Table of Content

12 December 2012, Volume 43 Issue 12

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STUDY ON THE WASHING PROCESS OF FCC CATALYST TO REDUCE AMMONIA NITROGEN CONTENT IN WASHING WATER

2012, 43(12):  1-4. 

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Factors such as ammonium salt amount, sulfuric acid dosage and washing procedure on the washing of FCC catalyst were studied. Test results showed that washing FCC catalyst under acidic conditions could consume less ammonium salt to reach the similar sodium oxide content of catalyst. An industrial trial was carried out based on this acidic condition washing procedure and the results showed that about 30% of ammonium sulfate can be saved to obtain the same catalyst quality. Moreover, the amount of ammonia nitrogen in the washing water of FCC catalyst was lowered by about 30%, which is a significant improvement in catalyst manufacture, waste treatment and environmental protection.

THE DEVELOPMENT OF RS-1100 DIESEL HYDRODESULFURIZATION CATALYST

2012, 43(12):  5-9. 

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NiMo/Al2O3 catalyst was prepared by impregnation method using alumina support from appropriate pseudo-boehmite. The effect of Ni/(Ni+Mo) atomic ratio on the activity of NiMo/Al2O3 catalyst was investigated and optimized ratio was acquired. The activity of NiMo/Al2O3 catalyst could be further improved by adding optimum amount of phosphorus promoter and chelating agent into the impregnation solution. The characterization of said impregnation solution by Raman spectroscopy and UV-Vis spectrophotometer showed that phosphorus-molybdenum heteropolyanions of [P2Mo5O23]6- existed in the solution, besides, some interactions between chelating agent and Ni2+ cations also happened. By optimizing preparation conditions, RS-1100 hydrodesulfurization catalyst with high activity was developed. The pilot-plant test results show that the activity of RS-1100 catalyst is higher than that of commercial RS-1000 catalyst at ultra-deep hydrodesulfurization stage, whereas, the bulk density of RS-1100 catalyst is lower. Diesel oil meeting European emission standard V can be produced by RS-1100 catalyst under suitable hydrogenation reaction conditions.

APPLICATION OF COMBINED CATALYST SYSTEM IN DIESEL HYDROTREATING UNIT

2012, 43(12):  10-13. 

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This paper briefly introduced ULSD (ultra low sulfur diesel) combined catalyst system and process developed by Fushun Research Institute of Petroleum and Petrochemicals. Test results of pilot plant showed that compared with applying single catalyst，using this combined catalyst system, under the same process conditions, clean diesel oil with much lower sulfur content could be acquired. Commercial cases of this technology, a 3.3 Mt/a diesel hydrotreating unit in Shanghai Petrochemical Company and a 3.0 Mt/a diesel hydrotreating unit in Zhenhai Petrochemical Company, indicated that FHUDS-2/FHUDS-5 combined catalyst system exhibited excellent deep hydrodesulfurization performance, which could provide diesel oil with sulfur content meeting the requirement of GB Ⅳ emission standard under mild process conditions.

SYNTHESIS OF FATTY ACID ESTERS BY ESTERIFICATION OF OLEIC ACID AND METHANOL OVER PHOSPHOMOLYBDENUM HETEROPOLYACID

2012, 43(12):  14-18. 

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Several metal salts of phosphomolybdic acid catalysts were synthesized and characterized by XRD and TGA. The catalytic performance of these prepared catalysts was studied by esterification of oleic acid and methanol reaction, and the effect of catalyst types, calcination temperature, acid/alcohol molar ratio, catalyst dosage, reaction temperature and reaction time on the conversion of oleic acid and methanol esterification was investigated. Test results showed that using SnPMo as catalyst with a dosage of 4% (based on the mass of oleic acid), under acid/alcohol molar ratio of 1:8 and refluxing at (68±1)℃ for 6 h, the conversion of esterification reached 95.4%. Moreover, this catalyst could be easily recovered and reused at least five times. The influence of various alcohols and fatty acids on the esterification was also investigated using SnPMo catalyst under the above reaction conditions. Results showed that the conversion of esterification decreased with the increase of alcohol carbon number, yet the carbon number of fatty acid had less influence on conversion.

INFLUENCE OF STEAM AND AIR ACTIVATION ON THE PHYSICAL PTOPERTY AND CATALYTIC PERFORMANCE OF VPO CATALYSTS

2012, 43(12):  19-22. 

