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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 August 2021, Volume 52 Issue 8
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    DEVELOPMENT BACKGROUND, DEVELOPMENT IDEA AND CONCEPTUAL DESIGN OF FCC PROCESS FOR TARGETED CRACKING TO LIGHT OLEFINS
    2021, 52(8):  1-11. 
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    Light olefins are important petrochemical raw materials, mainly produced by steam cracking, fluid catalytic cracking, olefin cracking process and methanol to olefins. Through technical characteristics analysis of the mentioned processes, it is found that the ratio of ethylene to methane in steam cracking and fluid catalytic cracking processes is too low, accompanied by high methane yield. The source of crude materials for the olefin cracking process is insufficient, while that of methanol to olefins process mainly comes from coal to methanol, resulting in high carbon emissions. Given the existing series of scientific problems in the production of light olefins, the targeted cracking to olefin process is proposed. The innovation is carried out from three aspects of feedstock structure, catalyst active component and catalytic reaction engineering. Through deep integration of existing technologies, four different schemes for producing ethylene + propylene + butene, ethylene + propylene, propylene and propylene + butene are formed, and the production schemes can be flexibly switched.
    EXPERIMENTAL STUDY OF RESIDUUM TO CHEMICALS（RTC） TECHNOLOGY
    2021, 52(8):  12-16. 
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    In order to broaden the resource of olefin production in petrochemical industry, and to utilize the heavy oil for high value, a serious of experiments for residuum to chemicals (RTC) technology was carried out on a pilot plant. The results showed that as compared with deep catalytic cracking (DCC) technology, the yields of LPG and propylene in RTC process were enhanced remarkably, and the yield of dry gas and coke were reduced when processing hydrotreating residuum blended feedstock. The RTC technology had good effect on the product distribution and product selectivity when processing heavier hydrotreated residuum.
    HIGH-EFFICIENCY CONVERSION ENGINEERING SOLUTION FOR INFERIOR RESIDUE
    2021, 52(8):  17-22. 
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    Aiming at the problem of unqualified high sulfur coke delivery in delayed coking unit caused by processing heavy and inferior crude oil, a high-efficiency conversion engineering solution for inferior residue was developed. Several new technologies were integrated into catalytic cracking unit, including reactor anti-coking technology, feed oil emulsification and atomization technology, 10 MPa grade steam generation technology, separation and processing technology of LCO and HCO, absorption and stability system energy-saving technology and flue gas purification technology, etc. The new solution can be used to carry out high-efficiency catalytic cracking for inferior residue in refineries and partially replace delayed coking technology to solve the problem of low value-added and high sulfur coke. The solution can increase liquid product yield, and reduce energy consumption of the unit and the whole plant.It is environmentally friendly and conductive to the FCC process, which breaks through the bottleneck of feedstock selection and significantly improve the economic benefits of refineries.
    OPTIMIZATION OF CO-PYROLYSIS PERFORMANCE OF LIGHT HYDROCARBON AND C4
    2021, 52(8):  23-27. 
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    In view of the shortage of ethylene feedstock and C4 excess in refinery, the pyrolysis performance of light hydrocarbon and refinery C4 feedstock was studied by using a small steam pyrolysis simulation experimental device. The effect of C4 addition and process parameters on the yield of triene (ethylene + propylene + butadiene，the same below) in SC-1 pyrolysis furnace was investigated. The experimental results show that the optimum mass fraction of C4 is 10%－20%, the suitable pyrolysis temperature is 840－850 ℃, and the dilution ratio (mass ratio of deionized water to feed oil) is 0.5, the yield of ethylene is 30.19%－31.87%, the yield of propylene is 16.57%－18.20%, and the yield of triene is 53.60%－53.77%, respectively. It can be seen that the co-pyrolysis of C4 and light hydrocarbon not only expands the feed source of ethylene, but also increases the added value of C4 products.
    DEVELOPMENT OF PRODUCTION PROCESS OF PETROLEUM-BASED RUBBER PLASTICIZER A1004 AND APPLICATION IN INSOLUBLE SULFUR
    2021, 52(8):  28-32. 
