Table of Content

12 June 2015, Volume 46 Issue 6

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DEVELOPMENT OF HYDROUPGRADING TECHNOLOGY FOR PRODUCING CLEAN TRANSPORTATION FUEL FROM COAL TAR

2015, 46(6):  1-6. 

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Two-stage hydroupgrading technology was studied in a pilot plant to produce clean transportation fuels from full-range fractions of coal tar. The effect of the process parameters, such as temperature, hydrogen partial pressure, LHSV and H2 to oil ratio, on the properties of hydrotreated oil was investigated. The hydrocracking process for the hydrotreated tail oil was carried out to determine the appropriate conditions. The results indicate that coal tar could be turned into light clean fuels under appropriate hydro-upgrading conditions and the total yield of naphtha and diesel is more than 95％. The sulfur content in the diesel fraction is less than 10?g/g and its cetane number is close to 45. The stability test of hydrotreating catalyst is conducted for more than 2 600 h, and the product properties remain stable. The hydro-upgrading results indicate that this technology realizes the purpose of clean utilization for coal tar and could be used in commercial unit for long-term operation.

EFFECTS OF OPERATING CONDITIONS ON CRAKING REACTION OF DCC LIGHT NAPHTHA FOR PRODUCING LIGHT OLEFINS

2015, 46(6):  7-11. 

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The reaction performance of DCC light naphtha was investigated in a fixed fluidized bed reactor. The operating conditions including reaction temperature, WHSV, water/oil and catalyst/oil ratio, were investigated to selectively obtain light olefin from DCC light naphtha and meanwhile control the formation of methane. The results show that the suitable operating conditions for DCC light naphtha catalytic cracking are 650 ℃, 6 h-1, water/oil of 0.3 and catalyst/oil of 10. The ethylene yield is10.92%, the propylene yield is 27.74%, the butylene yield is 12.97% and total light olefin yield (ethylene + propylene + butylenes) is 51.63% for the DCC light naphtha containing 69.02% olefin under the optimized conditions.

IMPROVING LIGHT OIL YIELD FROM LIAOHE VACCUM RESIDUE USING GROUP TECHNOLOGY

2015, 46(6):  12-16. 

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Liaohe vacuum residue (VR) deep solvent deasphalting test was conducted using n-C5 solvent at the conditions of solvent ratio 4:1 and 160/180 ℃ and . About 50% CCR and 90% asphaltene were removed and enriched in DOA. The group technology composed of deasphalting, catalytic cracking and coking was used to improve the light oil yield. The results indicate that with increasing the solvent deasphalting pressure, the deasphalting oil yields are increased. The total deasphalting oil yield reaches 74.22%, and the asphalt residue yield decreases significantly at 7.0 MPa. After catalytic cracking, the light oil plus LPG yields of light and heavy deasphalting oils are 25.74% and 12.72%, respectively. The light oil yield is about 7.17% by asphalt residue coking. Compared with coking, the total light oil yield of Liaohe VR is increased 4.06 % by using group technology.

HYDROCRACKING TECHNOLOGY AND UNIT DESIGN FOR NAPHTHA PRODUCTION

2015, 46(6):  17-20. 

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Hydrocracking is an important technology for maximizing reforming feedstock naphtha production. The influence factors of the reaction process were studied. The results show that the heavy naphtha yield is increased, but the heavy naphtha selectivity and potential aromatics content are reduced with increasing of conversion degree. While the changes of hydrogen partial pressure within the test range have little impact on those features. The heavy naphtha selectivity and potential aromatics content are improved by cycling the unconverted oil. The yield of heavy naphtha reaches up to 68% by this operation mode. Based on the test results, a 1 500 kt/a hydrocracking unit was built in Taizhou petrochemical Co. where the recycling mode for increasing naphtha and diesel suggested by RIPP was applied. The technology could meet the demands of reforming feedstock and clean diesel.

FLEXIBLE USE OF HYDROCRACKING UNIT TO INCREASE JET FUEL PRODUCTION

2015, 46(6):  21-25. 

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To increase jet fuel production and improve refinery benefit, the WEPEC broadened its hydrocracker feedstocks by processing LCO, CDU 2nd and 3rd cuts. Meantime, operation conditions are optimized according to the feed properties to maximize jet fuel. As the raw material range widening, the unit load and the output of jet fuel is improved significantly. After optimization, the jet fuel yield increases by 4.3%, 5.8% and 0.94% using the blending feed with LCO, CDU 1st and 2nd cut, respectively, compared with design requirement. The practice suggests that increase of jet fuel production can increase the benefit of the hydrocracking unit in the current market situation.

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INDUSTRIAL APPLICATION OF LIGHT NAPHTHA CAUSTIC EXTRACTION PROCESS

2015, 46(6):  26-29. 

