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Current Issue
12 June 2023 Volume 54 Issue 6
IN-SITU HYDROGENATION OF DICYCLOPENTADIENE OVER Pd/Al2O3 CATALYST
2023, 54(6):  1-6. 
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Two-step hydrogenation of dicyclopentadiene(DCPD) was carried out over Pd/Al2O3 as catalyst and formic acid as hydrogen donor instead of H2. The hydrogenation products could be further used to prepare high density jet fuel and fine chemicals. This process avoids the high pressure, flammable and explosive risk and the high requirements for the equipment when using H2 as the hydrogen source, and can be completed in an ordinary container. The effects of formic acid adding mode, reaction time, reaction temperature, reaction solvent and substrate concentration were investigated. The results showed that adding formic acid by interval with average weight was beneficial for the formation of endo-tetrahydrodicyclopentadiene, the yield of which could be up to 99% after reaction 10 h at 160 ℃. In isopropanol, ethanol or tetrahydrofuran solvent, DCPD concentration of 40%-60% could effectively promote the formation of endo-tetrahydrodicyclopentadiene. At the same time, the stability of the catalyst was investigated, and it was found that the catalyst could still maintain high catalytic activity after five cycles, which meant good potential for industrialization.
COMMERCIAL APPLICATION OF ALKALI CATALYTIC TECHNOLOGY FOR DIRECT PETROLEUM CUT TO CHEMICALS & MATERIALS
2023, 54(6):  7-11. 
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The commercial application of the new DPC alkali catalytic technology developed by China National Offshore Oil Corporation (CNOOC) in CNOOC Zhongjie Petrochemical Co., Ltd. was introduced. The DPC reacting process has the characteristics of weak hydrogen transfer, weak aromatics condensation and "cutting and cracking" of macromolecular aromatics with alkyl side chain. It has strong adaptability to crude oil, and is suitable for processing meta-cycloalkyl crude oil and inferior heavy oil. At the stage of industrial application, the blending amount of atmospheric residue in feed was gradually increased without significant adjustment of feed volume, reaction temperature, catalyst activity and catalyst/oil ratio. The calibration results showed that the mass yield of liquefied petroleum gas increased by 4.93 percentage points, the coke yield decreased by 0.95 percentage point, the volume fraction of propylene increased by 13.77 percentage points, and the volume fraction of(C3+C4olefins increased by 5.29 percentage points when the slag content was 70.5% and the storage of DPC catalyst was 70%; the mass yield of liquefied petroleum gas increased by 3.66 percentage points, the coke yield increased by 0.30 percentage point, the volume fraction of propylene in liquefied gas increased by 11.33 percentage points, and the volume fraction of (C3+C4olefins increased by 8.44 percentage points when the slag content was 91% and the storage of DPC catalyst was 91%. The unit has been running smoothly for 6 months after calibration, and the successful application of this technology provided a technical guarantee for the crude oil to chemicals technology with independent intellectual property rights of CNOOC.
OPTIMAL MEASURES FOR LONG-TERM SMOOTH OPERATION OF S Zorb UNIT
2023, 54(6):  12-17. 
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S Zorb technology is an important technology for SINOPEC to cope with the upgrading of gasoline quality. The long-term smooth operation is very important for the stable production of gasoline. By investigating the factors affecting the long-period smooth operation of two sets of S Zorb units with each processing capacity of 1.5 Mt/a, the measures of feedstock management, adsorbent management and process parameter optimization were summarized. The S Zorb operation cycle synchronized with FCC unit.
EFFECT OF RECYCLING DIFFERENT MATERIALS IN FCC UNIT BY LTAG PROCESS
2023, 54(6):  18-25. 
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The effect of recycling hydrogenated LCO, RLG diesel and kerosene fractions in catalytic cracking unit through LTAG (LCO to aromatics and gasoline) nozzles were analyzed in terms of improving the structure of refinery products and reducing the ratio of diesel to gasoline. The LTAG nozzles in FCC unit were used to reprocess hydrogenated LCO, which improved gasoline yield while increasing the production of vehicle diesel. The combination of LTAG process and RLG process in FCC unit could greatly reduce the output of diesel, decrease the ratio of diesel to gasoline, and increase the yield of light oil and economic benefit by recycling RLG diesel. At the same time, when the catalytic cracking unit recycled the kerosene fractions, more gasoline and LPG could be produced,thus improving the product structure, optimizing the product distribution,which could solve the market problem of jet fuel.
