Fourier transform infrared spectroscopy(FT-IR). The results showed that compact and uniform amorphous SiO2·xH2O coating layers with the thickness of around 100 nm were obtained under the volume ratio of H2O to TEOS was 18, the ratio of n(Si)/n(Bi) was 4, Tb was 45℃, and vd ≤ 0.3 mL/min. The coated pigments showed the nature of bright yellow, and the values of L*, a* and b* were 78.85, -6.85 and 71.63, respectively. Compared with the uncoated pigments, the acid mass loss of coated pigments under the most optimized condition, after half an hour immersion in 1 mol/L hydrochloric acid, declined from 100% to 28.25% and the tolerable temperature was improved from 600℃ to 860℃.
2020, 37(1): 117-122
doi: 10.11944/j.issn.1000-0518.2020.01.190160
Abstract:
A large amount of wastewater in the production process of 1, 2, 3, 9-tetrahydrocarbazol-4-one is generated and leads to severe harm. In this work, the effects and existing problems in oxidation treatment were investigated. Meanwhile, the new process route of high-temperature carbonization treatment was developed. The results show that the oxidation treatments with NaClO and H2O2 fail to achieve the desired effect, and the recycled solid is poor in color and has no catalytic activity. However, zinc chloride recovered through distilling at 143℃ and high-temperature carbonization at 500℃ for 40 min, exhibits excellent catalytic activity, which makes the conversion of monophenylhydrazone reach 52.6%. Ultimately, the reclamation of zinc chloride in the production of 1, 2, 3, 9-tetrahydrocarbazol-4-one is realized. At the same time, the experimental results provide a new way for the treatment of 1, 2, 3, 9-tetrahydrocarbazol-4-one production wastewater and comprehensive utilization of resources.
A large amount of wastewater in the production process of 1, 2, 3, 9-tetrahydrocarbazol-4-one is generated and leads to severe harm. In this work, the effects and existing problems in oxidation treatment were investigated. Meanwhile, the new process route of high-temperature carbonization treatment was developed. The results show that the oxidation treatments with NaClO and H2O2 fail to achieve the desired effect, and the recycled solid is poor in color and has no catalytic activity. However, zinc chloride recovered through distilling at 143℃ and high-temperature carbonization at 500℃ for 40 min, exhibits excellent catalytic activity, which makes the conversion of monophenylhydrazone reach 52.6%. Ultimately, the reclamation of zinc chloride in the production of 1, 2, 3, 9-tetrahydrocarbazol-4-one is realized. At the same time, the experimental results provide a new way for the treatment of 1, 2, 3, 9-tetrahydrocarbazol-4-one production wastewater and comprehensive utilization of resources.