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    The rubber plasticizer A1004 derived from vacuum distillates was prepared through hydrogenation deacidification-furfural refining-clay refining combined process, and the performance in insoluble sulfur was evaluated. The results showed that the combined process could be used to prepare rubber plasticizer A1004 that met the requirements of GB/T 33322—2016, and the product yield could reach up to 65.7% with the aromatic carbon fraction (CA) of 10.7%. The rubber plasticizer A1004 had a good performance in insoluble sulfur.
    PROBLEM ANALYSIS AND OPTIMIZATION SUGGESTIONS OF AMINE LIQUID SYSTEM IN PETROLEUM REFINERY
    Zhang Hongliang
    2021, 52(8):  33-36. 
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    Through correspondence and on-site investigation, the operating conditions of amine liquid installations in 28 petroleum refineries were analyzed in terms of the number of amine liquid systems, the circulation volume of amine liquid, the concentration of amine liquid, and the hydrogen sulfide content in amine liquid, and common problems, such as amine liquid foaming and equipment corrosion were investigated. The optimization suggestions for amine liquid systems were put forward, such as integrating amine liquid systems, adding purification facilities, standardizing the operation of the amine liquid, and using new desulfurizes, anti-clogging and foam suppression trays.
    INFLUENCE OF IMPURITY ON C5 RAFFINATE HYDROGENATION AND THERMODYNAMIC ANALYSIS
    2021, 52(8):  37-41. 
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    The 1.2 Mt/a coker gasoline hydrogenation unit of SINOPEC Zhenhai Refining and Chemical Company was reformed to process C5 raffinate with high diene content. The abnormal conditions such as no temperature rise in the pre-hydrogenation reactor (R200) of C5 raffinate and the increase of diene content in the reaction product were analyzed. The initial judgment was that the impurities such as DMF and DEA in the raw material caused the reversible deactivation of the catalyst. The thermodynamics of DMF hydrolysis reaction, the reaction of DEA and hydrogen sulfide were analyzed and verified by experiments. The results showed that the impurities in the reaction system such as DMF and DEA could cause the reversible deactivation of the catalyst. According to the test results, the corresponding measures were put forward to restore the normal operation of the unit.
    STUDY OF AROMATICS CONVERSION RULES IN HYDROTREATED LCO CATALYTIC CRACKING
    2021, 52(8):  42-48. 
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    Based on the commercial result of LTA technology in a refinery of SINOPEC，the conversion rules of the aromatics in hydrotreated LCO（hydro-LCO）catalytic cracking were studied in terms of molecular-based hydrocarbon. The results showed that 73.91% of monocyclic aromatics in products was from cracking reaction of the monocyclic aromatics like alkyl-benzene and naphthenic-benzene in hydro-LCO，and the rest was from the aromatization reactions of non-aromatic compounds including paraffin hydrocarbons and naphthenic hydrocarbons in hydro-LCO in the catalytic cracking process. The contents of dicyclic-aromatics and tricyclic and polycyclic aromatics in products were 37.77% and 18.49%, respectively, and the rests were made up from condensation reactions of monocyclic aromatics and dicyclic aromatics in hydro-LCO. The apparent conversions of alkyl-benzene，hydrocarbons like indane and tetraline and hydrocarbons like indene in catalytic cracking processing were 82.50%，93.80% and 80.72%, respectively. The results can be used to guide the further improvement of LTA technology and proprietary catalyst.
    STUDY OF PYROLYSIS PRODUCTS CHARACTERISTICS OF OIL SHALE KEROGEN
    2021, 52(8):  49-55. 
