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期刊基本信息
主办单位：中国石油化工股份有限公司
　　　　　石油化工科学研究院
编辑出版：石油炼制与化工编辑部
主　　编：汪燮卿院士
执行主编：李才英教授
副 主 编：刘鸿洲 刘迎春
国际标准刊号：ISSN 1005-2399
国内统一刊号：CN 11-3399/TQ
邮发代号：2-332

Table of Content

    12 November 2023, Volume 54 Issue 11
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    DEVELOPMENT OF A MODULAR DISTRIBUTED SYSTEM FOR HYDROGEN PRODUCTION FROM METHANOL AND APPLICATION IN THE HYDROGEN REFUELING STATION
    2023, 54(11):  1-7. 
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    To satisfy the hydrogen demand for hydrogen refueling stations, based on the analysis of the advantages and disadvantages of the existing hydrogen supply system, the catalytic process and chemical process of the distributed hydrogen production system were "re-engineered" to form a new distributed hydrogen production system. The development of a new type of catalyst for hydrogen production from methanol improved the reaction efficiency and reduced the reactor volume. The new catalytic oxidation catalyst has the advantages of high activity at low temperatures and good stability at high temperatures. The micro-channel technology was used to strengthen the heat transfer process in the distributed hydrogen production system, and the miniaturization of the device was realized. The coupling system of methanol reforming and catalytic oxidation made full use of the characteristics of endothermic-exothermic reaction and realized the closed-loop utilization of system energy. The distributed hydrogen production system developed in this paper was first developed in China, and the integrated hydrogen refueling station with the production of hydrogenation was demonstrated. The covered area of the distributed methanol hydrogen production demonstration unit was only 64 m2, and the methanol consumption of 1 kg fuel cell grade hydrogen was 7.37 kg. It provides a replicable and extensible experience for China to construct a safe, stable, and efficient hydrogen supply network, and has a positive significance for reducing the cost of hydrogen and promoting its application on a large scale.
    REVIEW ON CATALYTIC CRACKING TECHNOLOGY WITH DIVERSIFIED PRODUCT STRUCTURE
    2023, 54(11):  8-15. 
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    Catalytic cracking technology has become one of the core technologies in the transformation and development of refineries as the fuel-based refineries accelerate the transformation to integration of refining and chemical. A series of catalytic cracking technologies with product structure diversity developed by SINOPEC Research Institute of Petroleum Processing Co.,Ltd. were introduced, and the technological innovation, technological characteristics, application scenarios and industrial practice results were emphatically analyzed. Catalytic cracking technology realized the innovation chain from applied basic research to reactor technology development and then to transformation of production. A series of catalytic cracking technologies for enhancing petrochemicals production have become one of the most important technical support and solutions for refining enterprises to achieve the goal of “oil to chemicals”, which can realize the efficient utilization of refinery light distillate oil, heavy distillate oil and even crude oil.
    EFFECT OF POST-REFINING REACTION TEMPERATURE ON DISTRIBUTION AND PROPERTIES OF HYDROCRACKING PRODUCTS
    2023, 54(11):  16-21. 
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    The effect of post-refining reaction temperature on the distribution and properties of hydrocracking products was investigated by using the intermediate base VGO in single stage once-through hydrocracking process, and the reaction thermodynamic data was calculated. The results showed that inthe range of 320-380℃,the post-refining reaction temperature had little effect on product distribution, and the increase of post-refining reaction temperature was beneficial to the improvement of smoke point of jet fuel, cetane index of diesel and BMCI of tail oil, however, the bromine index and sulfur content of the product increased correspondingly. Thermodynamic data of reaction showed that high temperature was unfavorable to the reaction of olefin hydrogenation saturation and mercaptan formation, therefore it was inferred that the formation of mercaptan from olefin and hydrogen sulfide in the low temperature system of the test facility was the main reason for the increase of sulfur content in the product.
    PREPARATION OF MESOPHASE PITCH BY THERMAL CONVERSION OF AROMATICS-RICH COMPONENTS IN FCC SLURRY
    2023, 54(11):  22-28. 