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Vanadium phosphate oxide (VPO) catalyst precursor was activated under the atmosphere of air and steam/air (S/A) mixed gas respectively. The activated catalyst samples were characterized by XRD, XPS and SEM to study their crystal structure and surface property. Results showed that after activation under S/A mixed gas and air, the main crystal phase of the catalyst was (VO)2P2O7 and VOPO4, respectively. The presence of water vapor during activation reduced the average valence state of vanadium (AV)，but increased the P/V atomic ratio of catalyst surface. The catalytic performance of these prepared catalysts was evaluated by selective oxidation of n-butane to maleic anhydride reaction. It was shown that catalyst FVO-1 activated by mixed gas with S/A volume ratio of 1/3, having an AV of 4.198 and P/V atomic ratio of 1.17 exhibited good catalytic performance: its conversion of butane was 87.10% and the selectivity of maleic anhydride reached 72.89%.

EFFECT OF HYDROTHERMAL TREATMENT AND SILYLATION ON THE AROMATIZATION OF STRAIGHT-RUN GASOLINE OVER ZnO/HZSM-5 CATALYST

2012, 43(12):  23-28. 

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Nano-HZSM-5 samples were hydrothermally treated under various temperatures and modified by tetraethoxysilane (TEOS), then a series of Si-ZnO/HZSM-5 catalysts were prepared by stepwise wet impregnation method using zinc nitrate. The effect of hydrothermal treating temperature and silylation on the aromatization of straight-run gasoline over ZnO/HZSM-5 catalyst was investigated. Test results showed that with the increase of hydrothermal treating temperature, the aromatization stability of catalyst increased firstly followed by decrease, which indicated that suitable hydrothermal treating temperature was helpful for catalyst having good activity and stability in the aromatization of straight-run gasoline. Silylation treatment could further improve the aromatization stability of catalyst and reduced the amount of coke deposited on catalyst. However, when the mass fraction of SiO2 on the catalyst was over 12%, a significant decrease of catalyst aromatization performance was observed due to the reduction of catalyst pore size.

RESEARCH ON THE CONVERSION OF THIOPHENE DERIVATIVES UNDER CATALYTIC CRACKING CONDITIONS

2012, 43(12):  29-34. 

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Reaction performances of thiophene, 2-butylthiophene and benzothiophene were investigated by a FFB device under catalytic cracking conditions, and their reaction mechanisms and product sulfur distributions were discussed in detail. Results showed that the conversion of thiophene and benzothiophene were rather low (less than 20%), cracking to H2S was hard to happen in this case, thereby high selectivity of coke and liquid product was observed. As to 2-butylthiophene, it was quite active under catalytic cracking conditions, reactions including dealkylation, cracking of side chain and desulfurization took place mainly; in reaction product, sulfur distributed in gas reached 28%. With zeolite Y catalysts, good linear relationships existed in product yield-conversion, product sulfur distribution-conversion for thiophene species.

STUDY ON THE DEACIDIFICATION OF HIGH ACID VALUE LUBE BASE OIL

2012, 43(12):  35-38. 

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Pillared alkaline Ca-bentonite samples were prepared with organic amine and non-ionic surfactant and they were used as deacidification agent to remove acid from high acid value 650SN and other heavy lube base oil. Factors influencing the acid removal of lube base oil, such as the layer structure and composition of deacidification agent, as well as agent dosage, treating temperature and time were studied. Test results showed that pillared alkaline Ca-bentonite sample prepared with clay/CaO mass ratio of 5/3 exhibited the best acid removal rate; using said sample with a dosage of 1.5% (based on the mass of base oil), treating at 80℃ for 4 h, the acid value of 650SN lube base oil dropped from 0.109 8 mgKOH/g to 0.023 9 mgKOH/g. Compared with conventional alkaline bentonite, pillared alkaline Ca-bentonite possess better deacidification efficiency, less consumption and good adaptability to different lube base oil.

STUDY ON THE AMMONIUM SALT DEPOSITION IN AIR COOLER SYSTEM AND INFLUENCING FACTOR ANALYSIS

2012, 43(12):  39-43. 