PREPARATION OF MILLIMETER-SIZED MACRO-POROUS ALUMINA SPHERE BY HOT OIL-DROP METHOD
2023, 54(6):  26-31. 
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In order to solve the problems of the high micro-pore proportion, small pore volume of the present millimeter-size alumina sphere and high carbon deposition rate of the supported catalyst prepared by the existing process, the feasibility of preparing millimeter-sized alumina sphere using SB powder and alumina sol by hot oil-drop method was investigated. By optimizing the ratios of SB powder to alumina sol,mass ratio of aluminum to chloride in alumina sol, aging temperature, and aging time, the crushing strength of the prepared alumina pellets was higher than 55 N/pellet, the bulk density was 0.56-0.60 g/mL, the pore volume was higher than 0.75 mL/g, and the specific surface area was maintained above 155 m2/g after being treated with 650 ℃ and 10% water vapor for 48 h. The results of physicochemical analysis showed that the alumina pellet could be used as the support of continuous catalytic reforming catalyst.
EFFECT OF PROMOTER COBALT ON THE PERFORMANCE OF HYDROTREATING CATALYSTS
2023, 54(6):  32-38. 
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A series of CoMo/γ-Al2O3 hydrotreating catalysts with different Co content were prepared and characterized by XRD, H2-TPR, Raman, XPS and in-situ CO-FTIR analysis. The effect of Co content on the morphology of the active metal and the structure of active phase of the sulfided catalysts were investigated and correlated with the hydrodesulfurization (HDS) activity and polycyclic aromatic hydrocarbons (PAH) saturation activity of the catalysts. The results showed that with the increase of Co content, more CoMoO4 species were formed on the surface of the catalysts, and the CoMoO4 species with low crystallinity were more likely to form highly active CoMoS phase during sulfurization, thus improving the HDS activity of the catalyst. However, if the content of Co was too high, more Co9S8 phase with low desulfurization activity would be formed and competitive adsorption with CoMoS phase would occur, which would decrease the HDS activity of the catalyst. Because the active sites of catalyst for desulfurization and hydrogenation were not the same, the formation of Co9S8 phase did not reduce the aromatics saturation activity of the catalyst. When the mass ratio of CoO to MoO3 was 0.3, the catalyst had the best HDS activity, and when the mass ratio of CoO to MoO3 was 0.4, the catalyst has the best PAH saturation activity.
PREPARATION OF AgY MOLECULAR SIEVES AND ITS ADSORPTION PERFORMANCE OF PYRIDINE IN SIMULATED FUELS
2023, 54(6):  39-45. 
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AgY zeolite was prepared by ion exchange method, and characterized by X-ray diffraction. NaY and AgY zeolites were used to the static adsorptive denitrification of pyridine in simulated fuel. The results showed that the adsorption and denitrification capacity of AgY zeolite was better than that of NaY zeolite, and the suitable adsorption and denitrification conditions of AgY zeolite were as follows: an amount of simulated fuel of 15 mL, an amount of AgY zeolite of 0.2 g, an adsorption temperature of 333 K, and an adsorption time of 40 min. The cluster models of NaY and AgY zeolite were established by using Materials Studio software, and the adsorption energy of pyridine on NaY and AgY zeolite and the distance between pyridine and the active center were calculated. The distance between pyridine and the active center of AgY zeolite was smaller than that of NaY zeolite, so the adsorption performance of AgY zeolite was better than that of NaY zeolite. The adsorption behavior of pyridine on AgY zeolite confirmed to the Langmuir-Freundlich mixed model. The adsorption thermodynamics and kinetics of pyridine on AgY zeolites were investigated. The adsorption reaction is a spontaneous process of adsorption entropy increase, and the adsorption process accords with the quasi-second-order kinetic model at the temperature of 333 k.
STUDY ON CO2 REDUCTION BY CdS/CeO2 HETEROJUNCTION NANO-PHOTOCATALYST
2023, 54(6):  46-54. 
