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2023 Vol.40 Issue.4,Published 2023-07-15
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2023 Vol. 40 (4): 0-0 [Abstract] ( 295 ) [HTML 1KB] [ PDF 859KB] ( 647 )
1 Study on Ru-based catalysts coordinated with pyridine N-oxide for acetylene hydrochlorination
HU Jiaqi, WANG Fumin, ZHANG Xubin
To enhance the activity and stability of Ru-based catalysts for acetylene hydrochlorination, wet impregnation technology was used to prepare a new Ru-based catalyst coordinated with pyridine N-oxide, and the dosage of ligand was optimized. Under the conditions of 170 ℃, GSHV(C2H2)=360 h-1 and V(HCl)/V(C2H2)=1.15, the activity of the catalyst with the optimal dosage of 10% pyridine N-oxide ligand reaches the conversion of 96.1%, which only decreases 0.8% within 20 h. Kinetic analysis shows that the activation energy of the reaction decreases from 34.95 kJ·mol-1 to 25.58 kJ·mol-1. The results of TEM and XRD prove that Ru is highly dispersed in the catalyst. Furthermore, H2-TPR and XPS results certify that the pyridine N-oxide weakens the reduction of oxidized Ru species during the reaction. Moreover, the introduction of pyridine N-oxide inhibits the coke deposition, according to BET and TG data. TPD result confirms that the ligand enhances the adsorption of reactants on catalysts. Besides, theoretical calculations based on the frontier molecular orbital theory indicate that Ru can act as a transfer of electrons and greatly reduce the energy difference. And the introduction of ligand further weakens the energy difference of Ru donating electrons to HCl, which may be the microcosmic mechanism of the synergy, consistent with the experimental results. It can provide theoretical inspiration for designs and applications of Ru-based catalysts in acetylene hydrochlorination.
2023 Vol. 40 (4): 1-14 [Abstract] ( 318 ) [HTML 1KB] [ PDF 13848KB] ( 535 )
15 Synthesis and properties of methoxy-modified planarized triphenylamine electron donor
ZHANG Ye, ZHOU Xueqin, LIU Dongzhi, LI Wei
Using methyl 2-aminobenzoate as starting material, the Ullmann reaction and nucleophilic addition reaction were used to obtain a methoxy-modified planarized triphenylamine electron donor CMo. The elucidation of chemical structure were proved by 1H NMR, compared with common electron donor triphenylamine TPA and indoline YD, the ultraviolet absorption spectrum shows that the maximum absorption wavelength of CMo is 304 nm, which is red-shifted compared to YD (298 nm) and TPA (297 nm), and the maximum absorption peak has a large change rate with the enhancement of polarity, indicating that CMo can be delocalized to a large extent and has better electron donating ability. Cyclic voltammetry test shows that HOMO energy level (-5.21 eV) and LUMO energy level (-1.48 eV) of CMo are higher than that of YD (-5.38 eV, -1.70 eV) and TPA (-5.53 eV, -1.79 eV), and can be used as a new electron donor material in organic optoelectronic devices.
2023 Vol. 40 (4): 15-22 [Abstract] ( 293 ) [HTML 1KB] [ PDF 3535KB] ( 948 )
23 Preparation and denitration performance of surface grafted CuMnCeOx loaded high silica filter media
ZHANG Yajing, DIAO Yongfa, JIANG Jie
In order to develop a loading method with more general application range and stronger loading strength, Si—O—Si bond was formed between the silicon alcohol formed by hydrolysis of silane coupling agent and the substrate surface of the material, and the coating layer was grafted on the fiber surface, so that the catalyst and filter material could be firmly combined. Its structure and properties were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD), infrared (FTIR) and CO-SCR activity evaluation. It could be seen from SEM photos that the catalyst was evenly dispersed on the filter material. The XRD spectrum of the composite filter material showed that the polymetallic composite oxide was loaded on the filter material in an amorphous state. In addition, the conversion of NOx of the composite filter material was 90%, when the mass ratio reached 0.25. The composite filter material had good NOx removal effect in the range of 200~260 ℃. Furthermore, during the continuous 10 h stability test, the catalytic efficiency of the composite filter material did not decrease significantly, showing great resistance of catalytic performance.

