Table of Content

12 July 2023, Volume 54 Issue 7

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STUDY ON SCALE-UP OF STIRRED REACTOR FOR INDUSTRIAL PRODUCTION OF PSEUDO-BOEHMITE

2023, 54(7):  1-9. 

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The production of pseudo-boehmite by NaAlO₂-Al₂(SO₄)₃ process is a rapid neutralization reaction, the mass transfer effect of reactants directly affects the product properties, and the structure of stirred reactor influences mass transfer effect. When the production capacity of industrial production is expanded, the amplification effect of stirred reactor becomes the key to affect the product properties. The computational fluid dynamics (CFD) software fluent was used to numerically simulate three kinds of scale reactors: laboratory small reactor, industrial one-volume reactor and double-volume reactor. The effects of rheological properties of the reaction material, macro mixing time and height-diameter ratio of the reactor was investigated on the laboratory small reactor. Combined with the experimental results and the reaction mechanism analysis, it was found that in order to obtain products with larger pore volume, the flow pattern in the reactor should ensure rapid mixing and high super-saturation at the feeding site and low super-saturation at the lower part of the reactor. The simulation results showed that there was no strong mixing at the feeding site and local fast circulation at the bottom of the reactor in the industrial one-volume reactor, while there was strong mixing at the feeding site and fast circulation at the bottom of the reactor in the double-volume reactor. The results of industrial production showed that the pore volume of the product from double-volume reactor was better than that from the one-volume reactor. Therefore, when the reactor was scaled up to quadruple-volume reactor, taking the flow pattern in the quadruple-volume reactor to form the same flow pattern of the double-volume reactor as the objective, the parameters of the quadruple-volume reactor such as the height-diameter ratio, the size of the agitator, the structure of the reactor body and the installation mode of the baffle were optimized by numerical simulation method. The dimensions of the quadruple-volume reactor and its internal components were calculated, the quadruple-volume reactor was designed and manufactured, and the industrial test was carried out on the industrial plant of SINOPEC Catalyst Co. Ltd.,Changling Division. The results showed that the pore volume of the product from quadruple-volume reactor was the same as that from the double-volume reactor under the same process conditions, which successfully avoided the scale-up effect of the reactor.

STUDY ON OXIDATION OF 2-ALKYLANTHRACENE TO 2-ALKYLANTHRAQUINONE IN H₂O₂/HCl SYSTEM

2023, 54(7):  10-19. 

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In order to solve the pollution problem of the traditional production process of 2-alkylanthraquinone-phthalic anhydride method, a new technical route of 2-alkylanthraquinone production by oxidation of 2-alkylanthracene was developed. The 2-alkylanthracene could be oxidized into 2-alkylanthraquinone in a H₂O₂/HCl system. The main product was confirmed as 2-alkylanthraquinone by GC-MS and NMR, and the by-products were 1-chloroderivative and 2-chloroderivative of 2-alkylanthracene. The reaction mechanism was studied, and the oxidation active substance including HClO and ¹O₂ were confirmed. The effects of different solvents, reaction time, the molar ratio of H₂O₂ and 2-alkylanthracene, the molar ratio of HCl and 2-alkylanthracene, the mass fraction of water [w(H₂O)], the mass concentration of 2-alkylanthracene [ρ(R-AN)] were investigated. Based on the theory of Support Vector Regression (SVR), a yield prediction model was established. The prediction effect of the model was good and the relative error was mostly within 1.5%. The optimum process conditions of oxidation at atmospheric pressure and reaction temperature 70 ℃ were determined as follows: n(H₂O₂)/n(R-AN)＝5, n(HCl)/n(R-AN)＝5, w(H₂O)＝8%, ρ(R-AN)＝0.04 g/mL. When reaction time was 8 h, the yield of 2-alkylanthraquinone was more than 98%.

PREPARATION OF ALUMINA WITH HIGH SPECIFIC SURFACE AREA AND LARGE PORE VOLUME VIA ALCOHOL ADDITION

2023, 54(7):  20-25. 

