Table of Content

12 June 2024, Volume 55 Issue 6

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COMPONENT-BASED REFINING ACCELERATINGTHE TRANSITION OF OIL REFINING TO CHEMICALS PRODUCTION

2024, 55(6):  1-8. 

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Under continuous superposition ofmultiple development pressures, the transformationand upgradingof traditional refining industry is imminent. In order to make full use of the value from different molecular and component in crude oil and produce high value products economically and efficiently, the research of component-based refining has become an important direction to helpthe petrochemical industryto upgrade rapidly and move towards molecular refining. By comparing with traditional refining (fraction-based), the important relationship between specific components of crude oil and the target products,the implementation steps and key supporting technologies of the component-based refining were analyzed, and theeffects on increasing utilization ratio of crude oil resources and added value of products, reducing production cost and carbon dioxide emission and developing new materials were studied. In different component-based refining cases, the yield of ethylene and the benefit per ton of crude oil could be increased by 12.7% and 160.12 Yuan/t, respectively,and thecarbon dioxide emission reductionwas about 19.83 kg per ton crude oil. This study provides an important reference for the development and application of separation technology and key refining technology in the future.

NORMAL HEPTANE ISOMERIZATION CATALYZED BY IONIC LIQUID [Et₃NH]Cl-AlCl₃ PROMOTION BY CIRCULATION OF ISOBUTANE

2024, 55(6):  9-17. 

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Light hydrocarbonisomerization usually takes C₅ and C₆ hydrocarbons as feedstocks, and C₇+ hydrocarbons in the process of isomerization are prone to a relatively severe cracking reaction, resulting in low yield of isomerized oil. As a novellow-temperature catalyst, ionic liquid has also poor adaptability to macromolecular hydrocarbon feedstocks.Therefore, in the process of macromolecular hydrocarbon isomerization, inhibiting side reaction and improving the yield of isomerized oil during the isomerization of larger hydrocarbons have been the difficulty and focus of research. Based on the mechanism of the alkane isomerization catalyzed by ionic liquid, isobutane criculation can inhibit side reaction and promote the isomerization reaction, which served to reduce the content of C₄ alkanes in the isomerization product and increase the yield of isomerized oil. The influence of process conditions such as the addition amount of isobutane, reaction temperature, reaction time, stirring rate and acid-to-alkane ratio on the n-heptane isomerization catalyzed by chloroaluminate ionic liquid was systematically studied. The results showed that the circulation of isobutane significantly decreased the yield of the by-product C₄ components. The reason was that the substantial presence of isobutane in the system could significantly accelerate the rate of hydrogen transfer during the reaction, effectively inhibit the secondary reactions such as cracking and disproportionation. Under the conditions of an isobutane dosage of 30%, a reaction temperature of 50℃,a reaction time of 1 h,a stirring speed of 1500 r/min and an acid-to-alkane ratio of 1, the n-heptane conversion reached 91.0%, with isomeric hydrocarbon selectivity and liquid yield of 87.2% and 93.5%, respectively. Compared to those of the reaction system without isobutane, the isomeric hydrocarbon selectivity and liquid yield of the reaction system with isobutane at similar conversion rate of n-heptane increased by 16.0 percentage points and 14.8 percentage points, respectively.

EXPLORATION OF HIGH VISCOSITY OIL SLURRY DESOLIDIFICATION TECHNOLOGY

2024, 55(6):  18-23. 

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The solid particle of catalyst in FCC slurry is the bottleneck that affects its physical and chemical properties and high-value utilization. Therefore, slurry desolidification technology becomes the key breakthrough for further processing. Reagent sedimentation method is the main method of oil slurry desolidification, but the application effect is not ideal for high viscosity oil slurry. For further research, the slurry from a refinery was chosen as sample and named slurry Z. In order to reduce the ash content of the oil slurry, the viscosity of the oil slurry was changed by increasing the temperature, introducing dilution component and adding viscosity modifier. The results showed that the desolidification rate of the oil slurry could be increased to more than 80% by increasing the temperature to 130 ℃ or adding 0.1% viscosity modifier, and the desolidification rate of the oil slurry could be increased to more than 95% by adding dilution components such as diesel fraction or aromatic solvent oil.