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A CdS/CeO2 heterojunction nano-photocatalyst was prepared by hydrothermal method, the physical and chemical properties were characterized by XRD, HR-TEM, UV-vis, etc., photocatalytic performance for CO2 reduction was evaluated, and the reaction mechanism was deduced. The results showed that the CdS/CeO2 heterojunction nano-photocatalyst could widen the visible light absorption range and reduce the band gap of the catalyst compared with single CdS nano-particle and single CeO2 nano-particle. It could effectively delay the recombination of electron-hole pairs, reduce the arc radius and the transfer resistance of electron hole pairs, and thus improve the visible light sensing range and photocatalytic activity of the catalyst. It was proved that the heterojunction nanostructures prepared by semiconductor composite could effectively improve the photocatalytic activity of the catalyst of CO2 reduction. The heterojunction nano-photocatalyst CdCe-100 was prepared by adding 100 mg CeO2 nano-particles into 1 mmol Cd (OOCCH3)2·2H2O aqueous solution, the yield of CO and CH3OH for CO2 reduction was 213 μmol/g and 1 534 μmol/g, respectively, and the catalytic activity of CdCe-100 remained above 93% after six times of reuse.
IN-SITU ORIENTED CONSTRUCTION OF MFI NANO-ZEOLITE MEMBRANES WITH CONTROLLABLE b-ORIENTED LENGTH AND ITS SEPARATION PERFORMANCE FOR n-BUTANE/i-BUTANE
2023, 54(6):  55-63. 
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MFI nano-zeolite membranes were prepared in-situ on alumina supports by one-step constant temperature and two-step varying-temperature crystallization with urea as crystallization regulator. The structure and morphology of MFI zeolite and MFI zeolite membranes were characterized by XRD and SEM. A series of zeolite seeds with high transverse diameter ratio and longitudinal diameter ratio were obtained by adjusting the ratio of urea in the synthetic solution and the two-step in-situ hydrothermal crystallization time at variable temperature. When the amount of urea added in the synthetic solution (based on the mass ratio of urea to silicon) and the crystallization time of 120 ℃ for 6 h and then 180 ℃ for 8 h, the size of the zeolite was the smallest, and the b-axis was the shortest, only 60 nm. Under the same conditions, nano-MFI zeolite membranes with high b-axis orientation were prepared on alumina supports. Extending the crystallization time of the high temperature section to 14 h to obtain a b-axis oriented zeolite membrane with good permeability and separation ability for n-butane/i-butane liquefaction (40% of n-butane and 60% of i-butane), the osmoticflux of n-butane was 2.2×10-7 mol/(m2·s·Pa),and the separation factor was 23.9 under the condition of 25 ℃. The effect of 100 h continuous evaluation was not significantly decreased.
ANALYSIS OF KEY INFORMATION ON MICROSTRUCTURE OF CHUNFENG-TAHE BLENDED ASPHALT
2023, 54(6):  64-69. 
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Based on the evaluation of Chunfeng-Tahe blended asphalt with both high temperature performance and low temperature performance, the asphalt was characterized by FTIR, GPC and 1H-NMR, and the internal microstructural reasons of high and low temperature performance of the blended asphalt with Chunfeng vacuum residue (VR) and Tahe VR were explored. The results showed that Chunfeng VR has longer aliphatic chain and more developed branch chain, which can improve the low-temperature performance of Tahe VR, and make the blended asphalt retain the excellent low-temperature relaxation flow performance of Chunfeng VR. On the other hand, Tahe VR induces the adsorption of corresponding components of Chunfeng VR through its planar arrangement of aromatic ring structure, which makes the blended asphalt retain the characteristics of Tahe VR's highly condensed polycyclic aromatic hydrocarbon compounds and the high-temperature stability of the asphalt materials. By retaining the excellent performance of the initial two VRs, the blended asphalt possesses the good quality characteristics of both high and low temperature performance.
SYNTHESIS AND PROPERTIES OF NOVEL BIS-BENZOTRIAZOLE METAL DEACTIVATOR
2023, 54(6):  70-75. 
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N,N-bis(methylbenzotriazole methylene) dodecylamine metal deactivator was synthesized by condensation reaction of methylbenzotriazole, dodecylamine and formaldehyde. The synthesis conditions were optimized by orthogonal design. The structure and elemental composition of the synthesized product were characterized by IR, MS and elemental analysis, and the performance of the target product was evaluated. The results showed that the yield was over 98.0% under the conditions of optimized ratio of raw material of n(methylbenzotriazole): n (Formaldehyde) : n (alkylamine) = 2.0:2.1:1.0,anhydrous ethanol as solvent,reaction temperature of 80 ℃ and reaction time of 5 h. The relative molecular weight of the synthesized product was 475, and the element composition and molecular ion characteristic peak were consistent with N,N-bis(methylbenzotriazole methylene) dodecylamine. The corrosion inhibition of the synthetic product was excellent, the oxidation induction period was over 350 min, the base value was only about 110 mgKOH/g, the acid value was less than 2 mgKOH/g. The performance of the synthesized product was much better than that of deactivator T551, and had high thermal stability, good oil solubility and good synergistic effect with antioxidant T203 and acid antirust agent T746.