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    Py-GC-MS, EPR and FITR techniques were used to analyze the structural characteristics of kerogen and its pyrolysis products in Estonia oil shale. The relationship between the intermediate hot asphalt and the end products were studied at different temperatures. The results show that the pyrolysis of oil shale follows the pyrolysis path of kerogen into intermediate hot bitumen, and then bitumen into shale oil, retort gas and semi-coke. The generation trend of intermediate hot asphalt reflects the change of the growth rate of the final product. H2, CH4 and C2-C5 are mainly from the aromatization of aliphatic hydrocarbons in hot asphalt, the breaking of alkyl side chains of aromatic compounds and the condensation of oxygen-containing compounds, etc. The alkanes and olefin compounds produced by kerogen pyrolysis are the main components of oil and gas production. The free radical spin concentration of kerogen and shale oil is lower than that of hot asphalt and semi-coke. The g value of semi-coke is the biggest，that of kerogen takes the second place，and the g value of hot asphalt and shale oil is smallest.
    PERFORMENCE OF Cu-BTC FOR ORGANIC CHLORIDES ADSORPTION FROM MODEL OIL
    2021, 52(8):  56-63. 
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    The copper benzene-1,3,5-tricarboxylate (Cu-BTC) adsorbent was prepared by hydrothermal method and characterized by XRD, SEM, N2 adsorption-desorption and TG techneques. 3-chloro-2-methyl-1-propene(A), 1,4-dichlorobutane(B), 3-chloro-2-methylaniline(C)and 5-chloro-2-methylaniline(D) in simulated oil were removed by static adsorption method. The effects of adsorption time, adsorption temperature, mass ratio of solvent to oil and initial concentration of organic chlorides on the adsorption effect were investigated, and the adsorption conditions were optimized. The results showed that the optimal adsorption conditions were as follows: an adsorption time of 240 min,an adsorption temperature of 303.15 K, a mass ratio of adsorbent to oil equal to 1:40. The Langmuir, Freundlich, Temkin and D-R adsorption isotherms were used to fit the adsorption data, the Langmuir adsorption isotherms was more suitable to describe the adsorption data, and the maximum adsorption capacities for A,B,C and D were 11.90, 5.21, 23.81 and 47.62 mg/g, respectively. The adsorbent has good adsorption selectivity and is easy to adsorb organic chlorides with unsaturation bond.
    THERMODYNAMICS AND KINETICS OF ADSORPTION OF DIMETHYL SULFIDE ON COPPER-LOADED ACTIVATED CARBON
    2021, 52(8):  64-70. 
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    Copper-loaded activated carbon (J-AC) as the adsorbent, dimethyl sulfide in the petroleum ether solution for adsorption, through the specific surface area analyzer for specific surface area and pore structure of the adsorbent were characterized. Thermodynamics and kinetics model was used to analyze the experimental data fitting and the calculation of thermodynamic and kinetic parameters, and J-AC the adsorption mechanism of dimethyl sulfide was discussed. The results showed that the adsorption of dimethyl sulfide by J-AC was in line with the Freundlich isothermal adsorption equation, the fitting correlation coefficient was greater than 0.996, and the adsorption free energy, adsorption heat and adsorption entropy at different temperatures were all less than 0. The adsorption process was a spontaneous process in which the confusion degree of exothermic heat decreased. The adsorption kinetics of the process was in line with the pseudo-second-order kinetic model, and the fitting correlation coefficient was greater than 0.992. With the increase of the initial concentration of dimethyl sulfide, the pseudo-second-order rate constant gradually decreased.
    STUDY OF PREPARATION AND PROPERTIES OF CATALYST FOR ISOMERIZATION OF n-C5/C6 ALKANES
    2021, 52(8):  71-77. 
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    The n-C5/C6 isomerization catalysts were prepared by using the industrialized mordenite molecular sieves. The performance and hydro-isomerization process conditions such as reaction temperature, reaction pressure, liquid hourly space velocity and the ratio of hydrogen to oil for isomerization of n-C5/C6 alkanes over catalyst were investigated in the fixed-bed microreactor. The results showed that the optimum isomerization conditions were as follows: a reaction temperature of 280 ℃, a reaction pressure of 2 MPa, a liquid hourly space velocity of 1.0 h-1, a hydrogen/oil molar ratio of 2.77. Under these conditions, the once through isomerization rates of n-pentane and n-hexane were 67.3% and 85.2%, respectively. The liquid yield was 96%. When the topped oil from commercial reforming unit was used as raw material, the once through isomerization rates of n-pentane and n-hexane were 67.5% and 85.7%, respectively. The selectivity of C6 was 19.9%. The results of 600 h long-period evaluation test using topped oil as raw material showed that the isomerization performance of the catalyst was stable.