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Aiming at the difficult problem of preparing high-purity alumina with large specific surface area, large pore volume and large pore size, the effects of organic fatty alcohol on the specific surface area, pore volume and the most probable pore diameter of alumina during the preparation of high-purity alumina by alkoxy aluminum hydrolysis were investigated, and the influence mechanism was explored. The results showed that the addition of fatty alcohol and emulsifier at the same time was beneficial to the dispersion of alcohol in the slurry of aluminum hydroxide precursor, and more large pores could be formed effectively by drying and calcination, so that the specific surface area, pore volume and the most probable pore diameter could increase at the same time. The higher the amount of alcohol or emulsifier, the better the effect of pore enlargement, and the higher the carbon number of fatty alcohol, the better the effect of pore enlargement. As an additive, n-hexanol was better than isopropanol, n-butanol and n-amyl alcohol in pore enlargement. The addition of fatty alcohol did not increase the residual carbon content of alumina products and had no effect on the purity of alumina. Through optimization of process conditions, high-purity alumina with high specific surface area ≥ 270 m²/g, pore volume ≥ 0.80 cm³/g and the most probable pore diameter ≥9 nm could be obtained by this method.

IMPROVED KINETIC MODELING AND ALGORITHM OF THREE-COMPONENT REACTION NETWORK

2023, 54(7):  26-33. 

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In order to solve the problem that the eigenvector method cannot deal with complex reaction networks and that the equal time method is easy to appear negative and imaginary numbers, the reaction network kinetic model was improved. Firstly, the concentration of components was linearly independent solutions of component concentration to ensure the existence of the inverse matrix. Secondly, the real concentration was appropriately transformed into a virtual concentration to simplify the expression of concentration-time equation. Finally, the model algorithm was improved by using the concept of equal time. The results showed that in the improved model, the equilibrium concentration of components was determined only by the rate coefficient, which was independent of the initial concentration. With the decrease of the distribution entropy of rate coefficient, the middle of concentration-time curve of the components moved up, but the initial and terminal values did not change, and the improved algorithm made the calculation of the rate constant go on smoothly. The calculation results could be more reasonable by adjusting the value of △t in the matrix decomposition equation. When △t = 0.5, the mean deviation between the calculated concentration and the experimental value was the smallest, which showed that the new model made up for the shortcomings of the equal time method and the improved algorithm was effective and feasible.

MEASUREMENT OF ETHANE/ETHYLENE IGNITION DELAY TIME AND KINETIC MODELING UNDER HIGH PRESSURE AND HIGH TEMPERATURE

2023, 54(7):  34-40. 

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In order to study the ignition characteristics of ethane/ethylene at high pressure and temperature, the variation of ignition delay time of ethane/ethylene-oxygen mixture under different operating conditions was investigated by experimental method and kinetic modeling tools. The experimental data showed that there was no self-ignite of ethylene/ethane at the pressure of 1.0 MPa and the temperature of 680-800 K, but the self-ignition of ethane/ ethylene occurred at the pressure of 2.0 MPa. The initial ignition temperature of ethylene was lower than that of ethane, and the higher the temperature was, the shorter the ignition delay time was. In addition, the analysis of sensitivity and reaction pathway of ethane and ethylene self-ignition process showed that the reactions that promoted the self-ignition of ethane was dehydrogenation and formation of .C₂H₅ and .OH radical, and the primary reactions that promoted the self-ignition of ethylene was oxidation or dehydrogenation to form active free radicals .HCO,.O,.OH,.C₂H₃. The inhibition of self-ignition of ethane and ethylene was the reaction of consuming .OH and .HO₂ to form stable compounds, and oxidative dehydrogenation was the initial step of ethylene and ethane chain, the reaction rate had a great influence on the ignition delay time.

COMMERCIAL APPLICATION OF ADSORBENT RAX-4000

2023, 54(7):  41-45. 

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RAX-4000 is a new generation of p-xylene adsorbent developed by SINOPEC Research Institute of Petroleum Processing Co., Ltd. Its adsorption capacity, adsorption selectivity and productivity are significantly improved compared with the previous generation of adsorbent. RAX-4000 was successfully applied in the adsorptive separation unit of aromatics complex in SINOPEC Jinling Company. The results of long-period industrial application showed that the purity of p-xylene was 99.84%, the single-pass yield was 99.0%, the desorbent-to-feed mass ratio was 1.05, and the average chamber pressure drop was 0.21 MPa. RAX-4000 has been running smoothly and its technical index was advanced in the past 3 years.

