Table of Content

12 August 2019, Volume 50 Issue 8

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EFFECT OF COKE DEPOSITION OF CATALYST ON COUNTERCURRENT CONTINUOUS CATALYTIC REFORMING REACTION

2019, 50(8):  1-5. 

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The relations between the inlet temperature of the 4th reactor and its coke content on the catalyst, and the effects of coke on countercurrent CCR reaction were investigated at a 600kt/a countercurrent CCR unit of SINOPEC Jinan Branch Company. The results showed that the inlet temperature of the 4th reactor had a great influence on its coke content and total coke amount of the whole reactor system. The lower inlet temperature of the 4th reactor could reduce the total coke amount of countercurrent CCR; With the increasing of coke content on catalysts, the temperature drop in each reactor reduced, the yield of aromatics and hydrogen apparently decreased, and the conversion of both naphthene and paraffin decreased; and the conversion rates of low carbon number naphthene and C5 ring naphthene decreased more than that of high carbon number and C6 ring naphthene, respectively; the conversion rate of iso-paraffin and low carbon number normal-paraffin decreased greater than that of normal-paraffin and high carbon number normal-paraffin, respectively. The optimization direction of countercurrent continuous reforming technology is to control the overall carbon accumulation level on catalyst, especially to reduce the carbon accumulation on the 4th reactor as far as possible.

ANALYSIS OF NATIONAL STANDARD VI GASOLINE UPGRADING PROCESSES

Wang Wei

2019, 50(8):  6-12. 

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Based on the general refining process and gasoline pool of SINOPEC Wuhan Company，the advantages and disadvantages for upgrading gasoline quality from national standard Ⅴ to national standard Ⅵ were analyzed. The linear program model for gasoline blending was established for quantitative analysis of upgrading gasoline to national standard ⅥA and ⅥB. The sensitivity analysis of alkylate output，benzene content of reformer gasoline，olefin content and vapor pressure of S Zorb gasoline were performed to provide the basis for formulating the emergency plan of gasoline for sale.

SACALING PROBLEMS IN CONTINUOUS CATALYTIC REFORMING UNIT AND SOLUTIONS

2019, 50(8):  13-16. 

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The qualitative and quantitative analysis and IR characterization were conducted for scales in several parts of the continuous catalytic reforming unit. The reason of scaling and its influence on the unit were analyzed. The scale analysis showed that the samples at the top of the pre-hydrogenation reactor composed of corrosion products and coke, while the deposits at the steam turbine were mainly carbon deposition and impurity in steam. Samples contained metals including Fe (69.78%), Ni (19.16%), Cu (4.67%) and Ca (4.18%). Corrosion products and ammonium chloride were the major constituents in the separation tank of reforming products and the outlet tank of membrane separation compressor. After the overhaul of the device, the water injection operation in the pre-hydrogenation reaction section was resumed to remove the ammonium chloride in the system to prevent ammonium salt from separating out and blocking the pipeline. A new liquid-phase dechlorination tank is added, and a set of dechlorinating agent with excellent performance is added to control the chlorine content in the system and slow down the trend of salt deposition.

COMPARISON OF PROCESSES FOR RUBBER EXTENDER OIL DERIVED FROM NAPHTHENIC VGO

2019, 50(8):  17-21. 

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Rubber extender oil(rubber oil) manufactured from naphthenic VGO through different processes were investigated. The results illustrated that VGO high pressure hydrotreating process could directly produce environment-friendly rubber oil with aromatic-carbon ratio(CA) of 12%. The full-hydrogenation (hydrotreating-hydrodewaxing-hydrofinishing) process has strong adaptability to raw materials and could produce clean rubber oils with very low aromatics content. Combination process of hydrodeacidification and furfural extraction could produce environment-friendly rubber oil with CA of about 12%. environment-friendly rubber oil with CA of 21%-27% could be produced by the combined process of hydrotreating and furfural refining, which could adjust the production scheme flexibly according to product demand. The types of products were more abundant and the production adjustment was more flexible when the combined process coupled further with full-hydrogenation process.