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    The effects of reaction temperature, reaction time and reaction pressure on the thermal conversion behavior of FCC-KQ aromatics-rich components of FCC slurry were investigated by means of optical microscopy, softening point, yield and thermogravimetric analysis, and the formation mechanism of mesophase pitch was proposed. The results indicated that the softening point increased slowly and the yield decreased rapidly at low temperatures or a short reaction time, while the softening point increased rapidly and the yield decreased slowly at high temperatures or a long reaction time. The growth and melting of mesophase spheres was a rapid process, in which the softening point of thermal polycondensation residues increased rapidly. The anisotropic mesophase pitch C120 with a softening point of 121 ℃ was produced from FCC-KQ at 390 ℃ and 2 MPa for 8 h. The properties of C120 pitch were similar to those of A240 pitch, with higher carbon residues and lower heteroatom content.
    TRANSFORMATION STRATEGIES FOR MAXIMIZING THE UTILIZATION OF AROMATIC HYDROCARBON RESOURCES IN PARAXYLENE PLANT
    2023, 54(11):  29-33. 
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    In order to optimize the product structure of a refinery, the xylene unit was modified with the adaptability of changing catalyst, and the isomerization route was changed from ethylbenzene conversion type to de-ethylation type. While reducing the loss of aromatics, the source of aromatics could be maximized by converting them into p-xylene and benzene, thus increasing the utilization ratio of aromatics. At the same time, ethane-rich by-product gas was recovered as high value-added ethylene feedstock to achieve maximum benefits. The transformation strategy included the optimization of catalyst function, process flow adjustment and thermal integration，which could provide some reference for the transformation of similar units.
    EFFECT OF OLEFINS ON ADSORPTION AND SEPARATION PERFORMANCE OF 5A ZEOLITE ADSORBENT
    2023, 54(11):  34-40. 
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    The separation performance of 5A zeolite adsorbent for normal and isomeric alkanes was evaluated by dynamic pulse experiment and simulated moving bed experiment. The 5A zeolite adsorbent samples were characterized by XRD, SEM, N2 physical adsorption, and the effects of the type and the content of olefin on the separation performance of 5A zeolite adsorbent were investigated. The results of dynamic pulse experiment showed that the olefins with different structures in the adsorbent had different effects on the separation performance of 5A zeolite adsorbent, and isomeric olefins or cyclic olefins had a greater impact on the separation performance of 5A zeolite adsorbent than that of normal olefins. The results of simulated moving bed experiment showed that the yield of n-alkanes was decreased by about 5.6 percentage points when the mass fraction of cyclohexenes was 2%. Due to the reaction of isomeric olefins or cyclic olefins on the surface of molecular sieve, some mesoporous pores were blocked, which resulted in the decrease of the adsorption rate of 5A zeolite adsorbent for n-alkanes and the deterioration of separation performance.
    EFFECT OF ALKYL STRUCTURE IN SOLVENT MOLECULES ON CATALYTIC OXIDATION OF THIOPHENE
    2023, 54(11):  41-46. 
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    The difficulty of catalytic oxidative desulfurization in petroleum products is the removal of thiophene sulfur, but there are few studies on the effect of the composition of petroleum hydrocarbons on the oxidation reaction depth of thiophene. Using different hydrocarbons and alcohols as solvent, H2O2 as oxidant, and titanium-silicon molecular sieve (TS-1, TS-1-D) as catalyst, the oxidation of thiophene in solvent molecules with different alkyl groups was studied. The results showed that the structure of alkyl group in the solvent was an important factor affecting the oxidation degree of thiophene under the same reaction conditions. The higher the isomerization degree of alkyl group in the solvent, the greater the oxidation degree of thiophene.
    XYLENE ISOMERIZATION OVER ZEOLITE MCM-22
    2023, 54(11):  47-52. 
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    MCM-22 molecular sieve with different Si/Al ratios was synthesized by dynamic hydrothermal synthesis method using hexamethyleneimine (HMI) as template, and MCM-22 molecular sieve as acidic component, a bifunctional transformation type catalyst (Pt/MCM -22) for the isomerization of xylenewas prepared by supported platinum. The morphologies and properties of the molecular sieve samples were characterized by X-ray diffraction (XRD), specific surface area testing (BET), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and other methods. The performance of the catalyst was evaluated by using a micro-piston flow reactor and compared with that ofthe catalyst prepared with MORzeolite. The mechanism of the catalytic isomerization of xylene was further studied, and the evaluation results were explained. The results showed that MCM-22 molecular sieve had excellent isomerization activity and selectivity for xylene isomerization, and the acidity of the molecular sieve would affect its reaction performance.