EFFECT OF BLENDING DCC DIESEL INTO HYDROCRACKING UNIT OF NAPHTHENIC BASE INFERIOR PARAFFIN GAS OIL

2024, 55(6):  24-31. 

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In order to maximize the efficiency of resource utilization, a company carried out an industrial test of mixing about 5% deep catalytic cracking(DCC-plus) diesel fraction into 2.1 Mt/a naphthenic low-quality gas oil hydrocracking unit according to the feed characteristics of DCC-plus diesel and gas oil hydrocracking unit. The industrial test results showed that the yield of jet fuel increased by 1.93 percentage points, the smoke point of jet fuel increased by 1.2 mm, and the cetane value of hydrogenated diesel increased by 1.9 units, which improved the properties of jet fuel and diesel. After blending DCC diesel , the temperature rise of refining reactor increased obviously, and the consumption of hydrogen and electricity increased significantly. It is estimated that after blending DCC-plus diesel, which was originally used as a fuel oil blending component, was converted into heavy naphtha, jet fuel and diesel components with higher added value.The profit was 467 Yuan/t (in terms of DCC-plus diesel), and the economic benefit was 40.368 million Yuan/a.

INDUSTRIAL PRACTICE OF HYDROCRACKING UNIT TO PROCESS DIESEL FRACTION FROM RESIDUAL HYDROTREATER

2024, 55(6):  32-35. 

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In order to realize the high value-added utilization of the diesel fraction from residue hydrotreating (RHT) unit and give full play to the role of hydrocracking units in reducing diesel fuel, a commercial test of RHT diesel fraction was carried out in a hydrocracking unit. The load rate of hydrocracking unit was 56%, and after blending 21.4% RHT diesel fraction, most of the RHT diesel fraction could be converted into non diesel components, with an apparent conversion rate of 48.34%. The mass fraction of sulfur and nitrogen in hydrocracking diesel products was 1.3 μg/g and less than 0.3 μg/g, respectively. Compared to that of the diesel hydroupgrading unit, the properties of diesel product were slightly improved, with the cetane number of 62.7, which increased by about 17, and the total output of diesel product decreased by 14.09 t/h. The hydrocracking unit was used to process RHT diesel fraction, the process route was optimized, the component of diesel fuel was effectively reduced, and the quality of diesel fuel was improved. It can provide an industrial case for the high value-added utilization of RHT diesel fraction.

CHARACTERISTICS AND COMMERCIAL APPLICATION OF SLURRY BEDRESIDUE HYDROCRACKINGTECHNOLOGY

2024, 55(6):  36-43. 

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The slurry bed residue hydrocracking unit with the largest single design scale (3.0Mt/a)using imported process technology in China was firststarted in a company. After 177 days of continuous operation, the 72 h performance calibration test was carried out under the condition of86% actual processing load. The results showed that using the mixed feedstock of vacuum residue and catalytic cracking slurry with a carbon residue of 23.68%,a metal (nickel+vanadium) mass fraction of 138 μg/g, a sulfur mass fraction of 4.82%, and a C₅ asphaltene mass fraction of 17.65% ,under the conditions of a feed rate of 307.2 t/h ,a reactor pressure of 15.7 MPa, an average reaction temperature of 428 ℃, a mass ratio of fresh raw material oil tocirculating residue oil at the bottom of the vacuum column of 1.21,a Mo mass fraction of 1 650 μg/g and a gas-holding rate of 26.0% to 27.5%, the conversion rate was 90.0%, the mass fraction of tetrahydrofuran insoluble matter at the bottom of the vacuum column was 7% to 8%, the mass fraction of molybdenum was 2678 μg/g, and the energy consumption of the unit was 1906.50 MJ/t. The total pressure drop during the calibration period was 9.53 kPa, which was 25.1 times of the design value, so the unitwas difficult to raise the load.To solve the problems of increased pressure drop in the packed bed of the vacuum column and insufficient extraction of gas oil components from the oil residue, the operation of vacuumcolumn could be adjusted and technical transformation of the vacuum column could be tried.

SYNTHESIS OF Ni@SiO₂ AND ITS CATALYTIC PERFORMANCE FOR DICYCLOPENTADIENE HYDROGENATION

2024, 55(6):  44-51. 

