Table of Content

12 February 2017, Volume 48 Issue 2

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CLEAN PRODUCTION OF ZSM-5 MOLECULAR SIEVE BY BIPOLAR MEMBRANE ELECTRODIALYSIS

2017, 48(2):  1-5. 

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Sodium removal process of ZSM-5 zeolite was studied by bipolar membrane electrodialysis (EDBM). The results indicate that the zeolite with Na2O content less than 0.1% can be obtained by EDBM, meanwhile Si，Na and part of template agent can be recycled. The EDBM zeolite is equal to the ZSM-5 zeolite by NH4+ exchange method both in physicochemical properties and catalytic performance. The new process is eco-friendly with no ammonia or salty wastewater emission, and the water can be reused.

INTEGRATION PROCESS OF RESIDUE HYDROTREATING AND MIP LIGHT CYCLE OIL

2017, 48(2):  6-11. 

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The impact of the addition of MIP light cycle oil (LCO) into Changling residue on residue hydrotreating was discussed under different operating conditions. The results show that the addition of MIP LCO increases the HDS and HDM rate by 2.37 and 3.14 percentage points respectively. The MIP gas oil yield increases by 8.69 percentage points.

DEVELOPMENT OF FDHC TECHNOLOGY FOR DIESEL MIDDLE-PRESSURE HYDROCRACKING

2017, 48(2):  12-15. 

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To reduce the diesel/gasoline ratio, SINOPEC Fushun Research Institute of Petroleum and Petrochemicals has developed a diesel middle pressure hydrocracking FDHC technology, consisting of hydrocracking and hydrorefining processes. The problems of lower smoke point of jet fuel produced by middle pressure hydrocracking process and the quality reduction of products at the end of running are solved. The optimized catalyst system, feedstocks, and operation conditions make the FDHC technology suitable to process straight-run diesel fraction, meanwhile the high quality jet fuel, feedstocks for catalytic reforming and steam cracking can flexibly be produced. The smoke point of jet fuel produced reaches 28.1 mm, which can be used as 3# jet fuel. The BMCI of unconverted diesel oil is only 9.5, a high quality feed for steam cracking unit.

REVAMPING OF HYDROCRACKING UNIT FOR 5# WHITE OIL PRODUCTION

2017, 48(2):  16-20. 

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The flow diagram of the hydrocracking unit in original design in SINOPEC Maoming Company composed of steam strip followed by fractionation to produce heavy naphtha, jet fuel, diesel, and tail oil. The diesel cut was used as blending component of diesel pool of the plant. As the market changes, the unit was planned to be revamped to maximize the production of jet fuel and 5# industrial grade white oil instead of diesel blending cut. Two solutions were suggested: (?) increasing the temperature of diesel side stripper feed, (ii) adding new side line in fractionation column. The results indicate that the qualified 5# industrial grade white oil can be produced by both solutions but the latter is preferred, by which premium grade 5# white oil can be produced.

STUDY ON SELECTIVE CATALYTIC CRACKING REACTION OF PARAFFINS IN CATALYTIC CRACKING OF STRAIGHT-RUN NAPHTHA

2017, 48(2):  21-28. 

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The low conversion rate of paraffins, 52.58%—77.07%, limits the light olefins yield in straight-run naphtha catalytic cracking (SNCC). Reaction networks of n-octane, 2-methyl heptanes and 2,5-dimethyl hexane as models were established by DFT methods to investigate the initiative ways of ideal chain reaction and reaction direction. It is found that the existing naphthenic hydrocarbon with higher hydrogen donating ability in naphtha is the key reason for limited conversion of paraffins due to the hydride transfer reaction. The addition of IM-5 zeolite with specific microporous structure in catalyst can rationally strengthen the selective catalytic cracking reactions of paraffins in SNCC process.

STUDY ON NO REMOVAL WITH FeIIEDTA/(NH4)2SO3 SOLUTION

2017, 48(2):  29-35. 