    PREPARATION OF Co AND Dy MODIFIED γ-Al2O3 BY COMBUSTION METHOD
    2021, 52(8):  78-82. 
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    Co and Dy modified γ-Al2O3 was successfully prepared by using aluminum nitrate and glycine as raw materials，and cobalt nitrate and dysprosium nitrate as modifiers. XRD，N2 adsorption-desorption and SEM were used to characterize the products. The effects of the molar ratio of the modifier，calcination temperature and calcination time on the morphology of the products were investigated. The results showed that the optimum technological conditions for preparing Co and Dy modified γ-Al2O3 were n(cobalt nitrate)︰n(dysprosium nitrate)︰n(aluminum nitrate)= 0.02:0.01:1，a calcination temperature of 1 000 ℃，a calcination time of 3 h.
    THE ESTABLISHMENT OF SOOT DISPERSION SIMULATIVE METHOD AND STRUCTURE OPTIMIZATION OF ADDITIVES FOR CK-4 DIESEL ENGINE OIL
    2021, 52(8):  83-89. 
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    A new soot dispersion method-diesel engine oil aging-soot dispersion method was established to simulate the Mack T-11 engine test on the basis of the analysis of the Mack T-11 engine test conditions and the soot shape and composition. The influence of different composition ashless dispersant on the dispersion ability of diesel engine oil was investigated by the new dispersion method and molecular simulation technology. The results showed that the new dispersion method could effectively evaluate the soot dispersion performance of the high-grade diesel engine oil. The optimum dispersant was found by the new dispersion method and molecular simulation technology. The engine oil with the optimum additives and base oils passed the Mack T-11 engine test.
    INFLUENCE OF ADDITIVES ON ANTI-OXIDATION PERFORMANCE OF ENGINE OILS BLENDED WITH BIODIESEL
    2021, 52(8):  90-95. 
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    The simulated oxidation test method of engine oils blended with biodiesel was established referring to GFC Lu-43-A-11. Based on the oil formulation that fits the ACEA C3 5W-30 oil sequence, the influence of additives such as antioxidants, ZDDPs, detergents and dispersants, on anti-oxidation performance of engine oils containing biodiesel was studied. The results demonstrated that the additives such as amine antioxidants, secondary alkyl ZDDPs, high TBN detergents, high molecular weight succinimide dispersants showed better anti-oxidation performance of engine oils containing biodiesel.
    SELECTIVE SEPERATION AND RECOVERY OF VANADIUM FROM ACID LEACH SOLUTION OF WASTE FCC CATALYST BY CONTROLLED EQUILIBRIUM TIME OF EXTRACTION
    2021, 52(8):  96-102. 
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    Vanadium was selectively extracted from the Fe-containing acid leaching solution of waste fluid catalytic cracking (FCC) catalyst by controlled equilibrium time of extraction method using 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (P507) as the extraction agent. The test results showed that using the co-extraction system composing of 10% of P507, 5% of tributyl phosphate（TBP）, and 85% of sulfonated kerosene,under the conditions of a saponification rate of extraction agent of 50%, an extraction ratio of 1:1 and an extraction equilibrium time of 10 min, the extraction rate of vanadium reached 99.5% after five-stage countercurrent extraction, and the extraction rate of iron was only 5.2%. Under the conditions of a mass concentration of sulfuric acid of 150 g/L, a reverse extraction ratio of 6:1, and an equilibrium time of 15 min, the mass concentration of vanadium in the reverse extraction solution was 18 630 mg/L, the multistage reverse extraction rate of vanadium was 99.5%, and the mass concentration of iron in the reverse extraction solution was only 70 mg/L. The effective enrichment and recovery of vanadium was realized. Vanadium and iron could be separated effectively and vanadium could be enriched and recovered from sulfuric acid leaching solution of FCC waste catalyst by controlling equilibrium time of extraction method.