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Exo-tetrahydrodicyclopentadiene (exo-THDCPD), the main component of JP-10 fuel, is usually synthesized by hydrogenation and isomerization of dicyclopentadiene (DCPD). The saturated hydrogenation of DCPD is the key step, sothe synthesis of DCPD hydrogenation catalyst is particularly important. Based on this,Ni@SiO₂ catalysts with a nickel mass fraction of 30% were prepared by different synthesis methods (such as deposition precipitation method, ammonia evaporation method, gel method and impregnation method),using nickel nitrate hexahydrate and silica sol as raw materials,and applying to the hydrogenation of DCPD to tetrahydrodicyclopentadiene (endo-THDCPD).It was found thatthe Ni@SiO2 catalyst prepared by ammonia evaporation and calcination reduction had the characteristics of layered nickel silicate, abundant Lewis acid, Ni nano-scale dispersion and rich mesoporesstructure, which made it exhibit excellent catalytic activity in DCPD hydrogenation reaction. When the reaction temperature was 25℃, the conversion of DCPD was 99.9 % and the yield of endo-THDCPD was 99.9 %.

EFFECT OF OXYCHLORINATION CONDITIONS ON Pt REDISPERSION IN CONTINUOUS REFORMING CATALYST

2024, 55(6):  52-60. 

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The effects of oxychlorination conditions on redispersion of Pt grains in continuous reforming catalyst were investigated ina fixed bed reactor. The results indicated that increasing the temperature of oxychlorination and decreasing the molecular ratio of water to chlorine were beneficial to the redispersion of Pt grains and the metal dispersion of the catalyst. The improvement of metal dispersion was also related to the initial particle size of Pt grains. When the initial particle size of Pt grains was above 100 nm, it was difficult to increase the metal dispersion. Based on the above-mentioned laws, the oxychlorination conditions in an industrial plant were optimized. After 9 months of optimization, the metal dispersion of the catalyst recovered from 0.46 to 0.81 and its appearance was uniform white. The catalytic performance was recovered and the yield of aromatic increased by 2.3 percentage points.

EFFECT OF LOADING MODE OF La ON VANADIUM RESISTANCE PERFORMANCE OF Y ZEOLITE

2024, 55(6):  61-65. 

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Y2, Y3 and Y4 zeolite samples were prepared by loading the same content of rare earth La into Y zeolite via different methods, and the physicochemical properties and microactivity of Y zeolite samples were investigated systematically. The results showed that the La existed in ionic state in Y2 zeolite preparedby impregnation method, the La ions migrated into the internal structure of zeolites more easily during calcination, and most of them entered into the α-type supercage of zeolites, in the Y3 and Y4 zeolites prepared by precipitation method, La existed in non-ionic state and migrated less into the internal structure of zeolites during calcination. Compared with Y2 zeolite prepared by impregnation method, Y3 zeolite prepared by precipitation of La and oxalic acid first and then loading on the zeolite had better hydrothermal stability and activity, which indicated that the La present on the surface could improve the vanadium resistance of Y zeolite.

EXPERIMENTAL STUDY ON THE OXIDATIVE ABSORPTION OF H₂S BY CuCl₂ IN COOPERATION WITH FeCl₃/UREA DEEP EUTECTIC SOLVENT

2024, 55(6):  66-73. 

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In order to solve the problem of removing H₂S from small to medium-scale conventional sulfur-containing natural gas, a kind of FeCl₃/UREA deep eutectic solvent (DES) was synthesized from UREA and ferric chloride hexahydrate (FeCl₃.6H₂O) with addition of CuCl₂ to obtain FeCl₃/UREA-CuCl₂ desulfurizer. The structure and thermal stability of the DES were determined, and the effects of raw material ratio, CuCl₂ concentration, H₂S gas flow rate and temperature on the desulfurization performance were investigated through desulfurization experiment, and the regeneration process was also investigated. The results showed that the DES could exist stably at 80℃, and the DES with molar ratio of FeCl₃/UREA of 1:1 had better desulfurization performance.The introduction of CuCl₂ could significantly improve the desulfurization performance, the maximum sulfur capacity was 9.64 g/L. The desulfurizer is more suitable for desulfurization at lower gas flow rate and can be regenerated by passing O₂. The effect of the desulfurizer has little change after repeated use. The product of desulfurization is high purity rhombohedral sulfur (α-sulfur). The desulfurizer has the advantages of low cost of raw materials, simple synthesis, and high efficiency of oxidationand absorption of H₂S and conversion of H₂S into high purity sulfur,which can provide a reference for industrial natural gas desulfurization.