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The effects of (NH4)2SO3 concentration, initial FeIIEDTA concentration, gas flow rate, pH, temperature, NO concentration, and oxygen concentration in feed gas on NO removal by FeIIEDTA/ (NH4)2SO3 solution were investigated. The primary and secondary influence factors and the best process conditions were determined by orthogonal test. The results show that the influence order of different parameters on NO absorption is: the initial FeIIEDTA concentration > NO concentration in feed > temperature > oxygen concentration > feed gas flow rate > pH value > (NH4)2SO3 concentration. The optimum conditions for NO removal by FeIIEDTA/(NH4)2SO3 solution is: the initial FeIIEDTA concentration of 0.005 mol/L, NO concentration of 1072 mg/m3, 30 ℃, oxygen concentration of 4%, the gas flow rate of 800 mL/min, pH of 7, (NH4)2SO3 concentration of 0.2 mol/L. The NO removal rate reaches 92.5% and the absorption amount of NO is 3.29 mol /mol under the optimum conditions.

PREPARATION OF DIESEL STORAGE STABILITY ADDITIVES AND ITS EFFECT

2017, 48(2):  36-41. 

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The physiochemical properties and effect on diesel fuel storage stability of additive newly prepared by compound optimization technology were investigated quantitatively. The results show that the new additives have a better comprehensive performance than the similar ones of US army. The worse the storage stability of diesel fuel, the more obvious inhibition effect on existent gum formation is. The new additives can effectively reduce the total insoluble matter, and the total insoluble content decline rate is directly proportional to the severity of diesel quality decay. But the additives prepared have no influence on the acidity and color of the oil tested. The results confirm that the insoluble matter can be used as a quality index for diesel storage stability. It is expected the compound additive can make the diesel storage life span more than 1.6 times.

INVESTIGATION OF LOW TEMPERATURE SOLUBILITY AND PERFORMANCE OF MPTR DEMETALLIZATION AGENT FOR CRUDE OIL

2017, 48(2):  42-46. 

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The solubility of the active matter in MPTR demetallization agent for crude oil in DMF solvent and mixed solvent of DMF and TB at low temperature was investigated. The applicability of demetallization agent solutions with different composition at low temperature was discussed. Experimental results illustrate that the active matter in MPTR can well dissolve in DMF solvent when the MPTR/ DMF mass ratios are 1.05：0.95, 1.06：0.94, 1.07：0.93, and 1.08：0.92 at low temperature. In the dosage range of 120-180 μg/g of MPTR, single solvent TB cannot improve demetallization rate. Among the concentrations of the active matter in the range of 50-54% in solutions without TB, the performance of demetallization agent solutions with 53.5% of active matter is the best, the calcium removal rate reaches the maximum value of 55.8%.

CALCULATION OF COLLOID DIAMETER AND SOLVATION EFFECT OF ASPHALTENE BY INTRINSIC VISCOSITY METHOD——CHARACTERIZATION OF PETROLEUM DISPERSION SYSTEM IN ACTIVE STATE

2017, 48(2):  47-52. 

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To strengthen the effect on vacuum distillation, 0.002% octadecanol was added into Venezuela atmospheric residue oil, resulting in 4.01% more waxy oil yield. The colloid diameter D and solvation factor K of asphaltene were calculated by Einstein law of viscosity and Pals-Rhodes equation based on the measured viscosities of residue oil（asphaltene）-toluene solutions. The results show that the colloid diameter of asphaltene measured by intrinsic viscosity method is the one of adsorption-solvation layer around colloidal nucleus of asphaltene, affected by solvation effect. It is confirmed that the colloidal diameter of asphaltene can be characterized by the viscosities of residue–toluene solution. The trends that the addition of octadecanol reduces the colloidal diameter of asphaltene and solvent effect have a good relationship with the increase of waxy oil yield. The active state of crude oil dispersion system can be predicted based on the colloidal diameter of asphaltene and solvent effect calculated by intrinsic viscosity method.

COKING REACTION OF VACUUM RESIDUE MIXED WITH COKING GAS OILS

2017, 48(2):  53-56. 

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A vacuum reside was chosen as a coking feed. Three narrow cuts: ＜400 ℃(A), 400-430 ℃(B) , and 430—460 ℃(C) of the coking gas oil in the same refinery were used as hydrogen donors. The hydrogen-donating indexes and structure parameters of three narrow fractions were measured. Under the same coking conditions, the product yields of the residue blending with 10% narrow cut respectively were examined and compared with the results of pure residue without narrow cut. The order of hydrogen-donating indexes of three narrow fractions is A＞B＞C. The same order is for liquid yields for residue blending with three cuts. While the yield of liquid product of vacuum residue with cut A is higher than the pure residue.

