Table of Content

12 February 2014, Volume 45 Issue 2

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STUDY ON CONTACT CRACKING OF KUWAIT VACUUM RESIDUE AND ITS NARROW FRACTIONS

2014, 45(2):  1-7. 

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Kuwait vacuum residue is cut to 4 narrow fractions by SFEF and the residue and all the fractions are characterized by NMR and mass spectrum. The experiments of contact thermal cracking reaction of Kuwait residue and its fractions were conducted over inert particle in a laboratory fixed fluidized reactor. The results show that the yields of dry gas, coke and liquid increase linearly with the content of cores containing five or more aromatic rings, fA and (fN+ fP)，respectively. At the same process condition, the value of CH4/C3H6 as the index of cracking severity of feeds rises linearly with the content of cores containing five or more aromatic rings. The heavier the feed is, the lower the selectivity of hydrogen is, while the methane, ethane, propane and butane have the opposite results. The proportion of the hydrogen distributed in dry gas and coke is higher with the feed becoming heavier and meanwhile the proportion is lower in liquid.

STUDY ON AROMATIC BALANCE IN HYDROTREATED DIESEL CATALYTIC CRACKING PROCESS

2014, 45(2):  8-12. 

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The effect of temperature on the aromatic balance in FCC was simulated using hydrotreated diesel as a feed in a laboratory fixed-fluidized bed (FFB) unit. Test results show that the total amount of aromatics in the product increases by about 9%~12%, compared with the hydrotreated diesel feed, at any reaction temperature. The total amount of monocylic aromatics in the product has little changes in the test temperature range, but is lower than that of the feed. With increasing the temperature, the proportion of the monocyclic aromatics in gasoline is getting higher, but is becoming increasingly lower in diesel. The amount of di-aromatics decreases as the temperature increases, however is significantly higher than that of the feedstock. The amount of tricyclic aromatics and coke increases with temperature. A conclusion can be drawn that the main reason for the total aromatic unbalance is the aromatics generated from naphthene through dehydrogenation.

STUDIES ON FOULING OF FLUE GAS TURBINE IN FCCU

2014, 45(2):  13-17. 

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The scaling of flue gas turbine in fluid catalytic cracking unit (FCCU) causes the high failure rate of the turbine. The wear of catalyst particle was confirmed by analyzing the chemical composition of powder, fouling materials and catalyst in the trouble machine in a petrochemical corporation. It is found that the densification of deposited fine powder is a sintering process, proved by measuring the specific surface areas and pore volumes of the fresh catalyst, equilibrium catalysts and powder. It is the powder deposition and subsequent sintering that leads to the failure of the flue gas turbine.ine.

STUDY ON HYDRODYNAMIC AND MASS TRANSFER PERFORMANCE OF LPT-2 TYPE LIQUID DISTRIBUTOR

2014, 45(2):  18-21. 

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The hydrodynamic and mass transfer performance of LPT-2 type single spray head liquid distributor in the air-O2-H2O system was studied by an organic glass tower (ID1000mm) device. Results show that its pressure drop is between 40-120Pa/m, only 15% of the dry packing pressure drop of the high efficiency packing at liquid flow volume between 1.0-5.0m3/h and gas flow volume between 2000-10000m3/h; Its entrainment percent is between 0.2-2.4%, only 24% of that of the GXD type float valve; The HETP of the LPT-2 is between 0.1-0.25.The mass transfer performance is very close to high efficiency packing at the lower liquid flow volume, but about 50% higher than that of the high efficiency packing at the higher liquid flow volume. LPT-2 type liquid distributor can take the place of the high efficiency packing to work for its better hydrodynamic and mass transfer performance.

RESEARCH ON VAPORIZATION RATES OF SLURRY IN RFCC DISENGAGER

2014, 45(2):  22-25. 

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The method to calculate the vaporization rate of slurry was developed by the group contribution method based on the vapor-liquid equilibrium theory and used to predict the vaporization rates of slurry in the industrial RFCC disengager. The effect of oil vapor temperature and partial pressure of slurry on the bubble point, dew point temperature and vaporization rates of slurry were investigated. Results show that at constant slurry partial pressure the vaporization rate ascend with increasing temperature of the oil vapor. Besides, when the temperature is constant, the bubble point and the dew point decline with slurry partial pressure reduction, while the vaporization rates of the slurry go up. According to the least square method, the correlation of the slurry vaporization rates and operation conditions was established for predicting the vaporization rate of the slurry under different operating conditions. It can provide a simple mathematical model to determine the condensate amount in the disengager.