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In order to get the oil-gas-water equilibrium system of hydrocracking reaction effluent, a three-phase flash distillation module was established by HYSYS process simulation software combined with mass conservation principle. The impact of sulfur, nitrogen and chlorine contents in feed, amount of water injection and pressure on the deposition temperatures of NH4Cl and NH4HS in air cooler of reaction effluent (REAC) system were analyzed through the flash distillation module calculation. Results showed that the deposition of NH4Cl and NH4HS occurred mainly at the inlet and outlet of REAC system, respectively. The NH4Cl deposition temperature was greatly affected by the chlorine content of feed, thus, strengthening the dechlorination process of crude oil, setting the water injection point above the site of NH4Cl deposition and keeping 25% of liquid water in effluent could effectively reduce the risk of forming NH4Cl deposit. Sulfur content in the system and the amount of water injection were the main causes affecting the deposition temperature of NH4HS, enhancing desulfurization of recycle hydrogen and increase water injection to keep NH4HS deposition temperature below the operation temperature could avoid happening NH4HS deposition significantly.

A NOVEL LOW CORROSIVE COMPLEXING AGENT FOR REMOVING CALCIUM OF CRUDE OIL

2012, 43(12):  44-46. 

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Ammonium salt of nitrilotriacetic acid was prepared and used as complexing agent for removing calcium of crude oil, using crude of the 2nd distillation unit of Karamay Petrochemical Company as feed. Test results showed that this novel complexing agent exhibited good calcium removal effect under mild operation conditions and with less corrosion to equipment. Using said complexing agent with a mass fraction of 50 μg/g, treating and separating water from oil both at 120 ℃, with a crude flow rate of 2 m/s, the calcium mass fraction of the treated crude oil dropped from 7.1 μg/g to less than 3 μg/g.

INFLUENCE OF FEED PROPERTIES ON THE ENERGY CONSUMPTION OF CONTINUOUS CATALYTIC REFORMING

2012, 43(12):  47-49. 

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With REF-SIM kinetics reaction model of continuous catalytic reforming (CCR) and Petro-SIM process simulation software, a new index, R (A/(N+P)), of feed properties associated with unit energy consumption was proposed based on the analysis of reforming reaction process and mathematical regression method. It shows a good correlation between the new feed index R and unit energy consumption, better than that of the conventional feed index, potential aromatic content or aromatization index. Under the same octane requirement of product, the new feed index R can be used as a basic evaluation parameter when benchmarking energy consumption of different CCR units.

PRODUCTION ROUTE OF GASOLINE MEETING NATIONAL EMISSION STANDARD V FOR MOTOR VEHICLES

2012, 43(12):  50-54. 

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In this paper, the production rout of super low sulfur gasoline meeting National Emission Standard V at Sinopec Beijing Yanshan Company is introduced, as well as the technical characteristics and industrial application results of FCC gasoline hydrotreating and adsorption desulfurization processes, current status of producing gasoline meeting the requirements of Beijing local standard are reviewed, finally, some suggestions for extending super low sulfur gasoline production are proposed. On the whole, the configuration of gasoline production units in Yanshan Company is fine having enough super low sulfur blending components for gasoline pool; compared with conventional gasoline hydrotreating process, to reach the same sulfur removal rate of gasoline, adopting S Zorb process shows less octane number loss, lower hydrogen and energy consumption, it can well meet the demand of producing gasoline meeting National Emission Standard V for motor vehicles.

CALCULATION OF FOULING IN HIGH-PRESSURE HEAT EXCHANGER OF A HYDROGENATION UNIT FOR THE WHOLE OPERATION CYCLE AND APPLICATION EFFECT

2012, 43(12):  55-58. 

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With MATLAB software, the fouling of high-pressure heat exchanger in a gas oil hydrogenation unit was calculated throughout 3-year operation. The calculation results showed that the fouling rate of heat exchanger during operation was controllable; at the final stage of operation, the total resistance of scale was 1.2×10-3 (m2?K)/W. Based on the calculation results of fouling rate, the injection of scale inhibitor during operation was gradually reduced from 100 μg/g to 25—35μg/g, so that in this single operation cycle, the cost saving of scale inhibitor reached 11.59 MRMB. Besides, a fouling calculation method of heat exchanger based on ASPEN PLUS software and film coefficient theory was set up and the accuracy of this method was discussed as well.

FLOW STRUCTURE AND GAS-SOLID CONTACT EFFICIENCY IN FCC RISER

2012, 43(12):  59-63. 

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The detail flow structure and gas-solid contact efficiency in FCC riser were studied in a cycled fluidized bed cold model setup. Based on the gas and solid distributions, relative gas-solid contact efficiency (RCE) and cross-sectional average gas-solid contact efficiency (CCE) were defined. Results indicated that non-uniform axial and radial flow structures existed in riser, which were considered to be unfavorable to catalytic cracking reactions; RCE near the wall region of FCC riser was rather high and CCE decreased with the increase of riser height significantly.