    EFFECT OF SUPPORT MODIFICATION ON METAL DISTRIBUTION AND STATE OF Ru/MCM-49 CATALYST
    2023, 54(11):  53-59. 
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    Ru-Ca/H-MCM-49 catalyst and Ru-Mg/H-MCM-49 catalyst were prepared from MCM-49 zeolite modified by Ca and Mg and impregnated with Ru, and the effect of alkali metal modification on Ru particle size of Ru/H-MCM-49 zeolite catalyst was investigated. The catalysts were characterized by XRD, FT-IR, SEM, XPS, CO pulse adsorption, probe molecular reaction, and in situ CO-DRIFTS analysis. The results showed that the two modified metals had little effect on the distribution of Ru in the zeolite, and the Ru of both catalysts was distributed inside the zeolite, but the Ca modified Ru catalyst had the phenomenon of micro-porous blockage. The impregnated alkali metal species could significantly affect the size of Ru in the catalyst, and the support impregnated with Mg could better disperse Ru to form Ru nano-particles of about 2.7 nm, which showed higher probe molecular reaction performance. Catalyst Ru-Mg/H-MCM-49 adsorbed CO by linear multi-molecular adsorption, which had strong adsorption and activation effect on reactant molecules, and was beneficial to the hydrogenation activity of the catalyst.
    SYNTHESIS OF HIGH SILICA MCM-22 ZEOLITE WITH DUAL ORGANIC STRUCTURE-DIRECTING AGENTS AND ITS CATALYTIC PERFORMANCE
    2023, 54(11):  60-66. 
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    MCM-22 zeolite with high crystallinities was synthesized under optimized the crystallization time, amount of TMAdaOH and SiO2/Al2O3 molar ratio conditions by using hexamethyleneimine (HMI) and N,N,N-trimethyl-1-ammonium adamantine (TMAdaOH) as dual organic structure-directing agents. The zeolite was characterized by X-ray diffraction, scanning electron microscopy, N2 adsorption-desorption, NH3-TPD and TG analysis. The catalytic performance of H-type MCM-22 zeolite for the pyrolysis of triisopropylbenzene (TiPB) was investigated. The results showed that with the addition of a small amount of TMAdaOH, MCM-22 zeolite could be synthesized under a wide range of n(SiO2)/n(Al2O3), and MCM-22 zeolite had the advantages of crystal purity, high solid yield and adjustable acidity. The high silica MCM-22 with n(SiO2)/n(Al2O3) of 60-100 displayed better cracking performance for TiPB than that of conventional MCM-22 with n(SiO2)/n(Al2O3) of 30.
    CO2 CYCLOADDITION REACTION CATALYZED BY COMPOSITE CATALYSTS MIL-101@PIL
    2023, 54(11):  67-75. 
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    The reaction of CO2 with epoxides to form cyclic carbonates requires a catalyst with high-performance, low-cost and easy recovery. A metal-organic frameworks (MOFs)-based heterogeneous catalyst (MIL-101@PIL) was prepared for catalytic conversion of CO2 to cyclic carbonates. Firstly, the MOF precursor MIL-101-Cr was prepared by hydrothermal synthesis, and then biquaternary phosphonium ionic liquid (1,4-bis-triphenylphosphonium butane bromide) with large molecular volume was loaded into its pore channel to form the catalyst MIL-101@PIL. A series of comparative experiments showed that the catalyst MIL-101@PIL had high activity in the synthesis of cyclocarbonate by cycloaddition reaction without solvent and co-catalyst. Under the optimum conditions (MIL-101@PIL mass of80 mg, CO2 pressure of 1.4 MPa,propylene oxide amount of 17 mmol, reaction temperature of 90 ℃, reaction time of 3 h), higher yield (95%) and selectivity (99%) were obtained. The results showed that the catalyst (MIL-101@PIL) had high catalytic activity, which was mainly due to the synergistic catalysis between the coordination unsaturated Cr sites and the Br anions. Based on this, a possible mechanism of cycloaddition reaction catalyzed by catalyst MIL-101@PIL was proposed.