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Light FCC naphtha (LCN) caustic extraction technology developed by SINOPEC Research Institute of Petroleum Processing was adopted in Nanyang Wax Fine Chemical Factory of Henan Oilfield. The results of operation more than one year show that the removal of mercaptan from LCN is nearly 100%. The production is stable and the product can meet the requirement of national IV phase gasoline standard. After regeneration and reverse extraction process, the caustic liquor almost no longer contains mercaptan sodium and disulfide, thus long-term effective use of caustic liquor could be realized with zero discharge of caustic liquor residue.

EFFECT OF DEALUMINATION WITH ORGANIC ACID ON PERFORMANCE OF β ZEOLITE IN CYCLOPARAFFIN RING-OPENING

2015, 46(6):  30-35. 

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β zeolite was modified by dealumination with organic acid, and the physicochemical properties of the samples were characterized by XRD, BET, and NH3-TPD，27Al MASNMR，FTIR. Ethyl cyclohexane was used as a model compound to investigate the effect of modification on the performance of β zeolite for cycloparaffin ring-opening reaction. The results show that with increase of the dealumination degree, the crystallinity, specific surface area and acidic amount of the dealuminated β zeolites rise first and then decrease. The conversion，propylene yield and selectivity show the same trend. But little change of ethylene yield is observed. ECH ring-opening reaction reaches the optimal extent at 41.7% dealumination.

REPARATION AND CHARACTERIZATION OF SHELL-TYPE TITANOSILICATE SIEVES

2015, 46(6):  36-40. 

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With organic silicon and titanium, a new shell-type titanosilicate sieve (RTS) was synthesized by two step hydrothermal crystallization method. The physical properties and catalytic oxidation performance of RTS was characterized by various analytic instruments and phenol hydroxylation reaction. The results show that RTS has MFI topological structure, and the Ti species in RTS are mainly on the shell part of particles. The catalytic performance results indicate that RTS gives the same catalytic oxidation activity and benzene diol selectivity as that of TS-1, and the reusable performance is better than that of TS - 1.

DEVELOPMENT OF BIRD’S NEST FORM GUARD CATALYST AND ITS APPLICATION IN HYDROCRACKING UNIT

2015, 46(6):  41-45. 

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A series of bird’s nest form hydrogenation guard catalysts were developed as the feedstocks become worse and heavier in refineries and successfully applied in a commercial hydrocracking unit. The results show that the guard catalysts are characterized by larger capacity for intercepting impurity and depositing scale. The impurities are deposited uniformly in the guard catalyst bed, resulting in extended cycle length.

APPLICATION OF THE THIRD GENERATION RHT SERIES CATALYSTS FOR HYDROTREATING VR WITH HIGH N, LOW S AND HIGH Fe AND Ca CONTENT

2015, 46(6):  46-51. 

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A 1.7Mt/a residue hydrotreating unit of SINOPEC Changling Company, processed the feedstock with high S and low N, and high Fe and Ca content. The feed is difficult to hydrotreating and easy to cause pressure drop. The 2nd cycle of the unit adopted the 3rd generation RHT series catalysts developed by SINOPEC Research Institute of Petroleum Processing with an optimized catalyst grading. The commercial results demonstrate that the cycle life, processing capacity and mixing slag quantity increase obviously by the use of the 3rd generation RHT catalysts, compared with the second generation of RHT series catalyst, meanwhile the carbon residue conversion effect is better.

SYNTHESIS OF POLYTANGSTOZINCIC QUATERNARY AMMONIUM SALTS AND APPLICATION IN CATALYTIC OXIDATION DESULFURIZATION

2015, 46(6):  52-56. 

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Sandwich-type polytangstozincic quaternary ammonium salts Q12[WZn3(H2O)2(ZnW9O34)2](Q=[C18H37(CH3)3N]+, [C16H33(CH3)3N]+, and [C12H25(CH3)3N]+) were successfully synthesized, and the composite catalyst of mixed surfactant and the salts were made and characterized by X-ray diffraction, Fourier transform infrared spectroscopy, thermal gravity analysis, and elemental analysis. Using mixture of dibenzothiphene, a model compound and hydrogen peroxide, an oxidant as test feed, the as-synthesized composite materials were applied to the catalytic oxidative desulfurization of the mixture to evaluate their activity. The results show that the desulfurization rate of dibenzothiphene is enhanced with increasing alkyl chain length of the surfactant. At 60 °C for 2 h, the S removal rate reaches up to 94.4%.

EFFECT OF GLYCOL TREATMENT ON HYDROGENATION PERFORMANCE OF Ni-W/Al2O3 CATALYST

2015, 46(6):  57-62. 