SYNTHESIS OF IONIC LIQUID AND VERIFICATION OF MULTI-STAGE COUNTER CURRENT EXTRACTION DESULFURIZATION BY STRING CLASS EXPERIMENT METHOD

2014, 45(2):  26-30. 

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In this article, the immobilized 1-heptyl-3-methylimidazolium borofluoride ionic liquid was synthesized by two-steps synthesis. The ionic liquid was applied as extracting reagent for oil desulfurization using hydrogen peroxide (30%) as the oxidant. The desulfurization conditions were checked and optimized by changing the ratio of ILs/oil, extraction time, temperature, and rate. Theoretical stages of the multi-stage countercurrent extraction desulfurization of the ionic liquid were also calculated and verified by three sets of parallel string class simulation experiment under the optimized conditions. The results show that the best desulfurization rate of 77% for FCC gasoline was obtained after 60 minutes at V(IL):V(H2O2):V(Oil)=1:1:10, 60℃ and revolution speed of 600 r/min. After the 4 stages counter current extraction, the sulfur content of the feed gasoline decreases to 10 μg/g with the sulfur removal efficiency of 94% and the gasoline recovery of 95%, which shows good perspective for industrial applications.

STUDY ON CHARACTERIZATION OF HEAT-RESISTANT AND SALT-TOLERANT POLYMER PAMA AND PROPERTIES OF ITS SALTING SOLUTION

2014, 45(2):  31-34. 

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A macromonomer 4-Allyl-heptylphenol (AHP) was synthesized. The hydrophobic association acrylamide copolymer (PAMA) was synthesized using acrylamide (AM), AHP and 2-acrylamido-2-methylpropanesulfonic acid (AMPS) by aqueous micelle frees radical copolymerization technique. The macromonomer and copolymer were characterized by 1H-NMR and FT-IR. The effect of AHP dosage, polymer concentration, NaCl concentration and temperature on the viscosity of copolymer solution was tested. The results indicate that the copolymer exhibits good thickening and salt tolerant property by addition of AHP. The apparent viscosity of 1500mg/L PAMA with AHP (mole fraction of 1%) in 20,000mg/L brine solution is up to 178.6mPa.s at 53℃，and the viscosity of 1500mg/L PAMA with AHP (mole fraction of 1%) in 7,000mg/L brine solution is 110.8.6mPa.s at 90℃. PAMA displays a good heat-resistant property.

INVESTIGATION OF CALCULATION METHOD FOR TITANIUM SILICALITE ZEOLITE STRUCTURE

2014, 45(2):  35-40. 

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X-ray diffraction (XRD) technique was used to characterize the titanium silicalite (TS-1) zeolites with various amounts of titanium and the optimal test conditions were obtained by adjusting the instrument parameters. The calculation method for lattice parameters was established by the Rietveld full spectrum fitting technology for the XRD patterns. The calculation results suggest that when the mole fraction of the titanium in the raw material is less than 2.5 %, the lattice parameter of the TS-1 zeolite increases linearly with the titanium content, indicating part of the titanium in the raw materials entering into the framework of the TS-1 zeolite. The lattice parameter is basically unchanged above 2.5 % mole fraction. It can be inferred that the excessive titanium atoms（a part of the 2.5% above）do not enter into the framework of the TS-1 zeolite.

COMMERCIAL APPLICATION OF RL-2 LUBE HYDROTREATING CATALYST

2014, 45(2):  41-45. 

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The commercial application of RL-2 Lube hydrotreating catalyst in SINOPEC Jingmen Company is introduced. The commercial operation demonstrates that the catalyst has excellent reactivity, good selective ring-opening performance and good activity stability. The deactivation rate of the catalyst is only 3.67℃/a. The results of the stable operation for three years indicate that RL-2 catalyst can be used for the production of HVI Ⅱ group No. 10 lube base oil or even higher grade.

FIRST COMMERCIAL APPLICATION OF OLEFIN REMOVAL CATALYST OF ROC-Z1

2014, 45(2):  46-49. 

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A novel olefin removal catalyst (ROC-Z1) is developed by East China University of Science and Technology to replace the acid clay in the adsorption unit for olefin removal. This paper introduces the industrial test and operation of this catalyst in SINOPEC Zhenhai Refining & Chemical Company. The results of the industrial test show that ROC-Z1 can be used in the original process to replace the acid clay without changing any operation condition. The activity and stability of ROC-Z1 is much better than those of commercial clay used, the lifetime of ROC-Z1 is 4 times of that of the clay. The performance of ROC-Z1and its capability to reduce the solid waste of the process is so excellent that the industrial application prospect is good.

