Table of Content

12 August 2014, Volume 45 Issue 8

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DEACTIVATION KINETIC MODEL OF VGO HDS CATALYST RN-32V

2014, 45(8):  1-5. 

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A macro kinetic model of VGO hydrodesulfurization was established by VGO HDS test in a pilot plant hydrogenation unit (200mL fixed-bed) using RN-32V catalyst and VGO feed from the Qingdao refining and chemical Co., Sinopec. At the same time, a catalyst deactivation model based on the data of activity changes with operation time was founded. The verification test results show that the deactivation model can well predict the sulfur content of product at different operation time and the life span of catalyst. It is valuable for the operation of hydrogenation unit.

DEVELOPMENT AND COMMERCIAL APPLICATION OF CATALYST RSS-2 WITH HIGH SPACE VELOCITY FOR JET FUEL HYDROGENATION

2014, 45(8):  6-10. 

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On the basis of RSS-1A catalyst in RHSS technology, RSS-2 catalyst is developed through optimizing carrier, active metal, atomic ratio and promoter. The pilot plant test and commercial applications in a 0.80 Mt/a jet fuel hydrogenation unit in Yanshan branch, Sinopec indicate that RSS-2 catalyst has a high activity & a good stability, and is adaptable for different feedstocks. Compared with the first generation catalyst RSS-1A, under the same hydrogen pressure，the space velocity of RSS-2 can increase by 30% with lower reaction temperature and lower H2/oil ratio. The qualities of the product meet the specification of No.3 jet fuel, the same as RSS-1A.

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CHARACTERIZATION OF FCC CATALYST BY POST-PROCESSING TECHNOLOGY

2014, 45(8):  11-16. 

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A FCC catalyst prepared by post-processing technology using NaY molecular sieve as a raw material was characterized by XRD, BET, NH3 TPD, IR and SEM techniques. The results show that compared with a reference catalyst treated by conventional method, the catalyst post-processed has many sunken macroporous structure on the surface, a certain amount of rare earth ions from supercage migrates to sodalite cage, and more rare earth ions exists in the sodalite cage than in the reference catalyst. The post-treated catalyst has a larger surface area and pore volume, stronger acidity, higher heavy oil conversion rate, and micro reaction activity.

DETERMINATION OF SPHERICAL CATALYST STRENGTH FOR POLYPROPYLENE BY ULTRASONICATION

2014, 45(8):  17-21. 

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A method for determining spherical polypropylene catalyst strength by ultrasonication with a laser particle size analyzer is founded. The effect of ultrasonic power, stirring speed, concentration of the solution, the depth of the ultrasonic probe inserted into the solution on catalyst crush was investigated. Moreover，the strength of spherical polypropylene catalyst and their carrier were also measured for comparison. The tests indicate that for GS13L ultrasonic probe, the power tested within the specified range has no effect on the degree of fragmentation. No crushing of the sample was observed without stirring during ultrasonic process. The degree of fragmentation is higher at 200 r.min-1 speed of stirring than that of 400 r.min-1 stirring speed. It is found that the degree of fragmentation decreases with increase of the concentration of the solution. When the depth of the ultrasonic probe inserted into the solution is larger than 20mm, the efficiency of fragmentation will decline. In addition, it shows that the greater the strength of the carrier is, the greater the strength of the catalyst is. The strength of spherical polypropylene catalyst is lower than that of its carrier. The ultrasonication method builds a platform for further study on the relations between the strength and the physicochemical properties of catalyst and carriers.

PREPARATION AND APPLICATION OF HYDROUPGRADING CATALYST FOR INFERIOR DIESEL Part II.PERFORMANCE OF HYDROUPGRADING CATALYST PREPARED BY CO-GELLING

2014, 45(8):  22-27. 

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An unsupported diesel hydroupgrading catalyst was prepared by co-geling and characterized by N2 adsorption-desorption isotherms, XRD, NH3-TPD, Py-IR and SEM. The catalyst was evaluated by two different FCC diesels for the hydrodesulfurization, hydrodenitrogeneration and hydrodearomatization and tested the feed adaptability for high S and aromatics inferior feedstocks. The results show that at a temperature of 360 ℃, for the Qingdao FCC diesel consisting of difficult to be removed DBTs as the main S-containing compounds, the sulfur content can be reduced to 15 μg/g from 7 428 μg/g; for the Shenghua FCC diesel consisting of easily removed BTs as the main S-containing compounds, the sulfur content can be reduced to 14 μg/g from 5 114 μg/g. The catalyst can remove the N-containing compounds completely in the two FCC diesels. Besides, polycyclic aromatic hydrocarbons in the two FCC diesels can be removed by up to 99%.