COUPLING CONVERSION OF METHANOL AND BUTYLENE TO PROPYLENE ON Ce-MODIFIED HZSM-5 ZEOLITE CATALYST

2024, 55(6):  74-82. 

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In order to further improve the catalytic performance of HZSM-5 zeolite in the coupling conversion of methanol and butylene to propylene, a series of Ce-modified HZSM-5 (xCe/HZSM-5) catalysts with different Ce-loading were prepared by impregnation method. The effects of Ce-loading and reaction conditions (methanol/butylene molar ratio, reaction temperature and space time) on the catalytic performance of catalysts were systematically investigated. Combined with the catalyst characterization results, the effects of Ce modification on the performance and physicochemical properties of catalysts were analyzed, and the structure-activity relationship of xCe/HZSM-5 catalyst was discussed. The results showed that under the optimum reaction conditions including atemperature of 550 ℃, a pressure of 0.1 MPa ,a molar ratio of methanol/butylene of 0.8 and a space time of 2.3(g_cat.h)/mol_CH2, 2.5Ce/HZSM-5 catalyst with 2.5% Ce loading (w) showed the highest propylene yield of 41.9%. The interaction between Ce and hydroxyl groups (OH) on the HZSM-5 zeolite decreased the Bronsted (B) acid amount and formed a new Lewis (L) acid site Ce(OH)²⁺, which caused the reduction of the ratio of B/L acid sites, thus, the selectivity and yield of propylene were improved.

STUDY ON FORMATION OF BETA ZEOLITE HONEYCOMB MONOLITHS CATALYST BY USING RESPONSE SURFACE METHOD

2024, 55(6):  83-91. 

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Beta zeolite is an industrial catalyst with excellent performance in practical application due to its unique 3-D 12-membered ring channel structure, which can provide more active component adsorption sites.In industrial use,the honeycomb monolith catalyst has the advantages of high flux, uniform flow field,small pressure drop and non-clogging, which is the optimal solution for gas-solid or liquid-solid catalytic reactions.However, because of the high water absorption and shrinkage of Beta zeolite, it is difficult to form honeycomb, which greatly limits the industrial application of Beta zeolite.To solve the above problems,pseudoboehite (SB powder) was selected as binder, HNO₃ as solvent, and sesbania powder as extrusion-aid, and a series of Beta zeolite honeycomb monoliths were prepared at a water-to-powder ratio of 0.6. Based on the response surface method, the effect of the ratio of each raw material on the mechanical strength of the honeycomb monoliths was evaluated.The function of the second order polynomial approximation model of the relationship between the mechanical strength of the monoliths and the three variables was obtained. The reliability of the predicted model was proved by comparing the results with the predicted values. The optimal forming conditions of Beta honeycomb monoliths were found by using the model,which were the pseudo-boehmite mass fraction of 36.1%, the nitric acid mass fraction of 8.4%, and the cyanine powdermass fraction of 4.7%.

EFFECT OF ZEOLITE CONTENT ON THE PERFORMANCE OF DIESEL HYDRO-UPGRADING CATALYST FOR MAXIMUM INCREASING ETHYLENE FEEDSTOCK

2024, 55(6):  92-98. 

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In order to reduce oil and increase chemical, decrease the diesel/gasoline ratio, broaden the source of ethylene feedstock, and improve the economic benefitof refining and chemical enterprises, the straight-run diesel can be used as ethylene feedstock after hydro-upgrading. The effects of zeolite content in the catalyst on the yield and properties of modified diesel at different reaction temperature were investigated. The results showed thatthe total acid content and weak acid ratio of the catalyst increased with the increase of zeolite content. The aromatics index(BMCI) of modified diesel decreased with the increase of zeolite content and reaction temperature, but the yield decreased.At the yield of 50%,the BMCI of modified diesel could be reduced to 8.6 ,which was 25.7 less than that of the raw diesel,making it a high-quality ethylene feedstock.