STUDY ON TREATMENT OF REVERSE OSMOSIS CONCENTRATE WATER BY Co/MCM-41 STRENGTHENING ZERO-VALENT IRON/OXYGEN SYSTEM

2014, 45(2):  50-54. 

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A Co/MCM-41 was prepared by calcination of MCM-41 mesoporous zeolite impregnated with cobalt nitrate to strengthen zero-valent iron/oxygen system for removing organic matters in reverse osmosis concentrate water. The reaction conditions including reaction time and temperature, initial pH of the water, iron dosage and Co/MCM-41 dosage were investigated to examine the removal rate of COD and UV254. The orthogonal experiment results show that the removal rate of COD is up to 54 % under the conditions of 0.5 h, 20 ℃, initial water pH of 5, 5g iron and 3 g Co/MCM-41. The reaction time is the most important factor affecting COD removal. Besides, the removal rate of UV254 reaches 50.7 % under the conditions of 1.5 h, 20 ℃ and initial water pH of 3, 5 g iron and 4 g Co/MCM-41. The initial pH of the water to deal with is proved to be the most important factor affecting UV254 removal. Compared with the results of wastewater treated by iron scraps singly, it can be concluded that the presence of Co/MCM-41 plays an important role in strengthening the ability of zero-valent iron/oxygen system to degrade pollutants in the wastewater.

INFLUENCE OF CRASTALLIZATION CONDITIONS ON CATALYTIC PERFORMANCE DURING VANADYL PYROPHOSPHATE CATALYSTS PREPARATION

2014, 45(2):  55-59. 

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By changing crystallization conditions of stirring speed and adding different amount of dispersants (PEG) during catalyst preparation, a series of vanadyl pyrophosphate catalysts were prepared and characterized by XRD, BET and chemical titration to study the effect of crystal structure and micro-morphology on catalytic performance. Experimental results show that stirring speed and dispersant dosage have properly effect both on crystal structure and micro-structure, and the former has a great influence on the average oxidation state of vanadium as well. Appropriate choice of stirring speed and amount of PEG are helpful to achieve a high catalytic performance. Catalytic evaluation results show that at the synthesis conditions of stirring speed 225 r/min, PEG dosage PEG/V2O5=0.10, the n-butane conversion rate of the catalyst is 88 %, selectivity of maleic anhydride is up to 70 % with the yield of 61.7 %.

INFLUENCE OF CRYSTAL SIZE OF BETA ZEOLITE ON PERFORMANCE OF HYDROUPGRADING CATALYST

2014, 45(2):  60-63. 

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Beta zeolite is commonly used as an active component in catalyst. The effect of crystal size of Beta zeolite on the hydroupgrading catalyst performance for FCC LCO was studied. Three Ni-Mo catalysts supported on mixture of Al2O3 and Beta zeolites with different crystal size were prepared by impregnation. The catalysts were characterized by XRD and BET methods and evaluated in a micro-reactor using tetralin as a model compound for selective ring opening performance. And a 100mL hydrogenation unit was used for the catalytic performance test using FCC LCO as feedstock. It is found that the catalyst made from smaller crystal size Beta zeolite has higher external surface area and more hydrogenation activity sites, resulting in higher tetralin conversion and better hydroupgrading performance for FCC LCO.

COMMERCIAL APPLICATION OF LOW Pt CONTENT CATALYST FOR C8 AROMATICS ISOMERIZATION

2014, 45(2):  64-67. 

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Low Pt content SKI-110 catalyst，an ethylbenzene dealkylation C8 aromatics isomerization catalyst，developed by Research Institute of Petroleum Processing has been applied in a large integrated complex. The performance test results show that low Pt content SKI-110 catalyst exhibits good catalytic performance，the isomerization activity of para-xylene reaches 23.04%，the conversion of ethylbenzene reaches 70.40% and the xylene yield is up to 98.00%. Lower production cost for para-xylene and less energy consumption of the unit are achieved.

ANALYSIS OF START-UP AND OPERATION OF 2.0 Mt/a HYDROCRACKING UNIT WITH FULL CYCLE MODE

2014, 45(2):  68-73. 