BRIEF ANALYSIS FOR ATMOSPHERIC AND VACUUM DISTILLATION TECHNOLOGY AT HOME AND ABROAD

2014, 45(8):  28-34. 

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With the development of the atmospheric and vacuum distillation technology, a considerable progresses in process flow, mass and heat transfer, energy-saving and friendly environment are achieved. Three crude distillation units with different capacities at home and abroad are quoted as cases in this paper. The crude properties, product scheme, process flow and operating parameters are introduced in detail, while their equipment selection and engineering expertise are emphasized. The brief analysis is performed on their utility summary and energy consumption. The comparison and analysis conclude that the three sets of distillations have different characteristics. However, the energy consumption（387.3 MJ/t）of the domestic refinery is far lower than the foreign refineries.

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PREPRATION OF ENVIRONMENTAL RUBBER OIL AND CRACKING MATERIAL FROM FCC SLURRYY BY SOLVENT EXTRACTION

2014, 45(8):  35-39. 

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The environmental rubber oil or FCC feedstock were prepared from FCC slurry using furfural as a extract solvent and petroleum ether as a co-solvent. The influence factors of extract temperature, solvent/oil ratio and extraction stages were investigated by crosscurrent extraction and countercurrent extraction process. The results show that the optimum conditions for single-stage extraction were: extraction temperature of 50 ℃ and solvent/oil ratio of 2.5:1. At this condition the extraction effect becomes better with the extraction stage increasing. At three extraction stages, the polycyclic aromatic hydrocarbons (PCA) content of the refined oil obtained from the two processes were both less than 3% and their aromatic carbon rates were above 10%, meeting the EU requirements for environmental rubber oils. At the same time, the density of the refined oil was dropped below 0.9g/cm3 and the saturated hydrocarbon content reaches above 80%, which was considered to be a qualified FCC feedstock. The yield of the refined oil obtained from the multi-stage countercurrent extraction process reaches above 30%, remarkably higher than the yield obtained from the crosscurrent extraction process.

ANALYSIS AND MEASUREMENT FOR ENTRAINMENT OF DRY GAS REABSORBER IN FCCU

2014, 45(8):  40-43. 

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The problem of LCO absorbent entrainment of dry gas reabsorber in FCCU is analyzed. It is thought that relative serious foam system formed in the reabsorber is the reason for the entrainment when the high density FCC LCO is used as an absorbent. After the replacement of FCC LCO absorbent with top cycle oil, the liquid entrainment of dry gas is eliminated and the absorption efficiency is improved greatly. It is suggested to use top cycle oil as absorbent for FCC dry gas reabsorber to eliminate entrainment and improve absorption efficiency.

REASERCH ON MODIFICATION OF FCC CATALYST RESIDUE FOR LUBE OIL FINISHING

2014, 45(8):  44-48. 

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The residue produced during FCC catalyst manufacture process was modified by acids to prepare a lube based oil finishing material. The modification effect of acid type and quantity, temperature, liquid to solid mass ratio, reaction time and stirring rate was investigated. The properties of the samples before and after modification were characterized by means of XRF, FT-IR and the pore structure pattern was also determined by BET method. The results reveal that the pore structure of the treated residue is improved significantly and the number of acid site increases clearly. The modified FCC catalyst residue has a positive effect on lube oil finishing process, can replace clay as a finishing material. In addition, when HCl acid is used as the modifier, the most remarkable result appears at the modification conditions: 95℃, 2h, liquid to solid mass ratio of 2/1, stirring rate of 100r/min and under N2 protection.

IMPACT OF BLENDING FCC SLURRY OIL IN DELAYED COKING AND OPTIMIZATION DESIGN

2014, 45(8):  49-53. 

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Compared with vacuum residue, FCC slurry is low in viscosity, conradson carbon residue, hydrogen and resin content but high in aromatic content and gravity. The influence of blending FCC slurry on delayed coking was analyzed and the design optimization was proposed. The commercial results in a new 1.2 Mt/a delayed coking unit indicate that processing the feed blending with 25% FCC slurry, the coke and gas oil yield increase 2.7% and 2%, respectively， while the light oil (petrol + diesel) and total liquid yield reduce 5% and 3%, respectively. The residue carbon and aromatic content of LCGO, and the coke ash and volatile matter of coke are all increased. The remarkable wears of the heat exchangers, the fractionator, furnace, pumps and pipes and other equipments are observed, which impact the long-term operation. The optimization of the heat exchanger baffles, furnace type, furnace tube thickness, coke cleaning methods and fractionator process can reduce the catalyst deposition on the equipments and retard the coking on the surface of furnace tubes, thus extend the operation life time.