PREPARATION AND APPLICATION OF POROUS MATERIALS BY COMBINING BASE AND ACID MODIFICATION OF KAOLIN

2023, 54(7):  46-51. 

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The effect of modification of fully calcined kaolin with different alkaline concentration, different alkaline treating times, and acid treating of alkaline-leaching fully calcined kaolin was studied in details. The changes in porosity, chemical composition of modified fully calcined kaolin were characterized by XRD, N₂ adsorption-desorption and X-ray fluorescence spectrometer. The results showed that with the increase of alkaline solution concentration, the pore volume and BET surface area of the modified product increased, and the SiO₂/Al₂O₃ ratio reduced slightly, but with the increase of alkaline-treated times, the pore volume decreased and SiO₂/Al₂O₃ ratio increased. Moreover, the porous material with a pore volume of 0.81 cm³/g and a specific surface area of 408 m²/g could be obtained after alkaline-leaching fully calcined kaolin further modified by acid treating. When using the catalyst prepared from the porous material for catalytic cracking reaction,the slurry yield reduced by 3.07 percentage points, the gasoline yield increased by 2.68 percentage points, and the total liquid yield increased by 2.58 percentage points.

COMMERCIAL APPLICATION OF FCC CATALYST FOR INCREASING GASOLINE OCTANE NUMBER AND INCREASING PROPYLENE BUTENE PRODUCTION

Wang Wei

2023, 54(7):  52-56. 

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The No.2 catalytic cracking unit of SINOPEC SK(Wuhan) Petrochemical Company Limited had the characteristics of long reaction time, high reaction pressure and processing hydrogenated VGO feedstock, and the gasoline had low octane number and the yield of propylene and butene was low. In order to improve the economic benefits, the catalytic cracking catalyst HBC-3WH developed by SINOPEC Research Institute of Petroleum Processing Co., Ltd., was used to increase the octane number of gasoline and produce more propylene and butene. The commercial application results showed that the target product (LPG + gasoline) yield was increased by 1.04 percentage points, the relative yields of propylene, isobutylene and n-butene were increased by 1.0 percentage point, 0.45 percentage point and 0.91 percentage point,respectively, the coke yield was basically unchanged, the olefin volume fraction in gasoline was increased by 8.4 percentage points, and the research octane number was increased by 2.3.

STUDY ON IN-SITU CATALYTIC PYROLYSIS OF NAOMAOHU COAL WITH Ni/OLIVINE CATALYST FOR UPGRADING ITS PYROLYSIS OIL AND GAS

2023, 54(7):  57-63. 

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The Ni/olivine catalyst with olivine as a carrier was used to improve the tar quality of Hamin Naomaohu coal during catalytic pyrolysis. The effects of pyrolysis temperature and nickel loading on the yield and composition of tar were studied in a fixed-bed reactor. The tar quality was evaluated by simulated distillation, the specific composition of tar was determined by GC-MS, and the mechanism of quality improvement was analyzed. The results showed that the highest yield of tar was 16.20% at 500 ℃. After the adding Ni/olivine catalyst, when the Ni content was 5%, the tar yield decreased significantly and reached the lowest 14.36%, the mass fraction of heavy tar component decreased from 35% to 30%, and the light tar yield increased by 15.59%. The gas yield decreased significantly, but the H₂ content increased significantly. The relative content of short-chain aliphatic hydrocarbons, benzenes, phenols and naphthalenes in the tar components increased, which showed that Ni/olivine catalyst could improved the quality of tar by catalytic cracking of long-chain alkanes and polycyclic compounds in tar, and the best quality improvement effect was achieved when the Ni mass fraction was 5%.

PREPARATION OF COCONUT SHELL CARBON SUPPORTED RUTHENIUM AS A CATALYST FOR THE HYDROLYTIC DEHYDROGENATION OF AMMONIA BORANE

2023, 54(7):  64-70. 