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Ni-W/Al2O3 catalyst was prepared by loading Ni-W metals on Al2O3 support，and Ni-W/Al2O3–AT catalyst was prepared by post-treating the uncalcinated Ni-W/Al2O3 catalyst prepared with glycol solution. The physicochemical properties of the post-treated catalysts were characterized by XRD, H2-TPR, TEM, XPS and UV Raman spectroscopy (LRS). The results show that ethylene glycol not only promotes W species to form octahedral coordinated multi-core poly tungsten acid by improving the distribution of hydroxyl on the Al2O3 support surface, but also increases the dispersion and sulfidation degree of W species on the Ni-W/Al2O3–AT catalyst by weakening the interaction between Al2O3 support and active metals, resulting in more “Ni-W-S” active phase and higher hydrogenation performance of post-treated catalyst. The Ni-W/Al2O3–AT catalyst shows higher HDS, HDN and aromatics saturation performance than that of Ni-W/Al2O3 catalyst for the light coking VGO of Zhoushan petrochemical Co. The sulfur and nitrogen contents can be reduced from 6 850 μg/g and 3 720 μg/g in feed to 10 μg/g and 12 μg/g in product, respectively, the aromatics with ≥2 rings are reduced from 25.8% to 3.2%.

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STUDY ON COPRECIPITATION MECHANISM OF NEW Ni-Mo-W BULK HYDROGENATION CATALYSTS

2015, 46(6):  63-67. 

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The Ni-Mo-W catalyst precursors were prepared by co-precipitation method and then the Ni-Mo-W catalysts were finally obtained by drying, molding, and calcination. The synthesized catalysts were mainly investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XRS), scanning electron microscopy (SEM). The coprecipitation mechanism of nickel nitrate solution, ammonium molybdate, and ammonium tungstate solution was studied. The results show that after the pHs of material Ni(NO3)2?6H2O，(NH4)10W12O41?xH2O，(NH4)6Mo7O?4H2O was adjusted by ammonia water, coprecipitation under appropriate conditions was conducted. The composition of the precipitate is mainly composed of (NH4)Ni2Mo2O8(OH)?H2O and Ni4W6O21(OH)2?4H2O. NiWO4 and NiMoO4 were obtained after calcination of the precipitate. Ni-Mo-W compounds have layered structure. It is found that nickel ion first combines with tungsten acid radical ion, forming layered compound board, and then the molybdate come into the layer, resulting in Ni - Mo - W bulk catalyst precursor.

FORMULATED SOLVENT FOR ORGANOSULFURS REMOVAL FROM LPG IN FIBER FILM CONTACTOR

2015, 46(6):  68-73. 

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The mass transfer areas of the fiber liquid film contactor and the sieve plate tower, and the solubility for organosulfurs of N-methyldiethanolamine (MDEA) and formulated solvents (UDS-I, UDS-II, UDS-III, UDS-IV) were compared. In addition, the influence of operation conditions on the desulfurization performance of the preferred formulated solvent UDS-IV was investigated. The results indicate that the UDS-IV with improved mass transfer area and driving force can increase the remove rate of organic sulfur from LPG in a fiber liquid film contactor. The removal rate of total organosulfur of UDS-IV solvent is approximately 46 % higher than that of MDEA. Meanwhile, the distribution ratios of organosulfurs in UDS-IV solvent-LPG system are found 7-10 times as much as those in MDEA-LPG system. Under optimum operation conditions, UDS-IV solvent can reduce the contents of H2S and total sulfur of the LPG to less than 1 and 240 mg?m-3, respectively, and the removal efficiency for total organosulfur is above 93%. Key Words: liquefied petroleum gas; desulfurization solvent; organosulfur; methyl mercaptan; carbonyl sulfide; fiber liquid film contactor

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NUMERICAL SIMULATION OF GAS FLOW FIELD AROUND DIPLEG -TRICKLE VALVE IN FCC DISENGAGER

2015, 46(6):  74-78. 

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The numerical simulation of the gas flow field around the trickle valve of cyclone in FCC disengager was conducted by CFD software FLUENT6.2, and the erosion cause of trickle valve plate surface was analyzed. The calculation results indicate that the oil gas is entrained into the dipleg through the clearance between the valve plate and the valve port due to the negative pressure of the dipleg. The amount of oil gas increases with increasing the valve plate opening and the negative pressure. The oil gas carries catalyst particles to impact on the valve plate, which is the main reason of the erosion. The upflow of oil gas through the dipleg also reduces the separation efficiency of the cyclone separator.

SYNTHESIS OF TETRAMER MSAZ AND APPLICATION IN VISCOSITY REDUCTION FOR HEAVY CRUDE OIL WITH SURFACTANT

2015, 46(6):  79-83. 