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STUDY OF FACTORS AFFECTING HYDROGENATION ISOMERIZATION DEWAXING REACTION TEMPERATURE

2014, 45(8):  54-57. 

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Huizhou petrochemical company of CNOOC energy development Ltd introduced the hydroisomerization dewaxing technology developed by Chevron Company and invested in the construction of a 400 kt/a hydroisomerization dewaxing unit. The hydrocracking tail oil is used as a raw material. Under the same reaction pressure and hydrogen/oil ratio conditions, the effect of the feed rate and its wax content, and pour point of main product (150N base oil) on the reaction temperature were tested. The results show that in order to achieve the same properties of 150N base oil using the same kind of raw material, the reaction temperature is increased by about 0.5 ℃ for every increase of feed rate 1t/h; and that in the case of stable feeding quantity, reaction temperature needs to increase by about 1.2 ℃ for every 1℃ reduction of pour point of 150 base oil. When the feed rate and the property of base oil 150N remain unchanged, the reaction temperature increases with increasing wax mass faction of the feed.

EFFECT OF RESIDUE DISPERSANT ON COKE FORMATION IN FCC PROCESS AND ITS CHARACTERIZATION METHOD

2014, 45(8):  58-63. 

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The mechanism of coke formation in FCC process was studied. It was concluded that asphaltene, resin and the colloidal system composed of them were the closely impact factors on coke formation. The test results show that adding the right amphiphile with similar structure to resin into the feedstock as residue dispersant can perform better dispersion and reduce the additional coke. Due to some flaws in conventional coke reducing methods, such as ultrasonic method and emulsion method, an optimal multiple scattering method was proposed to characterize the dispersion effect. The stability of the feed using right amphiphile can be increased by 23.5%.

THERMAL HYDROCRACKING PROPERTIES OF ASPHALTENE IN TAHE RESIDUE OIL AND VANADIUM DISTRIBUTION IN PRODUCTS

2014, 45(8):  64-70. 

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Asphaltene in Tahe residue was analyzed by element compositions、IR、1H-NMR and thermogravimetry. The effect of temperature, the ratio of tetralin to asphaltene, initial hydrogen pressure, aromatics and resin on the thermal hydrocracking characteristics of asphaltene and vanadium distribution in products were investigated. It shows that when reaction temperature > 430 ℃, the condensation reaction of macromolecular radicals generated by asphaltene cracking was intensified due to the hydrogen capacity; increasing solvent-oil ratio and initial hydrogen pressure not only promote cracking of asphaltene but also inhibit the condensation reaction. Under the suitable operating conditions (430 ℃, ratio of Tetralin to asphaltene =2 and initial hydrogen pressure 4.0 MPa), the cracking and toluene insoluble rate of asphaltene is 55.69% and 41.69%, respectively. The vanadium in the toluene insoluble is 98.92%. When aromatics and resin account for 50% in the total material, the toluene insoluble reduces 8.32% and 5.55%, respectively for thermal hydrocracking with or without hydrogen donor. The distribution of vanadium in the toluene insoluble decreases less than 5%.

ADSORPTION SEPARATION OF NORMAL PARAFFINS FROM NAPHTHA BY SIMULATED MOVING BED BASED ON MOLECULE-SCALE MANAGEMENT

Jun-Tao JunLIU Liu Ji-chang Benxian Shen

2014, 45(8):  71-76. 

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Based on molecule-scale management, using 5A molecule sieve as adsorbent, a liquid-phase simulated moving bed (SMB) technology was used to separate normal paraffins from naphtha. The rules of separation process and effect of circulation ratio, distribution ratio and desorbent/naphtha flow ratio on the separation performance of SMB were investigated. Under 2.0 MPa, 170 ℃, LHSV of 0.024 h-1 and switching time of 900 s， the optimized operating conditions are：desorbent/naphtha ratio of 4, circulation ratio of 2.25 and distribution ratio of 3.00. For the feed naphtha with the normal paraffin content of 31.95%, the content of normal paraffins in desorption oil reaches 87.76%, and the content of non-normal paraffins in the raffinate is 97.83%. Compared with the naphtha feed, the ethylene yield increases by 13.1 percentage points using the desorption oil as a steam cracking feed; RON and the potential aromatics content of the raffinate increases by 19.2% and by 10.2 percentage points, respectively.

RESEARCH ON CO2 CAPTURE FROM FCC REGENERATION FLUE GAS

2014, 45(8):  77-81. 