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Ru/CSC catalysts were prepared by impregnation-reduction method using the coconut shell carbon (CSC) as support and Ru as active component, and the microstructure and morphology of the catalyst were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, TEM and N2 adsorption-desorption. The effects of light, metal loading, reactant concentration, catalyst dosage, and reaction temperature on the reaction rate of hydrogen production from ammonia borane hydrolysis were investigated. The results showed that there was a metal-support interaction between Ru and CSC, and the catalytic performance of 1.0% Ru/CSC catalyst for the hydrolysis of ammonia borane to hydrogen production under the condition of visible light irradiation was significantly better than that under the condition of no light irradiation. There was a positive correlation between the hydrogen production rate and Ru/CSC concentration. The interfacial reaction of catalyst was the rate-controlling step of hydrogen production from the hydrolysis of ammonia borane, which was independent of the concentration of ammonia borane. The conversion frequency (TOF) and apparent activation energy (Ea) were 334.8min^-1 and 59.9 kJ/mol, respectively, for the photocatalytic hydrolysis of ammonia borane to hydrogen at 1.0% Ru/CSC at 298 K.

PREPARATION AND APPLICATION OF HIGH DENSITY CAGE HYDROCARBON COMPOUND PENTACYCLO[5.3.0.0^2,5.0^3,9.0^4,8]DECANE

2023, 54(7):  71-75. 

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Using heterogeneous photocatalysts and photosensitizers to catalyze dicyclopentadiene intramolecular [2+2] cycloaddition reactions，it was found that the photocatalytic efficiency could be greatly improved. In particular, the composite M_xO_y-TiO₂ photocatalyst doped with other metals could catalyze the conversion of materials in a relatively short time and obtain pentacyclo [5.3.0.0^2,5.0^3,9.0^4,8] decane (BCU) with a higher yield. The density and volumetric calorific value of BCU caged hydrocarbon compound were higher than that of JP-10 liquid fuel. After the mixture with JP-10 liquid fuel, the density and volumetric calorific value of the complex fuel increased with the increase of BCU mixing ratio, at the same time had good low-temperature performance and low-temperature viscosity. When the mass fraction of BCU was 50%, the fuel density（20 ℃）was 0.995 g/cm³, the volumetric calorific value was 41.2 MJ/L, the freezing point was -43.8 ℃, and the dynamic viscosity（-20 ℃） was 19.3 mm²/s. Compared with JP-10, the compound fuel had a great increase in the density and volumetric calorific value, while maintaining good low temperature performance. The results showed that BCU could be used as a high performance fuel component and had a good application prospect.

THE SYNTHESIS AND RELATIONSHIP BETWEEN STRUCTURE AND PERFOMANCE OF POLYETHER AMINE FUEL DETERGENT

2023, 54(7):  76-83. 

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A series of polyether amine(PEA) detergents with different polymerization monomers, different degrees of polymerization and different amino-terminated structures were synthesized by the method of amine protection, the structures of polyether amines were characterized by HRMS, NMR and IR, and their detergency were compared, furthermore, the structure-activity relationship of PEAs was studied by establishing detergent model, gasoline model and coke model with Material Studio software. The results showed that the detergency of polyetheramine was closely related to the structure of polar group in its head and the structure of polymerization unit. When the molecular structure was the same, polyether amine with average number molecular weight about 1 000 had the best detergency; when polar groups were the same, the PEAs with higher proportion of epoxy butane had better detergency, and PEAs with pure epoxy butane chain had the best detergency; when the polymerization unit structures were the same, the order of detergency of the different amino-terminated detergents from high to low was mono-primary amine polyether amine > di-primary amine polyether amine ≈ N,N-dimethyl-1,3-propanediamine-terminated polyether amine. The results of molecular simulation showed that the adsorption energy between the head polar group and the carbon deposit, the interaction energy between the polyepoxide alkane chain and the fuel oil determined the detergency of polyether amine.

CORROSION AND TRIBOLOGICAL PROPERTIES OF A NOVEL IONIC LIQUID BASED HIPPURATE

2023, 54(7):  84-90. 

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Three ionic liquids based hippurate were synthesized: 1-butyl-3-methylimidazolium hippurate ([BMIM][Hip]), choline hippurate ([CHO][Hip])and tributyltetradecylphosphonium hippurate ([P₄₄₄₁₄][Hip]). The corrosion of the three ionic liquids to mild steel and the tribological performances of the three ionic liquids as lubricants the steel/steel friction pairs were investigated by electrochemical measurements and frictional tests, respectively. The traditional ionic liquids [BMIM][BF₄] was selected as a comparison. The results showed that traditional ionic liquids [BMIM][BF₄] had strong corrosion to mild steel. The three synthesized ionic liquids had very low corrosion to mild steel, and [CHO][Hip] had the least corrosion. The three synthesized ionic liquids showed excellent tribological performances the steel/steel friction pairs, [BMIM][Hip], [CHO][Hip] and [P₄₄₄₁₄][Hip] were 9.3%, 5.3% and 18.1% of the friction pairs worn by [ BMIM ][ BF₄], respectively.