Guide: 
2023 Vol. 40 (4): 23-30 [Abstract] ( 298 ) [HTML 1KB] [ PDF 4806KB] ( 613 )
31 Preparation and characterization of new fluoropolyurethane elastomers
WANG Jie, GAO Shangdong, ZHANG Huishu, LYU Xuchen, XIAO Libai, REN Xiangkui
A series of fluoropolyurethane elastomers were prepared by introducing long-chain fluoropolyacrylate into polyurethane system through chemical bonds. The structure of the materials was confirmed by Fourier Infrared Spectroscopy. The aggregate structure, mechanical properties and hydrophobic properties of the materials were studied in detail by X-ray diffraction, stress-strain, differential scanning calorimetry and contact angle experiments. The experimental results show that the properties of fluoropolyurethane are closely related to the number of side chain fluorine atoms. With the increase of the number of fluorine atoms, the contact angle of polyurethane increases, the surface free energy decreases, and the hydrophobicity is significantly improved. At the same time, the crystallinity and mechanical properties of the material can be adjusted by the number of fluorine atoms in the side chain. When the number of fluorine atoms is 8, the fluoropolyurethane has the best mechanical property.
2023 Vol. 40 (4): 31-36 [Abstract] ( 304 ) [HTML 1KB] [ PDF 6433KB] ( 626 )
37 Particle collision behavior and heat transfer performance in a Na2SO4 circulating fluidized bed evaporator
JIANG Feng, XU Di, QI Guopeng, LI Xiulun
A Na2SO4 circulating fluidized bed evaporation apparatus is designed and built by combining the fluidized bed heat transfer and fouling prevention technology and the evaporation process of Na2SO4 solution. 20%(mass fraction) Na2SO4 solution is selected as the liquid working medium. Polyoxymethylene (POM) and silicon carbide (SiC) particles are selected as the inert solid particles. The effects of the operating parameters, such as particle type, the amount of added particles (1%~3%), circulation flow velocity (0.37~1.78 m·s-1) and heat flux (7.29~12.14 kW·m-2), on the particle collision behavior and heat transfer performance are investigated. The results show that the addition of the POM and SiC particles can enhance heat transfer. The maximum enhancement factors are 9.5% and 13.4% for the POM and SiC particles, respectively, and the corresponding operating parameters are ε =1%,u=1.78 m·s-1,q=7.29 kW·m-2和ε =3%,u=0.37 m·s-1,q=12.14 kW·m-2. The characteristic frequency ranges of the collision acceleration signals are 0~1 000 Hz and 6 000~17 000 Hz for the liquid phase and solid phase, respectively. The generation of the vapor phase significantly strengthens the collision intensity of other phases. The standard deviation of the POM particles increases with the increase in the amount of added particles. The standard deviation of the SiC particles initially decreases and then increases at low circulation flow velocity but increases at high circulation flow velocity with the increase in the amount of added particles. The amount of added particles slightly influences the heat transfer coefficients of the two kinds of particles. The standard deviations and heat transfer coefficients of the two kinds of particles increase with the increase in circulation flow velocity. The heat transfer coefficients of the two kinds of particles obviously decrease with the increase in heat flux. The heat flux has no obvious effect on the standard deviation at low amount of added particles. At high amount of added particles, the standard deviation of POM particles increases with the increase in heat flux; however, the variation trend of the standard deviation of the SiC particles with heat flux is dependent on the circulation flow velocity.