THERMODYNAMIC CALCULATION FOR DEHYDROGENATION REACTION OF THICK RING COMPOUNDS

2024, 55(6):  99-106. 

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The Benson group contribution method was used to estimate the standard molar enthalpy of formation, absolute entropy and constant pressure molar heat capacity of compounds lacking in the hydrogenation reaction network of phenanthrene (PH), pyrene (PY) and 2-methylphenanthrene (2-MP). Based on physical property data, the enthalpy change, Gibbs free energy change, and conversion rate of each reaction in the PH, PY and 2-MP hydrogenation reaction network were calculated. The calculation results showed that the dehydrogenation reaction in the hydrogenation reaction network of PH, PY and 2-MP was all endothermic reactions, and there was a temperature-sensitive region inthe equilibrium conversion of dehydrogenation reaction in the hydrogenation network of PH, PY and 2-MP. The equilibrium conversion rate of each dehydrogenation reaction approached 100% by adjusting the reaction temperature, and the existence of methyl branched chain made the dehydrogenation reaction easier for the hydrogenation products of polycyclic aromatic hydrocarbons with the same degree of hydrogenation. For the hydrogenation products of polycyclic aromatic hydrocarbons with the same degree of hydrogenation and number of methyl branches, the more aromatic rings there were, the easier the dehydrogenation reaction was. Under reaction conditions of a pressure of 0-2 MPa and a temperature of 300-800 K, high temperature and low pressure were favorable for the dehydrogenation reaction in the hydrogenation reaction network of PH, PY and 2-MP.

RESEARCH ON 3D RECONSTRUCTION OF MICROSTRUCTURE OF RESIDUAL OIL HYDROGENATION PROTECTANT BASED ON MICRO-CT

2024, 55(6):  107-114. 

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Micro computed tomography (Micro-CT) is a non-destructive testing method that can quickly and accurately establish the 3D structure and composition of analytical objects. Taking the residue hydrotreating protectants after industrial operation as the research object, Micro-CT was introduced to characterize the microstructure of the residue hydrotreating protectant in 3D model creatively.By comparing the discrete graph of Micro-CT slice data with the distribution of SEM element discrete graph,the pores, metal sediments in the protectant were identified and confirmed, and 3D reconstruction technology was used to reconstruct the three-dimensional distribution model of pores and metal sediments.The results indicated that Micro-CT could construct 3D structures of protectant from micron to nano-scale. There were still a large number of unused closed pores inside the protectant, and increasing the connectivity of the pores was the key to improving the efficiency of the protectant.As a novel microstructural analysis method for residual oil hydrogenation protectant,Micro-CT can provide guidance for the development of residual oil hydrogenation protectant.

HYDRODYNAMIC CHARACTERISTICS IN EXTERNAL-LOOP AIRLIFT SLURRY REACTORS

2024, 55(6):  115-121. 

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The hydrodynamic characteristics in an external-loop airlift were investigated and the influences of operating conditions on gas holdup and slurry circulating velocity were analyzed.Three measurement methods were used to obtain the values of gas holdup and the results showed that these methods were of good accuracies.Three types of gas distributors were used during the hydrodynamic experiments, and the pipe ring distributor with hold at the bottom was recommended based on the experimental data comparison. It was found the relationship between gas holdup and slurry circulating velocity was linear, and correlations were developed to predict the values of slurry circulating velocity with average error less than 20%.

EMISSION CHARACTERISTICS AND RISK ASSESSMENT OF VOCs IN A TYPICAL PETROCHEMICAL INDUSTRIAL PARK

2024, 55(6):  122-129. 