APPLICATION OF FD2G TECHNOLOGY MODIFICATION TO FDHC TECHNOLOGY IN DIESEL HYDRO-UPGRADING UNIT

2023, 54(7):  91-97. 

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The original design of 0.9 Mt/a diesel hydro-upgrading unit in a refinery adopted the FCC diesel hydro-conversion technology (FD2G) developed by SINOPEC (Dalian) Research Instituteof Petroleum and Petrochemicals Co.,Ltd.(FRIPP). In order to cope with changes in the oil product market, the company decided to adopt diesel hydrocracking technology (FDHC）developed by FRIPP after the completion of the unit.By changing the feedstocks, changing the catalyst system and revamping the local process, the production scheme was adjusted from gasoline scheme to jet fuel scheme. The results of calibration showed that the yield of heavy naphtha was 21.90%, the potential content of aromatics was 48.5%, the yield of jet fuel was 33.33 %, the yield of refined diesel was 31.93 %, and content of sulfur and nitrogen was lower than that of raw diesel, which could be used as the blending component of diesel meeting the standard of China Ⅵ. As the first time that the diesel hydro-upgrading unit was successfully revamped from FD2G technology into FDHC technology in China, this industrial application can provide reference for same type units.

STUDY ON STYRENE TAR REPROCESSING IN DELAYED COKING UNIT

2023, 54(7):  98-104. 

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In order to solve the problem of large environmental protection pressure in the process of styrene tar treatment, the styrene tar was sent to a delayed coking unit for recycling. The results showed that the styrene tar was not suitable to be reprocessed during the cooling coke period due to discoloration of the cold-cut coke water and odor during coke removal. The method of recovering styrene tar during the production of the coke drum was feasible, but the recovering styrene tar would affect the side line of the fractionation column in coking unit, so it was necessary to control the amount and time of recovering styrene tar, optimize the process operation, maintain the equipment regularly, and analyze the content of styrene tar in various products of the delayed coking unit, cold-cut coke water, and sulfur-containing wastewater periodically. The problem of equipment and pipeline blockage during the recycling process has been solved through continuous optimization of process and equipment conditions. Furthermore, the unit operated smoothly after the recycling process. The styrene tar was successfully decomposed into the products of the delayed coking unit by reprocessing.

ENERGY CONSUMPTION AND COST ANALYSIS OF HYDROGEN PRODUCTION BY STEAM REFORMING OF NATURAL GAS

2023, 54(7):  105-112. 

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Based on the process parameters of the industrial natural gas hydrogen plant, a process model of natural gas hydrogen production was established by using Aspen Plus process simulation software. The energy consumption, material consumption, H₂ cost and carbon emission intensity of hydrogen production process under different process parameters were investigated. The results showed that the cracking reaction of methane was the main cause of carbon deposition in the conversion unit, and high water/carbon (H₂O/C) mole ratio was beneficial to inhibit thermodynamic carbon deposition. Besides, low H₂O/C mole ratio, low CH₄ content in dry gas of conversion unit and high H₂ yield of pressure swing adsorption (PSA) unit were beneficial to energy saving and material consumption reduction of H₂ production, and to reduction of carbon emission, the order of their influence on hydrogen production unit from high to low was H₂O/C mole ratio > H₂ yield of PSA unit > CH₄ content in dry gas of conversion unit. The change of CO content in dry gas of medium-temperature WGS had no obvious influence on the energy consumption, material consumption, H₂ cost, and CO₂ emissions intensity of the hydrogen plant.

EFFECT OF BIOCARRIERS ON N₂O EMISSION REDUCTION IN IFAS PROCESS FOR WASTEWATER TREATMENT

2023, 54(7):  113-122. 