2023 Vol. 40 (4): 37-49 [Abstract] ( 297 ) [HTML 1KB] [ PDF 7536KB] ( 794 )
50 Pilot study of blended diesel hydrorefining based on micro-interfacial intensification technique
SONG Junchao, LI Zhi, LI Pengcheng, CHEN Qiang, LIU Jinlong, LI Liquan, ZHU Jianhua
Based on micro-interfacial intensification technique, a pilot study of diesel fuel hydrorefining were carried out using blended diesel fuels as feedstocks, by means of an up-flow reactor which packed 2 L catalyst. The effects of process parameters such as reaction pressure, reaction temperature, hydrogen-oil volume ratio, space velocity, etc. and catalyst types on the performances of micro-interface intensified hydrorefining of diesel fuel were investigated. The experimental results showed that the hydrodesulfurization performance of micro-interfacial intensification hydrogenation was significantly better than that in conventional up-flow reactor, the difference of which reduced as the sulfur contents of refined oil declined in the range of investigated process conditions. Compared to diesel hydrorefining by conventional up-flow reactor, using the blended diesel with sulfur content of 1.58% as feedstock oil and HRC-1 as catalyst, the reactor pressure of micro-interfacial intensification hydrorefining could reduce by more than 3 MPa when desulfurization rate was above 99.75%. Using the blended diesel with sulfur content of 1.02% as feedstock oil, and HRC-2 and HRC-3 as grading catalyst, the main quality indicators of refined oils such as sulfur content could satisfy the requirements of China national standard (VI) for automobile diesel fuels under the condition of space velocity of 0.8 h-1, reaction pressure of 5.7 MPa, reaction temperature of 365 ℃ and the hydrogen-oil volume ratio being greater than or equal to 500. This processing technique could provide a reference for industrial scale-up of micro-interfacial intensification hydrorefining of blended diesel under medium-low reaction pressure.
2023 Vol. 40 (4): 50-57 [Abstract] ( 327 ) [HTML 1KB] [ PDF 2379KB] ( 1067 )
58 Kinetics of semi-batch reaction crystallization of methionine under CO2 acidification condition
CHEN Zhirong, ZHANG Fujia, YUAN Shenfeng, YIN Hong
Aiming at the synthesis of methionine by hydantion method, using potassium methionine as raw material, the reaction crystallization process of methionine under CO2 acidification condition was studied by batch-dynamic method, and the crystallization kinetic model was established. The population number balance equation was solved by moment method, and the crystallization kinetic parameters were obtained by fitting the data with multiple linear regression using least square method. The results show that the crystal growth is size-independent, and growth activation energy is 21.0 kJ·mol-1. The exponents of supersaturation with respect to nucleation rate and growth rate are 0.62 and 1.52, respectively. The effect of crystal agglomeration on the crystallization process cannot be ignored. The apparent gas velocity and stirring speed have obvious effects on crystal nucleation and agglomeration. High supersaturation and high stirring speed are not conducive to the increase of average crystal size.
2023 Vol. 40 (4): 58-66 [Abstract] ( 312 ) [HTML 1KB] [ PDF 2335KB] ( 715 )
67 Research and application of solution crystallization thermodynamics and process analysis
HU Taotao, YANG Li, LIU Peng, CHENG Jingcai, FAN Yiqun, ZHANG Yan, YANG Chao
Crystallization is an important means of separation and purification. Many products in the fields of medicine, food, fertilizer and so on are in the form of crystals. Thermodynamics is the theoretical basis of the study of the crystallization process. The thermodynamic properties of the target system have an important influence on the selection of crystallization methods (cooling crystallization, evaporative crystallization, anti-solvent crystallization, etc.), while the thermodynamic equilibrium relationship determines the limit of crystallization yield and the stability of different crystal forms under specific conditions. Therefore, the research of thermodynamics has important guiding significance for the optimization and amplification design of the crystallization process. In this paper, the measuring methods of solid-liquid equilibrium data of different crystallization systems were summarized; and several thermodynamic modelling cases of phase equilibrium using models such as NRTL, e-NRTL and MSE were shown; the methods of measurement and calculation of supersaturation, and metastable region and phase diagram in crystallization process optimization and selection of separation methods was introduced; in addition, the application status of process analysis technology in the field of solution crystallization was summarized,and its development tendency in crystallization field was prospected.