CAUSES AND SOLUTIONS OF FOG FORMATION IN NAPHTHENIC RUBBER EXTENDER OIL AT LOW TEMPERATURE

2019, 50(8):  22-26. 

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A specific experiment and analysis were carried out on the phenomenon of fog opacity in naphthenic rubber extender oil at low temperature by PetroChina Karamay Petrochemical Company. The results showed that the formation of mist at low temperature resulted from the trace amount of water in the oil. When the mass fraction of water was 11 μg/g in the rubber oil，the oil could still be kept clearly and brightly at low temperature. Through reforming the stripping section of vacuum column and using air impulse stripping 48 h in the air-drying tank and filter paper filtering before going out factory, the mass fraction of water in the rubber oil was controlled less than 10 μg/g and the problem of rubber oil fogging at low temperature was solved.

RESEARCH ON CATALYST GRADING TECHNOLOGY FOR ULTRA LOW SULFUR DIESEL PRODUCTION

Ge Panzhu Ding Shi Ju Xueyan Xi Yuanbing Li Dadong

2019, 50(8):  27-32. 

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In order to make better use of catalysts in different reaction regions of diesel ultra deep hydrodesulfurization technology（RTS）, in which two reactors in series were adopted，grading schemes for Ni-Mo-W type catalyst with high hydrogenation activity，Co-Mo type catalyst with high direct desulfurization activity，and Ni-W type catalyst with slight hydro-upgrading activity were compared in the pilot plant. The results showed that the effect of graded catalysts system on ultra-deep hydrodesulfurization was comparable to that of Ni-Mo-W catalyst alone. If Ni-Mo-W type catalyst was used in the first reactor and Ni-W type catalyst in the second reactor，the density and polycyclic aromatic hydrocarbon content of the product was effectively reduced. If the first reactor used Ni-Mo-W type and Co-Mo type catalyst in equal volume，and Co-Mo type catalyst was used in the second reactor，the hydrogen consumption could be effectively reduced.

COMMERCIAL APPLICATION OF FCC CATALYST HMIP-1 TO IMPROVE OCTANE NUMBER OF GASOLINE FROM HYDROGENATED VGO

2019, 50(8):  33-37. 

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The commercial application of HMIP-1 FCC catalyst for high RON gasoline using hydrogenated VGO as feed in SINOPEC Tianjin Company was presented. The result showed that the outlet temperate of the first riser reactor increased by 4℃, the gasoline yield increased by 1.4 percent point with RON improvement of 0.6, up to 89.5, while the yield of coke and throughput of the unit was similar to the blank one. HMIP-1 catalyst shows a significant advance in producing high RON FCC gasoline from hydrogenated VGO.

EFFICIENT SHAPE-SELECTIVE OXIDATIVE DESULFURIZATION BY PHOSPHOTUNGSTIC ACID/NANOCRYSTALLINE CATALYST TS-1

2019, 50(8):  38-45. 

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The catalyst (HPW-Nano-TS-1) with phosphotungstic acid (HPW) supported on nanocrystalline TS-1 was synthesized by impregnation method. The results of 31P MAS-NMR, FT-IR and UV-VIS characterization indicated that the preservation of the Keggin structure in HPW-Nano-TS-1 catalysts was confirmed. Catalytic oxidative desulfurization reaction and adsorption desulfurization over synthesized catalysts with model oil consisting of n-octane solution of organic sulfur was investigated. The time for the adsorption of thiophene, benzothiophene and dibenzothiophene over the nanocrystalline TS-1 and HPW-Nano-TS-1 samples gradually increased, and the saturated adsorption amount decreased accordingly. The introduction of HPW enhances the oxidative removal activity of nanocrystalline TS-1 for macromolecular dibenzothiophene. The removal rates of thiophene and dibenzothiophene were 98.5% and 58.0% at 60 °C, respectively. The order of removal of organic sulfide in the three models from easy to difficult is: thiophene > dibenzothiophene > benzothiophene, clearly different in the order of easy removal of benzothiophene from conventional microporous zeolite or polyoxometalate catalysts. It is due to the effects of shape-selectivity, diffusion effect as well as the electron cloud density of nanocrystalline TS-1 zeolite and HPW on the oxidation reaction of organic sulfur molecules.