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To upgrade the diesel, a new hydrocracking unit with 2.0 Mt/a capacity was built in Sinopec Qingdao Refining ＆ Chemical Company. The caliberation for the start-up operation indicate the good performance of the catalyst system of FF36/3963/FC32, under the conditions of 367℃in refining stage, cracking temperature of 381℃ with full recycle mode，the sulfur removal rate is 99.35% with the light fraction yield of 94.30%. In the normal production, the jet fuel yield can reach 36.55% by mild refining、more severe cracking conditions and more amount of recycle tail oil.

INFLUENCING FACTORS OF LONG CYCLE FOR PRODUCTION OF LOW SULFUR GASOLINE IN S ZORB AND COUNTERMEASURES

2014, 45(2):  74-78. 

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By adjusting operation parameters，Shanghai VI gasoline, equivalent to Euro V gasoline (S is less than 10 μg/g) could be produced in Gaoqiao S Zorb unit. This paper analyzes the factors influencing the long cycle for production of low sulfur gasoline, including feedstock properties and fluctuations, cycle fluency of adsorbent, valve equipment failure rate and filter life. Some countermeasures are proposed.

DETERMINATION OF C1-C4 ALCOHOLS IN MOTOR GASOLINE BY GC-MS METHOD

2014, 45(2):  79-83. 

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C1-C4 alcohols have been used as additives to produce unleaded gasoline. However, the contents of them should be controlled strictly. Gas chromatograph-mass spectrometry (GC-MS) method for determination of C1-C4 alcohols in motor gasoline was proposed. The qualitative analysis was conducted by full scan, and each peak was identified by mass spectra of the standard substances and GC retention time. The quantitative analysis was carried out by selected ion monitoring (SIM) scan, which can reduce the interference of the matrix efficiently. The internal standard was introduced to improve the stability of detection. The results exhibit that the GC-MS method has a good linear response to C1-C4 in the mass fraction range of 0.1% to 9.0% (R2≥0.995). The recoveries of standard additions are in the range of 91.47%-104.56% and the relative standard deviations are less than 2.3%. The good accuracy and repeatability make this method available for rapid and accurate determination of C1-C4 alcohols in motor gasoline.

INVESTIGATION ON IRREVERSIBLE ADSORPTION OF LIGHT HYDROCARBON COMPONENTS ON Al2O3 CAPILLARY COLUMN

2014, 45(2):  84-89. 

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C1~C4 light hydrocarbons can be well separated by Al2O3 capillary column according to the difference of adsorption-desorption ability. It is recognized that there are irreversible adsorption for some light hydrocarbons in some extent, influencing the accuracy of Al2O3 capillary column analysis results. The irreversible adsorption of light hydrocarbon components on different type of Al2O3 capillary column was studied. Several column operation conditions, such as column temperature, carrier gas flow rate and sampling amount, were investigated quantitatively. The results show that the irreversible adsorption is obvious mainly for alkadienes and alkynes, especially for propadiene, 1,2- butadiene and propyne on S and M type Al2O3 capillary columns. The column temperature and carrier gas flow rate have a remarkable effect on the irreversible adsorption and the sampling amounts have no influence on it. The experimental correction factors detected are higher than that of theoretical correction factors for some alkadienes and alkynes because of the irreversible adsorption, so the accuracy of quantitative results can be ensured only by calibration area normalization method.

DETERMINATION OF HEAVY METAL CONTENT IN CRUDE OIL SAMPLE BY DRY ASHING-ICP-OES

2014, 45(2):  90-94. 

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The heavy metal elements in crude oil samples pretreated by dry ashing were determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The primary parameters of ICP-OES, such as, wavelength for element analysis, radio frequency (RF), atomization pressure, type and concentration of acid solutions were optimized using standard solutions prior to analyze the practical samples. The accuracy and precision of the method were investigated by analyzing the results of crude oil samples. Under the optimum conditions, the recoveries of Fe, Ni, Cu and V determined by this method are 90.3%~108.0%, which is within the scope of standard (90%~110%). The detection limit of the method and the relative standard deviations are lower.

DEVELOPMENT AND SUPPORTIVE POLICY OF EUROPE IN BIO-REFINING TECHNOLOGIES

2014, 45(2):  95-100. 

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The current status of the bio-refining business and relevant supportive policies are introduced. The research and development of the second generation bio-refining technologies and industrial applications are elaborated. Benefit from the biased policies, the bio-refining technologies in Europe are developed in fast pace, some of the technologies have been commercialized. However, the large scale industrialization of the bio-refining process is still in the initial stage. Some energy concerns in Europe also pay close attention to the investment and R&D in the biomass resources. The relevant strategies and plans of the bio-refining business provide valuable references.