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An oil-soluble tetramer (maleic anhydride - styrene-octadecyl acrylate – acrylamide) viscosity reducer MSAZ was synthetized for Gudong heavy crude in Shengli oilfield with high amount of asphaltene and resin. Ratio of monomers, reaction temperature, reaction time and quantity of initiator were studied to find the best synthesis conditions. The best synthesis conditions are 85 ℃ and reaction time of 6h at the monomer ratio of n (octadecyl acrylate) : n (styrene) : n (maleic anhydride) : n (acrylamide) = 4.25:3:2:0.3. At 50 ℃, viscosity reduction rate could reach to 75.8% with 500ug/g MSAZ dosage. Surfactants such as lauryl sodium sulfate (SDS) were mixed with MSAZ, respectively to enhance viscosity reducing ability. At the test temperature of 50 ℃, viscosity reduction rate reaches to 85.2% using 500 ?g/g MSAZ mixed with 0.7% SDS. Surfactants with acidic functional groups in ends show a higher viscosity reduction rates than those with basic functional groups in ends. Molecular weight and distribution of MSAZ analyzed by GPC are that Mw is 20~30 thousands, Mn is 10~20 thousands and polydispersity index is about 2. The experimental results show that within the polymer intrinsic viscosity η of around 11~12 mL/g, MSAZ gives the best viscosity reduction results.

RESEARCH ON SYNTHESIS OF POUR POINT DEPRESSANT POLYMETHACRYLATE FOR LUBRICATING OIL

2015, 46(6):  84-88. 

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The methacrylate ester - diisooctyl maleate - styrene terpolymer was synthesized through esterification and polymerization using methacrylic acid, high carbon alcohol and maleic acid isooctyl ester and styrene as raw materials, toluene as solvent, and p-toluene sulfonic acid as catalyst. The synthesis conditions and pour point depressing performance of the terpolymer was studied. The results show that the terpolymer, synthesized at the conditions of molar ratio of monomers of 5:1:1, initiator of 0.8% and 105 ℃, 5 h, has the best pour pint depressing performance. The pour point of the 150SN base oil decreases 22 ℃ when the dosage of depressant is 1.0%.

CAUSES OF FOULING AT TOP CIRCULATION OF ATMOSPHERIC COLUMN AND COUNTERMEASURES

2015, 46(6):  89-94. 

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To study the fouling causes of atmospheric column in Tianjin petrochemical company, the composition of the scaling and the properties of materials at the top of atmospheric column were analyzed. Based on the analysis results, technical measures were suggested，such as changing amount of corrosion inhibitor and regulating solution of injection water, adopting the new process and scale dispersant, resulting in improved fouling situation of the atmospheric column. The circulation volume at the top of column meets the design value and no harmful effect is found in down-stream products.

AN ASYNCHRONOUS TIME SLOT-BASED CONTINUOUS TIME FORMULATION FOR SCHEDULING CRUDE OIL OPERATIONS

2015, 46(6):  95-100. 

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Scheduling of crude oil operations is the first step of the refinery operations, which decides the subsequence process management. Based on the information of vessels, berths, terminal storage tanks, pipelines, factory tanks and crude distillation units of the refinery system and the consideration of the actual operation, like terminal tanks of single store, the feed quality requirements for the distillation units, et al, a blended crude transportation scheduling model was established based on asynchronous time characterization. Taking a typical domestic coastal oil refinery as an example, the feasibility of the model and solution efficiency was validated. The proposed model can obtain the optimal scheme in a short time despite the large scale of the model, which ensures the reasonable operations of terminal storage tanks, pipelines, factory tanks, fully shorten the delay shipping date and unloading time, and satisfies the requirements for smooth running of the crude distillation units, and realizes critical operation. The practical values of this scheduling model are worthy of being appreciated.

REQUIREMENTS OF GASOLINE ENGINE TECHNOLOGY FOR FUEL UNDER NEW FUEL CONSUMPTION AND EMISSION LAWS

2015, 46(6):  101-106. 

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The paper expatiated on the evolution of fuel consumption and emission regulations, current status, and the future plans in China. The development and application of gasoline engine and emission technology under new fuel consumption and emission laws were delved. Based on the inspection on several batches of CN Ⅳ and CN Ⅴ gasoline, the change of distillation, aromatics content, and vapor pressure were analyzed after the introduction of the CN Ⅴ gasoline emission standards. The effect of these indicators on gasoline engine and emission post-treatment technology was clarified. The requirements of engine technology for fuel were suggested. The results indicate that after CN Ⅴ gasoline was brought into effect, more problems exist, such as heavy components, high aromatics content, low vapor pressure in winter, resulting in abnormal running with higher fuel consumption and poorer emission if the new engine and emission technology are applied. Therefore, to improve the fuel consumption and emissions, the strict control of fuel indicators and the quality of fuels are necessary.