EFFECT OF MODIFIED ZSM-5 ZEOLITE WITH DIFFERENT METALS ON n-PENTANE AND METHANOL CO-AROMATIZATION

2019, 50(8):  46-51. 

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ZSM-5 molecular sieve were modified with different metals by impregnation method to obtain zeolite catalysts with different metals loads. The catalysts were characterized by XRD, Py-IR techniques. The aromatization performance of the samples in n-pentane and methanol co-aromatization was investigated in a fixed-bed micro-reactor. The results showed that Zn, Ag, Ni, and Cu, modified catalysts improved the aromatic selectivity, among which the Ni and Ag modified catalysts showed the better aromatization effects. With the optimal metal load, the conversions of n-pentane and methanol were 100%; the aromatic selectivity was up to 37.69%. The catalysts modified with Zn, Ag, Ni, and Cu showed the formation of new L acid, decrease of B acid and increase of L acid, which promoted the dehydrogenation reaction, forming more aromatics from olefin intermediates and improving the aromatic selectivity. The content of different aromatic components in the products increased with the modification of different metals

DEVELOPMENT OF AVIATION LUBRICATING OIL 4060

2019, 50(8):  52-57. 

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According to the requirements of piston aeroengine and the problems such as more coke deposits and poor low temperature start-up performance,in use of the synthetic hydrocarbon aviation lubricating oil, a new type of lubricating oil – 4060 aviation lubricating oil was developed to meet the needs of the users. The developed oil had excellent sludge dispersibility, anti-corrosion and anti-oxidation stability, shear stability, excellent lubricating performance and material compatibility. All the performances met GJB 1219A—2009 specification for aircraft reciprocating engine (piston) oil. The production process of the developed oil was investigated, and the stability of batch product was good. The developed oil passed L38 bench test, 300h engine test and 600h engine test, and had successfully completed the aircraft test flight. The test proved that 4060 aviation lubricating oil has very good cold starting performance, and can extend the oil changing period to 4 times of that of before.

TRIBOLOGICAL PROPERTIES OF LUBRICATING OILS CONTAINING TRIETHANOLAMINE BORIC ACID ESTER UNDER ELECTROMAGNETIC FIELD

2019, 50(8):  58-63. 

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Electromagnetic effect generated by friction self on tribological properties of 150SN base oil and lubricating oils containing triethanolamine boric acid ester (TBE) was investigated by four ball tester. The morphologies of the worn surfaces and the chemical states of several typical elements on the worn surface were analyzed by means of scanning electronmicroscope (SEM), X-ray photoelectron spectroscopy (XPS), and energy dispersive spectrometer (EDS). The tribological mechanisms by the physicochemical effects of electromagnetic field were discussed. The results indicated that under electromagnetic field, friction coefficients and wear scar diameters (WSDs) of steel balls lubricated by 150SN mineral oil was higher than those without electromagnetism impact. The WSDs of steel balls lubricated by triethanolamine (TBE)-doped oils under electromagnetic field were all smaller than those under non-magnetic field, but the friction coefficients were higher. It is inferred that a protective coat is formed on the frictional surface due to the effect of electromagnetic field on the interaction of elemental boron and nitrogen in TBE with metal interfaces, resulting in the formation of the film containing element boron and nitrogen through tribochemical reaction and the improvement of the tribological properties of lube oil containing TBE.

EXPERIMENTAL STUDY ON INHIBITING OXIDATIVE COLOR DECAY AT HIGH TEMPERATURE OF AVIATION LUBRICATING OIL

2019, 50(8):  64-68. 