    SPONTANEOUS IGNATION CHARACTERISTICS AND FLAME PROPAGATION SPEED OF ESSENTIAL COMPONENTS IN GASOLINE
    2023, 54(11):  76-85. 
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    The spontaneous ignition characteristic and flame propagation velocity of several kinds of gasoline were compared by using constant volume combustion bombs, which provided a theoretical basis for gasoline blending and alternative fuel selection from the view of combustion science. It was concluded that furan-based fuels could maintain high flame propagation speed, had a wide dilution boundary at low equivalence ratios, and were potential lean-burn components.
    PREDICTION MODEL OF RESIDUE HYDROCRACKING PRODUCT DISTRIBUTION IN SLURRY BED BASED ON NEURAL NETWORK
    2023, 54(11):  86-95. 
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    Pearson correlation coefficient method was used to select the variables in the residue slurry bed hydrogenation test data sample, 17 intput variables with low correlation were obtained by optimization, and a BP neural network model with the structure of 17-14-7 was established to simulate the distribution of hydrogenation products (cracking gas, gasoline, diesel, vacuum gasoline, residue, insoluble matter) and hydrogen consumption. Aiming at the problem of data imbalance and small amount of data in the original data, data expansion was relational model. The results showed that the improved BP neural network model had a structure of 17-15-7 after data expansion, and its prediction accuracy was greatly improved, with the maximum relative error reduced from 66% to 6.57%. In order to further improve the prediction accuracy and calculation efficiency of the model, the convolutional neural network model was introduced, and the maximum relative error of the model was reduced to 5.38%. Combining genetic algorithm with neural network model to optimize the model, the accuracy of model prediction of reaction product distribution could be further improved, and the maximum relative error of Convolutional neural network optimized by genetic algorithm was less than 2%.
    NINE-LUMPING KINETIC MODEL FOR n-BUTANE AROMATIZATION REACTION SIMULATION
    2023, 54(11):  96-100. 
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    n-Butane was used as the model compound for aromatization, and the distribution of products was investigated under different conditions. According to the aromatization reaction mechanism and product distribution characteristics, the kinetic parameters of n-butane aromatization were obtained by solving a set of nine-episode chemical kinetic model equation with eight virtual reaction paths, and the prediction results of the nine-lumped kinetic model were verified by the experimental data. The results showed that the maximum absolute error between the predicted value of the product distribution model and the measured value of the test was less than 5.0%, which indicated that the model was accurate and reliable, and could reflect the reaction law of aromatization of light hydrocarbons, it could be used to simulate and optimize the actual production process.
    PREPARATION OF CHITOSAN-BENTONITE ADSORBENT AND ITS REGENERATION PERFORMANCE FOR TRANSFORMER WASTE OIL
    2023, 54(11):  101-108. 
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    In order to solve the problem of regeneration of transformer waste oil, a composite adsorbent was prepared from chitosan (CS) and bentonite (BT) as raw materials. The results showed that when the mass ratio of CS to BT was 5% and the calcination temperature was 300 ℃, the decolorization and impurity removal performance of C5/BT-300 composite adsorbent was the best. The optimum process conditions for the treatment of transformer waste oil by using the composite adsorbent C5/BT-300 were as follows: the mass fraction of the adsorbent was 4%, the adsorption temperature was 50 ℃, and the adsorption time was 90 min. After the treatment of C5/BT-300 composite, the light transmittance of transformer waste oil increased to 99.5%, the color number decreased to No. 1, and the breakdown voltage increased by 60.2%; the dielectric loss factor, water concentration and acid value were reduced by 80.7%, 68.7% and 74.1%，respectively. Compared with common adsorbents such as bentonite and activated carbon, C5/BT-300 composite showed better adsorption and regeneration performance. In addition, a convenient, efficient, intelligent and green regeneration device for transformer waste oil was developed, and the regeneration process of transformer waste oil and the regeneration process of adsorbent after treatment were optimized.
    DETERMINATION OF TRACE ELEMENTS IN PETROLEUM COKE
    2023, 54(11):  109-116. 