DEVELOPMENT OF SILAHYDROCARBONS FOR THE LUBRICANT OF SPACE MOVING PARTS
2023, 54(6):  76-83. 
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In order to widen the working temperature range of space liquid lubricants, reduce its volatility under high vacuum conditions, improve its lubrication performance and prolong its the space lubrication life, a new kind of space lubricating oil based on silahydrocarbon was designed and synthesized. The various compositions were studied, and a space lubricating oil named RIPP?4758 was developed. All the performance tests were compared with perfluoropolyethers (PFPEs) and multiply-alkylated cyclopentane (MAC), which were widely used in space machinery. The results showed that RIPP 4758 space lubricant had outstanding viscosity-temperature performance, low temperature performance, low volatility and lubrication performance. The application results showed that RIPP 4758 could be applied to a wider working temperature range, high vacuum resistance, and good lubrication and wear resistance.
APPLICATION OF HVI II+10 LUBE BASE OIL IN TURBINE OIL
2023, 54(6):  84-89. 
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Based on the lube base oil resources of SINOPEC Maoming Company, the paper described the problems of corrosion and filterability in the production of turbine oil in recent years. The compatibility of HVI Ⅱ+ 10 (Maoming) with different functional agents and anti-rust inhibitors was analyzed. The results showed that the anti-rust and filtration performance of the turbine oil products prepared with lube base oil HVI Ⅱ+ 10 (Maoming) was poor under the same dosage of functional agent A, and this problem could be solved by using AC 716 anti-rust agent. The filtration and anti-rust performance of L-TSA (A grade) turbine oil could be improved by using functional agent B and functional agent C.
ANALYSIS AND PRACTICE OF INTEGRATED UTILIZATION OF HEAT PUMP IN REFINERY FACING “CARBON PEAKING AND CARBON NEUTRALITY” STRATEGY
2023, 54(6):  90-96. 
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In response to the national strategy of “carbon peaking and carbon neutrality”, the application of heat pump technology has become an effective path to change the energy ladder supply system of refining process. Based on the heat demand and waste heat resource of PetroChina Harbin Petrochemical Company (HPC) in the refining process, it showed that the energy-saving potential of refining enterprises through direct heat exchange or hot water indirect heat exchange has reached a bottleneck.The integrated heat pump technology becomes another way to break the thinking pattern. Through exergy analysis and carbon emission analysis, the key energy-saving factors of steam heating and heat pump heating (compression type, absorption type) were compared and analyzed theoretically, and the optimal application scenario of heat pump technology in oil refining process was given. An example of HPC heat pump waste heat recovery project showed that the heat pump technology in refining industry energy saving and carbon reduction action was significant.
RESEARCH ON INTELLIGENT FAULT DIAGNOSIS SYSTEM OF ETHYLENE PLANT BASED ON DATA ANALYSIS AND BP NEURAL NETWORK
2023, 54(6):  97-104. 
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In view of the characteristics of the strong correlation, continuity and complexity of each unit in the chemical production process, the Aspen simulation was carried out on an ethylene production unit. The data were extracted and the sensitivity analysis was carried out. It was found that the equipment failure could be reflected by the change of heat load of reboiler and condenser in fractionating column. Then, a dynamic model was established by taking the demethane column, deethane column and ethylene rectifying column as examples. The data sets of four observable parameter, temperature, pressure, methane content and feed flow, which caused the change of thermal load, were classified and coded, then the intelligent diagnosis system model of thermal utility (mainly steam) was established by using three-layer BP neural network. 10 000 samples of different observable parameters and their combined data were trained and verified. After the periodic diagnosis results were obtained, the complete fault condition of the integrated equipment was determined. The results of test set sample verification showed that the accuracy of BP neural network diagnosis model was high, reaching 99.75%. The practical application results showed that the fault diagnosis system could quickly and effectively judge the cause of equipment failure in the actual operation.
OPTIMIZATION OF HEAT EXCHANGE NETWORK FOR HYDROGEN PRODUCTION UNIT FROM COAL WATER SLURRY
2023, 54(6):  105-110. 