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In order to study the emission characteristics,regularity and influence of volatile organic compounds (VOCs) from the petrochemical industry, VOCs in the air arounda petrochemical industrial park in North China was monitored, and environmental risks and human health riskswere assessed. The results showed that main VOCs in the air were alkane and olefin, and the VOCs in most of the sampling sites were low in content, and similar in composition and no obvious characteristic pollutants. The VOCs content around some sampling sites such as air flotation tank and ethylene plant was higher, and the VOCs composition were obviously affected by the devices emission. In general, low carbon alkanes such as ethane,propane and butane, and low carbon olefins such as ethylene and propylene were the main species in the petrochemical industrial park. The generation of ozone was mainly contributed by olefin, andpropylene, ethylene, propane, toluene, m/p-xylene and other compounds were the key active species. Aromatic hydrocarbons such astoluene, m/p-xylene, benzene and o-xylene were the main components contributing to the formation of secondary organic aerosol (SOA). The results of health risk assessment showed that VOCs in the ambient air of the petrochemical industrial park did not have a high carcinogenic risk to the employees,and the non-carcinogenic risk was low.

ENERGY VARIATION AND FLEXIBILITY OPTIMIZATION OF MULTI-PERIOD ATMOSPHERIC AND VACUUM DISTILLATION UNIT HEAT EXCHANGER NETWORK

2024, 55(6):  130-136. 

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The energy consumption of atmospheric and vacuum distillation unit is the highest in refinery, and the optimization of heat exchanger network is an effective means of energy saving. Given the variability of crude oils, heat exchanger network that was previously designed for specific crude oils is no longer optimal for other crude oils. A multi-period flexible optimization method was proposed: firstly, Aspen Plus was used to simulate the process of different crude oil periods; then pinch design method was adopted and Aspen Energy Analyzer was used to simulate the current heat exchanger network, identify the pinch position offset, find the unreasonable energy use, and eliminate some common cross-pinch heat transfer by changing the pipeline structure and adjusting the heat transfer matching. The application results in a refinery showed that the multi-period flexible design could save 1 421, 880, 3 842 and 3 421 kW of heating furnace heat load and equivalent cooling water heat load in period 1, 2, 3 and 4, respectively. Further study and flexible design of multi-period heat exchanger network can make greater contribution to energy saving and consumption reduction in refineries

DISCUSSION ON THE NEW INTEGRATED MANAGEMENT MODELOF “LARGE SEWAGE PLANTS” IN REFINING AND CHEMICAL ENTERPRISES

2024, 55(6):  137-142. 

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In view of the problem that the complex and varied characteristics of wastewater in refining and chemical enterprises and the simple and extensive process operation mode was difficult to adapt to the increasingly strict discharge standards, a new integrated management mode of  “large sewage plant” was put forward. Through the three links of “sewage, activated sludge and waste gas” between sewage plants, and the two centralized modern and innovative management methods of “centralized management of pharmaceuticals and centralized control of operations”, we coordinated the environmental protection resources of the enterprises, maximized to extend the environmental protection radiation margin of the sewage plants, and achieved the unified management of the sewage system, the dynamic allocation of contaminant load and the utilization of internal resourcing, thus achieving a win-win result of environmental protection and economic benefits.

APPLICATION OF 95+ TECHNOLOGY IN FIRED HEATER AND ITS EFFECTS OF ENERGY-SAVING AND EMISSION REDUCTION

2024, 55(6):  143-147. 

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The technical route and application effects of high-efficiency super-clean waste heat recovery 95+ technology in the fired heater of a refinery were introduced. The cores of the technology lies in the fuel gas purification system and the fuel gas-airdouble parallel heat exchange system,as well as the two-stage air preheater arrangement. The results of application in many units showed that 95+ technology could meet the requirements of design index and had considerable economic and social benefits.It couldbe used as a reference for energy-saving and emission reduction in similar types of units or other fired heaters in future.

SYNTHESIS AND PERFORMANCE RESEARCH OF CYCLIC DICARBOXYLIC ACID MONOESTER ANTI-WEAR AGENT

2024, 55(6):  148-153. 