AN ANALYSIS OF FACTORS AFFECTING THE HEAT BALANCE OF WASTE HEAT RECOVERY SYSTEM USING WATER AS HEAT MEDIUM

2012, 43(12):  64-67. 

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To keep the heat recovery unit with water as heat medium running steadily, it is essential that the system should be operated in heat balance. A heater of a delayed coking unit using water heat medium system is studied to analyze the factors affecting heat balance, such as water flow rate, fuel consumption, air consumption and temperature of water entering flue gas heat exchanger. Results indicate that the water flow rate, fuel consumption and air consumption are the main factors affecting the heat balance of system; based on the actual heater operation data, selecting suitable value of fuel consumption and air consumption as design basis in system design is important.

APPLICATION OF CATALYST PHYSICAL SEPARATION TECHNOLOGY IN CONTINUOUS CATALYTIC REFORMING UNIT

2012, 43(12):  68-70. 

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Catalyst of CCR unit in Refinery of Lanzhou Petrochemical Company was separated and graded by physical separation technology based on catalyst density. The recovery rate of usable catalyst (coke content less than 5.8%) reached 91.79%, not only some nonporous beads were sorted out, but also catalyst particles could be graded according to the amount of coke deposited on the catalyst. The commercial operation results showed that the reuse of usable catalyst could meet the demand of reaction and regeneration.

AN ANALYSIS OF FACTORS AFFECTING TURBINE OIL QUALITY AND COUNTERMEASURES

2012, 43(12):  71-74. 

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Key factors affecting the quality of turbine oil were analyzed including lube base oil quality, blending process and so on. It was found that the quality of turbine oil was depended on the air release value, anti-emulsion performance and water content of lube base oil. In blending process, the blending temperature should be in the range of (55±5) ℃, the mass fraction of emulsion inhibitor should be in the range of 100—200 μg/g, prior to blending the main additive complex should be diluted by base oil. To ensure qualified turbine oil, it is essential to avoid any miss blending of other oil products in turbine oil during blending process, storage and transfer

SYNTHESIS OF LOW VISCOSITY OIL FROM OLIGOMERIZATION OF MIXED α-OLEFINS CATALYZED BY CF3SO3H

2012, 43(12):  75-77. 

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Poly-alpha-olefins synthetic oil (PAO) was one of the most widely used synthetic lubricants at present. The oligomerization of C6, C10, C12 α-olefins was studied with CF3SO3H as catalyst. The effects of process conditions including catalyst dosage, feed composition, reaction temperature and reaction time, on the PAO yield and the performance of synthetic lubricant were studied. Results showed that under the conditions of catalyst/feed molar ratio of 0.36, reaction temperature of 40 ℃ and reaction time of 3 h, PAO with low viscosity (100 ℃ kinematic viscosity of 4.83 mm2/s), low condensation point (-30℃) and high viscosity index (140) was synthesized with a yield of above 70 %, and its performance well met the requirements of base oil for high quality PAO synthetic lubricants.

PROCESS SIMULATION AND IMPLEMENTATION OF DELAYED COKING UNIT

2012, 43(12):  78-82. 

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A case study of building models concerning delayed coking by using Petro-SIM desktop refining simulation software to optimize delayed coking operation and the whole refinery is introduced. Results show that models set up by Petro-SIM software not only can optimize the operation of single device and combined unit, but also to implement the desktop management of enterprise. In this case using Petro-SIM model to optimize the operation parameters of absorption-stabilization system of delayed coking unit, the C3 content in dry gas could be lowered significantly reducing economic loss; with Petro-SIM whole process simulation model, adjusting the recycle ratio of delayed coking unit from 1.15 to 1.08, the product distributions of whole refinery would be improved, providing an enhanced economic benefit of 8.9 MRMB annually by calculation.

TYPES OF SOLID MATTER IN FCC SLURRY OIL AND RECYCLE STOCK

2012, 43(12):  83-86. 

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Using filtration-burning method to measure the solid matter content in FCC heavy oil, the particle size distribution, chemical composition and structure of the solid matter in slurry oil, recycle oil and VGO were analyzed in detail. Results showed that the main solid matter in slurry oil was catalyst, which particle size was in the range of 0.5—20.0 μm. The compositions of solid matter in recycle oil and VGO were complicated, besides catalyst particle, also some Fe2O3 and Sb2O5. It seemed that Fe2O3 was from the corrosion of equipment and pipeline, Sb2O5 might come from passivating agent used in FCC process, their particle size distributions were rather wide with quite an amount of particles over 100 μm.