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The self-made high-temperature oxidation experimental device was used to analyze and compare the color decay of oxidized oil at high temperature of domestic and imported aviation lubricants. The mechanism of inhibiting color decay was discussed by GC/MS. The experimental results showed that the antioxidant Tz516 was an important factor influencing the color blackening of the domestic aviation lubricant. The addition of the phenolic antioxidant T501 could effectively inhibited the color blackening of oxidized oil caused by the amine antioxidant Tz516. As the amount of T501 is gradually increased, a large number of T501 antioxidant molecules occupied a "predominant" position in the oxidation system and consumed most of the free radicals, resulting in a decrease in the number of free radicals reacting with the antioxidant Tz516. It is concluded that the competitive mechanism of antioxidants affects the inhibiting color decay process of oils.

PREPARATION AND PROPERTIES OF BARIUM COMPLEX GREASE WITH HIGH DROPPING POINT

2019, 50(8):  69-74. 

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The synthetic methods of complex barium greases with high dropping points were explored. DSC, XRD, FTIR and SEM were used to study the relationship between dropping points and crystalline aggregation of thickeners in complex barium greases. The results revealed that the dropping point of complex barium hydroxystearate greases with sebacic acid was higher than that of barium stearate greases with sebacic acid due to the hydrogen bonds formed between hydroxyl group (-OH) of 12-hydroxystearate and carbonyl group (C=O) of sebacic acid within complex barium hydroxystearate grease thickeners, resulting in the cocrystallization structure created inside the thickeners.

ANALYSIS OF REFINERY SPENT CAUSTIC AND PHENOL OXIDATION BY HYDROGEN PEROXIDE ON TITANIUM SILICALITE MOLECULAR SIEVE

2019, 50(8):  75-78. 

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The content and components of phenols in refinery spent caustic waste were analyzed. The results indicated that refinery spent caustic waste contained phenols with different structures, the amount of phenol accounted for around 60%. The hydrogen peroxide oxidation of phenol indicated that the oxidation effect was poor and the removal of phenols was only 0.5%. With titanium silicalite molecular sieve as catalyst, the effect of oxidation was substantially improved and the removal of phenol reached 94.7% under the best condition. Titanium silicalite molecular sieve displays outstanding catalysis performance.

DEVELOPMENT AND INDUSTRIAL APPLICATION OF TREATMENT TECHNOLOGY FOR SPENT CAUSTIC CONTAINING SULFUR FROM PROPANE DEHYDOGENATION UNIT

2019, 50(8):  79-83. 

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The development and industrial application of a treatment technology for the spent caustic containing sulfur from propane dehydrogenation unit were introduced. The technology consisted of alkalization neutralization-wet air oxidation-acid neutralization. The industrial unit using the technology operated stably. The S2- mass concentration of the effluent of this unit was less than 1 mg/L, and the COD was less than 200 mg/L. Up to now, a number of units have been built adopting the developed treatment technology.

APPLICATION OF CARBOXYMETHYL CHITOSAN / PHYTIC ACID COMPOSITE FILMS FOR METAL IMPURITY ADSORPTION IN TRANSFORMER OIL

2019, 50(8):  84-88. 

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The carboxymethyl chitosan solution and phytic acid solution were mixed by solution blending process and then freeze-dried to prepare the composite films. The structures of the films were characterized by infrared spectroscopy, thermogravimetry analysis and scanning electron microscopy; and the adsorptions of copper, iron, and aluminum impurities in transformer oil were evaluated. The results suggested that the phytic acid did not destroy the porous structure of the composite film, and the films could effectively adsorb metal impurities in transformer oil. When the mass ratio of phytic acid to carboxymethyl chitosan was 0.4, and the adsorption temperature was 70℃, the adsorption efficiency of the porous composite film for copper, iron and aluminum in the transformer oil was 70.51%,68.99% and 87.23%, respectively.

STUDY ON GAS-SOLID FLOW CHARACTERISTICS IN RISER REACTOR WITH DIFFERENT NOZZLE ANGLES

Wang Shengsheng Liu Bingchao Zhu Xiaolin Li Chunyi

2019, 50(8):  89-95. 