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In order to meet the current demand for upgrading traditional processes in municipal wastewater treatment plants, the integrated fixed-film activated sludge (IFAS) process with bio-carriers is an efficient treatment method to strengthen the pollutant removal effect and improve microbial diversity and system stability. In addition, the IFAS process has the potential to reduce N₂O emissions compared to a single process, since it promoted simultaneous nitrification and denitrification and was beneficial to the growth and reproduction of specific ammonia-oxidizing microorganisms with low N₂O emissions. This article summarized important discussions of IFAS process in the field of improving quality and efficiency of wastewater treatment processes and N₂O emission reduction etc.. Then, the mechanism of N₂O production in IFAS process and the mitigation mechanism of N₂O emission by bio-carriers were analyzed. Finally, the future research direction of IFAS process in synergistic carbon reduction and pollution reduction was prospected.

STUDY ON DEGRADATION OF PHENANTHRENE BY SODIUM PERSULFATE ACTIVATED BY SULFUR MODIFIED NANO ZERO-VALENT IRON

2023, 54(7):  123-129. 

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The remediation of polycyclic aromatic hydrocarbons (PAHs) in soil and groundwater environment has become an important environmental problem in the world. In order to solve the problem of low degradation efficiency of Fe-based activated materials during chemical degradation, nano-zero-valent iron (nZVI) and sulphur-modified nano-zero-valent iron (S-nZVI) were prepared by liquid-phase reduction method, and the phenanthrene degradation process was optimized by degradation kinetics, activation material characterization and oxidant ratio test. The results showed that S-nZVI had the highest activity when the molar ratio of S/Fe was 0.28, and the degradation rate of phenanthrene was 88.44% at 90 min. The order of activation effect from high to low was S-nZVI > nZVI > Fe²⁺> no activator. The results of energy spectrum analysis showed that the reference S/Fe molar ratio of S-nZVI nano-activated material was 0.08. When the molar ratio of persulfate/S-nZVI was 200, the activated degradation efficiency was still high.

SIMULTANEOUS DETERMINATION OF HYDROCARBON TYPES OF LCO BY AUTOMATIC SOLID-PHASE EXTRACTION AND GAS CHROMATOGRAPHY-MASS SPECTROMETRY

2023, 54(7):  130-136. 

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A method for the determination of hydrocarbon types in light cycle oil (LCO) by automated solid-phase extraction (SPE) coupled with gas chromatography-mass spectrometry was developed. Samples were extracted and pretreated by automatic solid-phase extraction. The extraction conditions, such as the kind of the type of extraction solution, the ratio of sample treatment amount and fixed phase addition amount, the flow rate of elution extraction solution and the volume of air, were optimized. The results showed that when the sample treatment amount was 0.1 mL, the extraction solution of saturated hydrocarbon component was 1.8 mL n-hexane, the extraction solution of aromatic component was 2 mL mixed solution with the volume ratio of dichloromethane to ethanol of 5.0/1.5, the fixed-phase packing in the SPE column was 1.65 g, the flow rate of extraction solution was 1.5 mL/min, the volume of the air eluted by the saturated hydrocarbon component was 0.6 mL, and the volume of the air eluted by the aromatic hydrocarbon component was 18 mL, the recoveries ranged from 98.5% to 100.5% with RSD (n=6)≤7%. The method was suitable for the composition analysis of LCO. The automatic solid-phase extractor was highly automatic, and the analysis efficiency was improved. Under optimized conditions, the analysis results were accurate and repeatable.

PROGRESS IN THE HETEROGENEOUS CATALYSTS FOR AMINATION OF FATTY ALCOHOL

2023, 54(7):  137-144. 

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As an important fine chemical intermediate, aliphatic amines are widely used in dyes, pesticides and other fields. The reductive amination of alcohol is one of the most promising methods with wide source of raw materials, simple process and green economy. The development of catalyst is the key and difficult point of the reaction. The research progress in heterogeneous catalysts for amination of fatty alcohol was reviewed, and the catalytic performance and reaction regularity of Ni, Co, Pd and Ru catalysts for different substrates were introduced. The modification of metal (such as its geometric structure, its electronic structure) and support (acid-base, metal-support interaction) sites were described as the main means to improve the performance of catalysts. The frontiers of the topic, including the preparation of high performance catalysts, the study of reaction mechanism and structure-activity relationship, and the development of mild reaction and polyols systems, were put forward.