    DEVELOPMENT OF GREEN REUSE ENGINEERING TECHNOLOGY FOR MOTHER LIQUOR AND FILTRATE CONTAINING SILICON IN PRODUCTION OF Y MOLECULAR SIEVE
    2021, 52(8):  102-107. 
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    The composition, volume and properties of solid particles of the existing mother liquid and filtrate containing silicon in the production of NaY molecular sieve were analyzed. A rapid solid-liquid separation technology was developed to remove NaY microcrystals and P-type heterocrystals, so as to improve the proportion of silicon reuse. In order to further improve the utilization rate of silicon, the online mixing and full reuse technology of mother liquor and filtrate containing silicon was determined. Through the industrialization of the two technologies, on the premise of ensuring the inner property of NaY molecular sieve, the annual silicon utilization rate was increased to 92.85%, which not only reduced the production cost, but also alleviated the environmental pollution caused by the discharge of silicon waste liquid of molecular sieve.
    SIMULATION AND OPTIMIZATION OF C4/C5 FRACTIONATING COLUMN FOR CONTINUIOUS REFORMING UNIT
    2021, 52(8):  108-114. 
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    Aspen HYSYS software was used to simulate the process of C4/C5 fractionating column (T202) for 1.2 Mt/a continuous reforming unit in SINOPEC Luoyang Company. The ideal model which was close to the actual operation of the device was obtained. The bottom temperature and feed temperature were optimized by the model. The influence of bottom temperature on the vapor pressure of chemical light oil and the effect of feed temperature on the hydraulic operating point of the tray were investigated. The results showed that with the increase of bottom temperature of T202 from 135.5 ℃ to 138.5 ℃，the vapor pressure of chemical light oil at the bottom of the column decreased from 96.71 kPa to 88.76 kPa, and the operating cost was saved by 4.5 million yuan per year as the chemical light oil fractionating column C201 could be discontinued. With the increase of feed temperature to 102 ℃，all plate hydraulics operation points were in the optimum operation area, and the separation accuracy of the column was improved.
    PROGRESS OF PREPARING METHODS OF METAL SUPPORTING MOFs CATALYSTS AND APPLICATION IN CATALYTIC HYDROGENATION
    2021, 52(8):  115-121. 
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    Two preparation methods of MOFs-based catalysts are discussed, namely direct usage of MOFs as the support of metal nanoparticles and deriving into carbon-based nanoparticles from MOFs after being pyrolyzated at high temperature. Compared with traditional supported catalysts, metal nanoparticle catalysts supported by MOFs show a larger specific surface area with a richer pore structure; MOFs-derived carbon-based metal nanoparticle catalysts have adjustable structures and better stability. In addition, the application of MOFs-based catalysts prepared by these methods in hydrogenation has been discussed. The development and application of MOFs-based catalysts are also prospected.
    RESERACH PROGRESS OF AMIDE GREASE
    2021, 52(8):  122-128. 
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    With excellent high temperature stability, oxidation stability, mechanical stability, radiation resistance and long useful life, amide grease was used for lubrication in the fields of aviation, aerospace, nuclear power, and so on. The research progress of amide grease in the world was reviewed, and the influence of the structure of amide thickener on its thickening ability and grease performance was discussed. The synthesis methods of amide thickeners were summarized and compared, including amination of acyl chloride, amination of ester and amination of carboxylic acids. Several efficient and promising amide synthesis methods were introduced for improving the shortcomings of the latter two methods. In general, the method for preparing amide soap-based thickener by the amination of carboxylic acids have the advantages of high availability of raw materials, low cost, simple process and superior product comprehensive performance. It is a competitive synthetic method. Finally, the future development tendency of amide grease is prospected.