2023 Vol. 40 (4): 67-77 [Abstract] ( 363 ) [HTML 1KB] [ PDF 1251KB] ( 2226 )
78 Quantitative risk analysis(QRA) of liquefied petroleum gas (LPG) leakage accident
GAO Sida, HAO Lin, ZHU Zhenxing, WEI Hongyuan
In order to conduct a quantitative risk analysis (QRA) on the storage warehouse of liquefied petroleum gas (LPG), SLAB model, dynamic BLEVE fireball model and multi-energy model were employed to calculate the dispersion of LPG, the thermal effects and the overpressure. The combination of these models can predict the consequences of such accidents more comprehensively. The calculation results of these models are used to assess the degree of damage to buildings and the probability of human burns. The result shows that the fatality rate due to heat radiation reaches 80% within an area of 8 m in diameter, 50%—75% of the outer walls of the surrounding buildings will be damaged, the highest fatality rate for outdoor people due to overpressure reaches 96%, the evacuation area should be at least 20 m away from the location where the leak occurred. The method used in this research can quantify the risk of liquefied petroleum gas storage, which is helpful for the design of intrinsic safety and the formulation of quantitative specifications.
2023 Vol. 40 (4): 78-85 [Abstract] ( 387 ) [HTML 1KB] [ PDF 4090KB] ( 1343 )
86 Thermal kinetics of N-methylmorpholine-N-oxide in the decomposition process
GAO Jiancun, SHI Chenguang, WANG Wei, LIU Sisi, LI Yujing, WANG Shengnan
N-methylmorpholine-N-oxide (NMMO) is widely used in cellulose solvents. In this paper, the thermal kinetics of NMMO was studied. First, the adiabatic decomposition experiment was carried out using the accelerating rate calorimeter (ARC), and the initial decomposition temperature of NMMO under adiabatic mode was 119.87 ℃. The apparent activation energy was 219.7 kJ·mol-1 and the reaction order was 1 by kinetic calculation. Second, differential scanning calorimetry (DSC) was used to investigate the decomposition process at different heating rates, and the thermal kinetics parameters of NMMO were obtained by Friedman method, Flynn-Wall-Ozawa method and ASTM E698 method software AKTS. The initial decomposition temperature was 161.07—186.40 ℃, and the apparent activation energy of the three models were 81—134 kJ·mol-1, 75.81—100.34 kJ·mol-1 and 101.92 kJ·mol-1, respectively, which were lower than those of the ARC experimental results. Finally, the risk level of NMMO thermal decomposition was three grade by the risk matrix method. The results provide theoretical basis for reducing risk in NMMO production, storage and transportation.
2023 Vol. 40 (4): 86-93 [Abstract] ( 434 ) [HTML 1KB] [ PDF 2918KB] ( 1568 )
94 Entrainment performance of Y-type guided fixed valve tray
YUE Xirong, ZHAO Pei, LU Kuanhua, NIU Jinglong
Using the air-water system, the entrainment performance of Y-type guided fixed valve tray was studied in a plexiglass cold mold tower with diameter of 1.2 m, plate spacing of 0.45 m and four trays inside. The effects of changing three outlet weir heights, three liquid flow intensities and two opening rates on the entrainment performance of Y-type guided fixed valve tray were investigated, and the experimental results were compared with the sieve trays. The results show that the entrainment performance of Y-type guided fixed valve tray has a stable regularity with the increase of the valve hole kinetic energy factor, and it performs better under low weir height and low liquid flow intensity. Compared with the sieve tray, the structure of Y-type guided fixed valve shows obvious advantages of anti-entrainment and has a higher upper limit of gas phase load operation. The model correlation formula of entrainment rate of Y-type guided fixed valve tray with two kinds of opening rate was obtained by fitting the experimental data, which can provide reference for the design of subsequent trays and the separation of high viscosity system.