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The CO2 capture test was conducted in a flue gas device with 2 m3 / h capacity by chemical absorption. The results show that the suitable process conditions are: absorbent 15%~30%, absorption temperature 60-70℃, desorption temperature 90-120℃, gas-liquid ratio 70-250 and total reflux mode of absorbing liquid. The capture rate of CO2 is 95%, and desorption rate reaches 80% using a new developed absorbent CHA. The absorption rate of the CHA is equivalent to that of ethanolamine (MEA) and the energy consumption and the corrosion to equipment are less than MEA. The rate of corrosion of CHA is only 0.0136mm/a, while the rate of MEA is 0.0325mm/a. The SO2 in flue gas has an import influence on CO2 capture and should be removed in advance.

STUDY ON PRODUCTION OF ULTRA-HIGH VISCOSITY INDEX LUBE BASE OILS

2014, 45(8):  82-86. 

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Lubricating base oils with high viscosity index are the important basic raw materials for production of high-grade internal combustion engine oil. At present a few domestic manufacturers produce them with low output, and No domestic plant produces the ultra-high viscosity index base oils. The preparation of ultra-high viscosity index lube base oils was studied. The results indicate that when oily wax is used as feed, the lube base oils with viscosity index higher than 146, which meet the requirements of UVHVI150, UHVIS150 and UHVIW150, can be produced by combined technology of iso-hydrodewaxing and ketone-benzol dewaxing process.

PERFORMANCE OF OIL SOLUBLE POLYETHER IN TURBINE OIL

2014, 45(8):  87-91. 

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Oil soluble polyether (OSP) has a good oil solubility and unique ether chain structure. Taking OSP as a base oil component of turbine oil is an efficient way to improve the performance of turbine oil. The performance of the oxidation resistance, detergency, and sludge generation trend and demulsification of the turbine oil with OSP was investigated. The test results indicate that with the increase of the OSP in base oil, the viscosity of the turbine oil does not change, but the viscosity index increases and the pour point decreases. The other indicators have no obvious change. It is concluded that OSP and the complex agent F-2 can match well. The turbine oil with OSP has a good oxidation resistance, detergency and demulsibility ability and can inhibit the sludge generation trend.

FACTORS AFFECTING HEAT CAPACITY OF TRANSFORMER OIL

2014, 45(8):  92-96. 

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In this work, several liquid specific heat capacity measuring methods were introduced. The effect of temperature,viscosity,refining depth and hydrocarbon composition on the specific heat capacity of transformer oil were investigated using the measuring methods. It is found that the repeatability of flow calorimetric method（ASTM D2766—1995） with the deviation less than ±2%, is better than that of the differential scanning calorimetry (ASTM E1269-2005) method. The investigation finds that the specific heat capacity of transformer oil increases linearly with increasing temperature in the range of -20—100 ℃. The heat capacity of the oils by traditional solvent refining is hardly affected by refining depth and additives. The test results show that for the oils with the same viscosity but different aromatic contents, the heat capacities are basically the same and that the heat capacities are directly related to alkane content but increases slowly with temperature for the higher alkane content oils. As a result, the heat capacities of the oils with different alkane content are very close at 100℃. While for oils from the same oil sources, refining process and having similar carbon type composition but different boiling range, even the viscosity increases three times, the heat capacity only increases 2.6%，indicating the slightly increase of heat capacity with viscosity..

DEVELOPMENT AND INDUSTRIAL APPLICATION OF RAPID CRUDE OIL EVALUATION SYSTEM BY NIR

2014, 45(8):  97-101. 

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On the basis of existing technology, the secondary development of RIPP`s rapid crude oil evaluation system by near infrared was conducted. A rapid evaluation model was established based on the database of crude oils processed in refineries by combination of crude data library spectrum fitting and identify technique. The secondary developed rapid evaluation system was applied to A, B two refineries to identify and predict the kind and properties of the crude. The results demonstrate that the established evaluation system can identify well the crude oils processed by refineries under the conditions of the perfect database. The density of crude oil, acid value, content of sulfur and carbon residue of the two refineries can be predicted with small deviation from the standard (RMSEP). The repeatability is equal to the standard method.

RAPID DETERMINATION OF HARMFUL ELEMENTS IN MOTOR GASOLINE BY ICP-MS

2014, 45(8):  102-106. 

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The method for determining harmful elements of copper, lead, iron, manganese, sulfur and phosphorus in motor gasoline by inductively coupled plasma mass spectrometry (ICP-MS) was studied. The samples were measured directly after diluted properly. The dynamic reaction pool technology （DRC）was used to eliminate the interference of polyatomic ion. By discussing the effect of the reaction gas flow of methane and oxygen on the back ground equivalent concentration (BEC), the optimum reaction gas flow was ascertained. The detection limits for copper, lead, iron, manganese, sulfur and phosphorus are 0.009, 0.024, 0.024, 0.072, 5.138, 0.557 μg/L, respectively. Precision and accuracy of the method are good enough to meet the requirements of gasoline detection.