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    A rapid method for the determination of trace elements in petroleum coke was established by energy dispersive X-ray fluorescence spectrometer (ED-XRF). The influence of sample preparation method, powder and pressed powder, matrix and quantitative curve fitting on the test results was investigated. The high content of sulfur in petroleum coke was the greatest factor in matrix interference. Both the basic parameter method and the α-empirical coefficient method could be used to correct matrix, so that the content of S, Fe, Ni, V, Ca in petroleum coke could be determined accurately within 10 minutes. This method had good linear independence for the quantitative curves of each element in the corresponding test range, and the determination coefficient R2 was greater than 0.99. The quantification limit of S was 0.040%，and the quantification limits of Fe, Ni, V, Ca were 5.4, 1.4, 2.1, 2.8 μg/g, respectively.
    INFLUENCE OF LEAKAGE PROCESS MATERIALS ON CIRCULATING COOLING WATER SYSTEM OPERATION AND ITS SOLUTION
    2023, 54(11):  117-121. 
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    The leaking process materials do great harm to the operation of circulating cooling water. The influence of leakage materials on the quality of the circulating cooling water and the reproduction of microorganisms was studied by simulating the condition of leakage material in the laboratory. The scheme of circulating cooling water treatment including leakage material detection, corrosion, scaling and microbial control was established. The results of continuous operation in a refinery for 30 months showed that the average corrosion rate for carbon steel test tube was 0.0186 mm/a, the average adhesion rate was 7.85 mg/(cm2/month), the average total number of heterotrophic bacteria was 4.85×104mL-1, and the average quantity of the slime was 1.01 mL/m3. The effect of circulating water treatment meets the requirements of safe and stable operation of the production plant.
    RESEARCH PROGRESS IN CATALYSTS FOR OXIDATION OF C4 HYDROCARBON TO METHACROLEIN
    2023, 54(11):  122-130. 
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    Methyl methacrylate (MMA) is an important organic chemical raw material, which is widely used in the preparation of surface coatings, synthetic resins, paint coatings, and polymer materials. With the continuous development of China's petrochemical industry, especially the construction of large-scale ethylene plants, C4 resources (isobutane and isobutylene, etc) are becoming increasingly abundant, therefore, the clean process of producing MMA via C4 hydrocarbon oxidation shows significant economic and technological advantages. The oxidation of C4 hydrocarbons to methacrolein (MAL) is the key step of C4 hydrocarbon oxidation to produce MMA. The research status of catalysts (including Mo-Bi, Mo-Sb, Mo-V-Te, heteropoly acid and V-based catalysts) for the oxidation of C4 hydrocarbons to methacrolein was mainly reviewed, and the key research directions of catalysts in the future were further explored.
    RECENT ADVANCES IN CATALYTIC SYNTHESIS OF BIOMASS-DERIVED GLYCOLIC ACID
    2023, 54(11):  131-137. 
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    Glycolic acid is a kind of α-hydroxy-carboxylic acid with the simplest structure, which is widely used in materials, medical treatment and environmental protection and so on. However, the current glycolic acid synthesis technology has some problems, such as complex process and high cost of impurity removal. Under the background of ‘double carbon’, it is of great significance to develop a new synthesis technology of bio-based glycolic acid. The research of biomass-derived glycolic acid synthesis began to rise 30 years ago, and became a research hotspot in the past 5 years. The characteristics of different synthesis methods, such as cellulose conversion method and saccharide liquid phase oxidation method, were compared in detail from two aspects of synthetic methods and technical routes. It is pointed out that emphasis in the future lies in the active to exploration of new catalyst design method and new process for synthesis of bio-based glycolic acid.
    REVIEW OF INFLUENCING FACTORS OF DILUTION-INDUCED ASPHALTENE PRECIPITATION
    2023, 54(11):  138-142. 
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    Dilution-induced asphaltene precipitation can significantly reduce the viscosity of crude oil and improve the liquidity. This article reviewed the current research status of asphaltene and explained the influencing factors of asphaltene precipitation theoretically by Smoluchowski’s aggregation model. The results showed that asphaltene precipitation was affected by both thermodynamics and hydrodynamics factors. In addition, the new microfluidic technology was introduced, and on this basis, further research on the kinetics of dilution-induced asphaltene precipitation was prospected.