2023 Vol. 40 (4): 94-101 [Abstract] ( 343 ) [HTML 1KB] [ PDF 4576KB] ( 742 )
102 Study on oil displacement performance of a temperature-resistant and salt-resistant oil-based supramolecular system
JU Ye, QU Jin, LI Xiang, LIU Fenggang, LI Xiaowei, WANG Shuo, MA Xinru, LIU Xiaofei
Polymer microspheres have the characteristics of low injection climbing pressure, good deep migration effect, temperature resistance and salt resistance, and low cost. As a commonly used oil displacement agent, polyacrylamide microsphere emulsion cannot achieve good oil displacement under such reservoir conditions of high temperature and salinity. Therefore, it is necessary to study the new oil-based supramolecular systems of non-polyacrylamide. In this paper, 50 nm and 100 nm polyacrylamide microspheres commonly used in oilfields and oil-based supramolecular microspheres are selected for comparative research. In the analysis and observation, the particle size, viscosity, and agglomeration behavior of the polymer microspheres, the oil-water mass transfer behavior in the capillary, and the interfacial tension reduction of each sample, the effects of temperature and surfactant on the peeling of crude oil droplets of polymer microspheres were studied through microscopically visible oil droplet exfoliation experiments. By calibrating the moving speed of the outer contact line generated by different microspheres during the peeling process of crude oil droplets, the microscopic effect of different types of microspheres peeling off oil droplets was quantitatively analyzed. The results show that the polymer microspheres and the surfactant have a synergistic effect, which can greatly improve the speed of stripping oil droplets. Among these three kinds of microspheres, the oil-based supramolecular microsphere system has better temperature resistance and salt resistance, and the effect of stripping oil droplets is the best, followed by 50 nm microspheres, and 100 nm microspheres had the worst peeling effect. Therefore, the oil-based supramolecular system is a new type of oil displacement system with good development prospects.
2023 Vol. 40 (4): 102-110 [Abstract] ( 418 ) [HTML 1KB] [ PDF 5034KB] ( 1000 )
111 Separation behavior of copper and arsenic in acid leaching solution of copper smelting dust
YUAN Song, LI Minting, WEI Chang, SUN Xu, LI Xingbin, DENG Zhigan, JIANG Ziwei
In order to solve the problem of separating arsenic from valuable metals in the acid leaching solution of copper dust, this paper adopts the method of pressure synthesis of scorodite to realize the efficient separation of Cu and As, and stable solidification of arsenic in the form of scorodite. The effects of temperature, total pressure and initial pH on the separation of Cu and As, and the synthesis of scorodite were studied under pressurized system. The results show that increasing the reaction temperature is beneficial to the separation of Cu and As and the synthesis of scorodite with good crystal shape, while the formation of jarosite at lower temperature affects the synthesis of scorodite and the separation of Cu and As. The higher the initial pH value is, the more easily Fe3+ in the system hydrolysis, which is not conducive to the synthesis of scorodite, and further affects the separation efficiency of Cu and As. The increase of total pressure is conducive to the separation of Cu and As, but not conducive to the stable solidification of scorodite. If the oxygen pressure is too high, the oxidation rate is accelerated, and the hydrothermal hydrolysis reaction of Fe3+ is easy to occur. The morphology of scorodite changes from biconical to agglomerate, which reduces its stability. Under the conditions of initial molar ratio of Fe to As of 1.2, initial pH of 0.4, reaction time of 2 h, initial concentration of copper ion of 9 g·L-1, total pressure of 0.8 MPa and temperature of 160 ℃, the precipitation rates of As and Cu are 81.57% and 12.27%, respectively, and the separation coefficient of Cu and As is 76.88, which can effectively separate Cu and As. And the crystalline scorodite was obtained.