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Because of the ring tension of the cyclic structure, its low-temperature performance is better than that of long-chain alkanes. A series of monoester products were synthesized by esterification of several cyclic anhydride and alcohol (ethers) as raw materials, and their anti-wear effects and low-temperature performance were analyzed respectively. The research results showed that among the studied cyclic dicarboxylic acid monoester products, the methyl hexahydrophthalic anhydride (MHHPA) reacted with 2-Butoxyethanol (2-B) to prepare methyl hexahydrophthalic ethylene glycol butyl ether monoester (2-BM), which had both good anti-wear performance and low-temperature properties. With an additive amount of only 200 μg/g in ultra-low sulfur diesel, it can significantly improve the lubrication performance of diesel, reducing the average wear scar diameter (WSD) by 242 μm, decreasing the average friction coefficient by 51% and increasing the average oil film coverage by 10%.The freezing point of 2-BM is -42 ℃, which has a good application prospectat low-temperature conditions.

PREPARATION AND PERFORMANCE RESEARCH OF AROMATIC AMINE OLIGOMER ANTIOXIDANT FOR LUBRICATING OIL

2024, 55(6):  154-159. 

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Aromatic amine oligomer antioxidants for lubricating oil were prepared by formaldehyde condensation method, the effects of different catalytic conditions on the structure and properties of the products were investigated, and triethylamine was selected as the catalyst. The results indicated that the formaldehyde condensation reaction of N-octylphenyl-1-naphthylamine under alkaline catalysis mainly occurs on the aromatic ring, and the product had good antioxidant performance for lubricating oil. The optimum synthesis conditions were as follows: triethylamine as catalyst, a reaction temperature of 65 ℃, a molar ratio of N-octylphenyl-1-naphthylamine to polyformaldehyde of 1:0.75, and a reaction time of 40 h.

DETERMINATION OF DISSOLVED OXYGEN CONTENT IN OIL PRODUCTS BY RAPID LIQUID PHASE EXTRACTION METHOD

2024, 55(6):  160-163. 

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Dissolved oxygen has adverse effects on the properties or processing performance of oil products like crude oil, fuels and industrial chemicals. However, current detection methods have problems such as cumbersome operation, poor adaptability or poor data precision. To solve these problems, liquid phase rapid extraction method was applied to determine the dissolved oxygen in oil products using oxygen sensor as detector. The results indicated that the determination time was less than 3 min, the recovery rate of oxygen was between 94% and 104%, the mean standard deviation for five parallel determinations was less than 3% and the detection limit was less than 1.5 mg/L.

DETERMINATION OF PLATINUM AND PALLADIUM CONTENT IN CATALYST BY ICP-OES

2024, 55(6):  164-171. 

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A novel method was developed to determine platinum and palladium content in industrial reforming oil decolefin catalyst under single acid closed digestion condition by ICP-OES. The effects of pretreatment and digestion conditions on the digestion of catalyst were investigated, and the digestion effects of the single acid digestion and conventional mixed acid digestion were compared. Additionally, this study systematically discussed the selection basis for spectral lines used in platinum and palladium analysis, as the influence of aluminum matrix on measured elements, impact of impurity elements, and interference between Pt and Pd elements results. The pre-treatment and digestion conditions for single acid were determined as follows: the catalyst samplewas burned at 550 ℃ for 4 h in air atmosphere and ground to a particle size of less than 120 μm; 0.2 g samples and 3 mL concentrated hydrochloric acid were added and digested in an airtight digestion tank at 180 ℃ for 6 h. Compared with the conventional mixed acid digestion method, the established method is simple, rapid and accurate, and has the advantages of less acid consumption,being friendly to laboratory personnel and environment. The method can be applied to the accurate determination of Pt and Pd in the range of 2.08-12 500 μg/g Pt and 2.67-12 500 μg/g Pd in the catalysts utilized in industrial reforming.

RESEARCH PROGRESS OF SEPARATION AND ANALYTICAL METHODS FOR METALLOPORPHYRINS IN PETROLEUM

2024, 55(6):  172-178. 

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Metal elements in petroleum can adversely affect petroleum processing. Some metal elements can be removed by electrodesalination, while the metal porphyrin compounds are more difficult to remove. Metal porphyrin compounds have complex structure and generally concentrated in colloid and asphaltene. With the development of analytical technology, a comprehensive understanding of the metal porphyrin compounds has been gradually gained. This paper systematically summarized the research progress of analytical methods for metal porphyrin compounds, outlined the characteristics of various separation and characterization methods, and gave an outlook on the direction of research on the molecular structure of metal porphyrins by new analytical methods.