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Hydrogen production from coal water slurry (CWS) is one of the important hydrogen sources in the refinery. It was found that the heat exchange network had the problems of insufficient heat recovery and large consumption of circulating water. The analysis results showed that the current heat exchange network could not recover energy sufficiently and consumed excess cooling water, and the energy saving potential of the unit was 7 723 kW. Based on the analysis results, the heat exchange network was optimized according to the pinch principle, which could save 7 723 kW of heat utility and 11.524 million Yuan annually. The optimized transformation scheme had the advantages of low cost, short payback period, obvious energy-saving effect and greatly increased economic benefits.
STUDY ON INFLUENCING FACTORS AND OPTIMIZATION OF CONDITIONS FOR TOTAL ACID VALUE DETERMINATION OF LUBRICATING OIL BY POTENTIOMETRIC TITRATION
2023, 54(6):  111-119. 
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Acid value is an important index to measure the quality and performance of lubricating oil products. The influence of single factors, such as titrating solvent, sample volume, titrating rate and titrating mode, on acid value determination of lubricating oil by potentiometric titration was discussed. In view of the existing problems, the response surface method was used to characterize the synergetic effect of each single influencing factor, screen the optimal test conditions, and avoid the influence of the improper selection of test conditions on the test results. The results showed that the predicted results by response surface method were basically consistent with the actual test results, which could optimize test conditions, shorten test time and reduce the number of test error.
CAUSE ANALYSIS AND COUNTERMEASURES FOR COKING OF FEED HEAT EXCHANGER IN S Zorb UNIT
2023, 54(6):  120-125. 
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Coking and blockage of feed heat exchanger in the S Zorb unit of a refining and chemical company affected the long-term operation of the unit and safe and stable production of the whole plant. Through analysis and judgment, the main reasons of coking and blockage in the heat exchanger were the high content of gum in the feed gasoline, unclean on-line cleaning of the heat exchanger and impurities in the feed.The coking and blockage situation of the feed heat exchanger in the unit has been obviously improved by taking some measures, such as strengthening the management of feedstocks, improving the cleaning method of heat exchanger, and adding scale inhibitor. The operation period of the heat exchanger was increased from 2 months to more than 14 months.
RESEARCH ON THE CORROSION-EROSION PREDICTION OF FCC SLURRY PIPE BY NUMERICAL SIMULATION
2023, 54(6):  126-132. 
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The outlet pipeline of slurry pump for FCC unit was taken as the research object. Based on the analysis of high-temperature sulfur corrosion and erosion mechanisms, a numerical simulation method for predicting damage characteristics of pipelines in the presence of both corrosion and erosion was established. The distribution of the flow field parameters, the concentration of the corrosive medium and the collision angle of the solid catalyst were obtained by coupling multi-physical field models. The parameters such as erosion rate, corrosion rate, and surface thinning rate were used to quantitatively characterize the damage rule. The results showed that the irregular movement of solid particles could be driven by high pressure and turbulent flow pattern, which resulted in a large risk of erosion and wear; the distribution of the corrosive medium near the wall of the pipeline was not uniform. Under the synergistic action of erosion and corrosion, the average damage rate of pipeline wall was 0.46 mm/a, and the maximum damage rate was 0.55 mm/a. The damage behavior and thinning rate predicted by the model were in good agreement with the experimental results, which could provide support for monitoring and life prediction of pipelines.
EBULLATE-DBED RESIDUE HYDROCRACKING PROCESS AND ITS ROLE IN THE STRUCTURAL TRANSFORMATION FOR REFINARY
2023, 54(6):  133-138. 
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In recent years, the domestic oil refining capacity continues to increase, overcapacity has intensified, and the oil refining has been transforming to the chemical industry. In heavy products, the standards of low sulfur petroleum coke and low sulfur heavy marine fuel oil are about to be implemented or have been implemented, the comprehensive utilization of residual oil is very important. The ebullated-bed residue hydrocracking process has the advantages of the high yield of light products, high aromatics content in light products and low sulfur content in heavy products. Three kinds of ebullated-bed residue hydrocracking process have been developed at domestic and foreign markets, which are H-Oil process of Axens, LC-Fining process of CLG and STRONG process of FRIPP. According to the technology and product characteristics of ebullated-bed residue hydrocracking, the process could be used in refining and chemical enterprises to make residue light to provide intermediate feedstocks for chemical products. The unconverted residue could also be used to produce low sulfur petroleum coke and low sulfur heavy marine fuel oil or its components.