2023 Vol. 40 (4): 111-121 [Abstract] ( 291 ) [HTML 1KB] [ PDF 6512KB] ( 442 )
122 Research on polypropylene washing-deashing process
YE Xinxin, XING Zhaoliang, JIANG Tao, LI Jian
Removing the ash and improving the purity of polypropylene resin are important to extend its application in the fields of electronic and electrical membrane parts, medical and health products, food safety appliances. In this research, we designed a system of "n-hexane+isopropanol" to wash and remove the ash in the polypropylene powder to reduce the content of catalyst residual elements such as Ti, Mg, Al, etc., thereby obtaining high-purity polypropylene. The effect of process conditions such as detergent type, washing temperature, detergent ratio, washing time and detergent dosage on the ash removal effect was systematically studied, and the performance change of polypropylene resin after washing and deashing treatment was explored. The experimental results show that the total ash content is reduced to 30.81 μg·g-1, the ash removal rate reaches 79.99%, and the polypropylene purity is significantly improved by using the "n-hexane+isopropanol" composite detergent to wash the polypropylene powder. At the same time, washing and deashing treatments improve the isotacticity of polypropylene.
2023 Vol. 40 (4): 122-128 [Abstract] ( 318 ) [HTML 1KB] [ PDF 1526KB] ( 920 )
129 Optimization of heterogeneous Fenton treatment of organic complexes in electroplating wastewater based on response surface methodology
ZHAO Jin, CHENG Yu, JIANG Tianxiang, CAO Junrui
In order to improve the catalytic efficiency and optimize the operating conditions of heterogeneous Fenton process for electroplating wastewater treatment, a supported fly ash heterogeneous Fenton catalyst was prepared by using phthalic acid and hydrochloric acid as the buffer solution. And the effect of factors, such as catalyst dosage, initial pH value and H2O2 dosage on the catalytic efficiency of organic complexes in electroplating wastewater were investigated, respectively. On the basis of single factor experiments, the Box-Behnken Design response surface methodology was used to optimize the experimental design, the optimized conditions and the interaction between multiple factors were obtained by model construction and variance analysis, and then the accuracy of the model was verified. The results show that the order of influence of various factors on the removal rate of CODCr in electroplating wastewater is as follows: initial pH value>catalyst dosage>H2O2 concentration, and the significant interaction occurred between initial pH value and H2O2 concentration. Moreover, the optimal reaction conditions are as follows: catalyst dosage 16.86 g·L-1, initial pH value 3.49, H2O2 concentration 50.6 mmol·L-1. Furthermore, the average actual value of CODCr removal rate is 94.2%, which the relative error only 0.95% compared with predicted value. Therefore, it is feasible to optimize heterogeneous Fenton degradation of organic complexes in electroplating wastewater by response surface methodology.
2023 Vol. 40 (4): 129-136 [Abstract] ( 309 ) [HTML 1KB] [ PDF 3798KB] ( 607 )
137 Research on resource utilization technology of saline wastewater in antibiotic production
YANG Ting, ZHU Xingchi, GUO Xiaofu, LI Fei, LI Hong, WANG Jing, JI Zhiyong
The manufacturing process of antibiotics would inevitably generate considerable salt-containing wastewater, whose major contents are sodium chloride and potassium chloride. This wastewater, if it is discharged directly, can lead to both environmental pollution and resources wastage. In this study, a process of "mechanical vapor recompression (MVR) + cooling crystallization" was adopted to treat the wastewater and obtain valuable salt like NaCl and KCl. The separation effect and economic energy consumption at different temperatures were mainly investigated. Under preferred process operating conditions of (85.00±0.50)% water evaporation at 90 ℃ atmospheric pressure and crystallization temperature 25 ℃, the yield of NaCl could reach more than 85.00%, and the quality of NaCl and KCl met the requirement of the corresponding national standard for industrial product.
2023 Vol. 40 (4): 137-143 [Abstract] ( 303 ) [HTML 1KB] [ PDF 2508KB] ( 888 )
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