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The effect of angles between nozzle and riser in vertical direction on the flow properties was investigated in a large CFB cold simulation test device. The axial and radial distributions of particle concentration，instantaneous particle concentration signal and probability density analysis in three angles cases were investigated. The results showed that in the pre-lift section and the conveying section，no significant difference between the three cases was found，and the difference existed mainly in the vicinity zone above the nozzle; compared with the traditional equal-diameter riser，the solid-holdup of the bed in the variable-diameter riser increased，the particle distribution was more uniform, but the particle concentration gradient reduced，which is beneficial to the mixing and contact of the gas-solid two phases. As the nozzle angle increased，the diffusion velocity of the gas increased over the entire section，the radial distribution was more uniform，the gas-solid separation phenomenon was effectively suppressed，the gas-solid turbulence was more severe，resulting in more effective contact in the variable-diameter riser.

COMPARISON OF PROPERTIES OF C5 and C7 ASPHALTENES FROM DIFFERENT HEAVY OILS

2019, 50(8):  96-102. 

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Asphaltenes were prepared with n-pentane and n-heptane from Middle East vacuum residue (MEVR), Canada oil sand vacuum topped bitumen (VTB), China Liaohe vacuum residue (LHVR), Venezuela atmospheric residue (VAR), and Venezuela vacuum residue (VVR). Those asphaltenes were compared and analyzed by element analysis, GPC, 1H-NMR, 13C-NMR, XRD and SEM techniques. The results showed that C5 asphaltene and C7 asphaltene of five heavy oils have obvious differences in content, molecular structure, average number of structural units, molecular size and microstructure. Aromatic carbon ratio of those asphaltene ranged from 0.47 to 0.54. The C7 asphaltenes of VTB and LHVR were less in aromatic carbon in ordered stacking structure, while more aromatic carbon was in MEVR, VAR and VVR asphaltene structures.

DISCUSSION OF FLOCCULE APPEARENCE IN JET FUEL FREEZING POINT TEST

Li Chenlin Wu Baoping Wen Zedong Tong Jun

2019, 50(8):  103-108. 

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The floccule appeared in the jet fuel of hydrocracking in freeze point test and disappeared when the oil temperature rose. By adjusting the blending ratios of FCC diesel, purchased wax oil and CDU diesel in the raw materials, the aromatic hydrocarbons and n-alkanes components in the raw materials were reduced, the suspended substances were still found in the freezing test, while measures by adjusting the operating conditions, the fractionator effect, the jet fuel distillation range and the other factors affecting the quality of the jet fuel could not eliminate the presence of suspended matter. The laboratory analysis found that no suspension appeared for dried jet fuel. It is the water from air dissolved in the oil that causes the appearance of floc. Therefore, measures must be taken to isolate water when jet fuel is tested at freezing point.

ESTABLISHMENT OF TEST BENCH FOR HIGH TEMPERATURE DEPOSIT AND RING BOND OF GASOLINE ENGINE OIL EVALUATION AND METHOD STUDY

Huang Shengjun Fu Dailiang Wang Long Qu Yue Shi Shengling Yao Xi Ma Jiankai

2019, 50(8):  109-115. 

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According to the Coordinating European Council CEC L-88-02 method，the PSA TU5 engine was used as the test machine to establish an evaluation bench for light load engine oils. The reference oil RL216 and test oil were selected for the evaluation method establishment of high temperature deposits and piston ring bond of gasoline engine oil. The test results showed that the calibration of reference oil met the calibration range of the method. The bench test had a good repeatability and could be used to investigate the motor kinematic viscosity growth of engine oil，piston sediment and piston ring bond，engine oil consumption and other indicators，and to distinguish the high temperature oxidation resistance and cleanness of different engine oils. The experimental results indicated that the content of elements Zn and P in the test oil showed an upward trend，and that the increase of kinematic viscosity expressed some relations with oil consumption. Reducing the base oil evaporation loss of the engine oil was beneficial to passing through the TU5 stand. The establishment of TU5 engine bench can better provide the bench support and evaluation means for the development of high-grade engine oil in China.