INFLUENCE OF ADDING SBS ON PERFORMANCE OF ZHONGHAI NO.70 HEAVY DUTY ROAD ASPHALT

2017, 48(2):  57-62. 

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The effects of SBS types on the properties of Zhonghai 7# heavy duty road asphalt were investigated after the SBS modified asphalts were prepared under the same conditions. The results indicate that the modification effect on Zhonghai asphalt depends on the kinds of SBSs. The SBS (1301-1H) can improve the pavement performance of Zhonghai asphalt at high temperature, while the effect of SBS (796) on the low temperature property of Zhonghai asphalt is the best. The SBS（501）is the best in improving the ability to resist temperature sensitivity of asphalt. The compatibility between SBS (796) and Zhonghai asphalt is the best, proved by the test of storage stability at high temperature and fluorescence image analysis. Within the scope of the experimental investigation, the I-D modified asphalt can be obtained using the compound of SBS (501) and SBS (796), all the indexes of the asphalt product can meet the JTG F40-2004 technical requirements.

ELUCIDATION OF MICROSTRUCTURE ON MOS2-TiO2 INTERFACE IN MO/TiO2 CATALYST BY HREM AND CRYSTALLOLOGY

2017, 48(2):  63-67. 

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Nano anatase-TiO2(A-TiO2) support was synthesized by hydrothermal method. Subsequently, Mo/TiO2 catalyst was prepared by impregnation method and sulfided by dry method under H2S/H2（10 %）mixed gas. The microstructure of the sulfided Mo/TiO2 catalyst was observed by HREM. The results indicate that except base-bonding, MoS2 slab is also anchored on (101) facet of TiO2 with edge-bonding through (001) facet of MoS2. The facet angle between (001) MoS2 and (101) A-TiO2 is 66°. This orientation relationship is elucidated by Coincidence Reciprocal Lattice Points (CRLP) theory.

INDUSTRIAL APPLICATION OF SULFIDE TYPE REFORMING PRE-HYDROGENATION CATALYST THFS-I

2017, 48(2):  68-72. 

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The first industrial application of a new high efficient THFS-I sulfide type reforming pre-hydrogenation catalyst developed independently by COONC Tianjin Chemical Research and Design Institute Co.Ltd. in a 800 kt/a reforming pre-hydrogenation unit of CNOOC Zhoushan Petrochemical Co. Ltd. was introduced. The industrial application results show that THFS-I has advantages of good stability and high HDS and HDN activities for pre-hydrotreating of secondary processing naphtha. Compared with FH-40C, the metal components of THFS-I catalyst are in a vulcanized state before activation and there is no need for presulfiding process. Therefore, it is no hydrogen sulfide occurred during the activation process, leading to no hydrogen sulfide corrosion and pollution of environments, and to a more efficient and environmental friendly start-up.

STUDY ON ALKYLATION OF BENZENE WITH METHANOL OVER ZSM-5 AND ZSM-11 ZEOLITES

2017, 48(2):  73-78. 

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Zeolites of ZSM-5, ZSM-11 and hierarchical pore structure ZSM-11 were synthesized via steam-crystallization and characterized by XRD, SEM, NH3-TPD, BET and TG techniques. The results show that synthesized ZSM-5 and ZSM-11 possesses similar BET surface area, micropore volume, crystal size, and acidity. Mesopores were introduced in hierarchical ZSM-11, and the micropores of the ZSM-11 sieve were retained. In the alkylation of benzene with methanol, ZSM-11 showed better activity and stability compared with ZSM-5, owing to the higher diffusion rates of the C7, C8 and other aromatics in ZSM-11 sieve. Hierarchical ZSM-11 performed further improvement in activity in contrast with conventional ZSM-11. At 460°C, 0.20MPa and the WSHV of 3h-1, the benzene conversion reaches 54.3%, and the total selectivity for toluene and xylene is 91.9% with xylene selectivity of 37.9%. Meanwhile, the activity of hierarchical ZSM-11 is stable after 240 h on stream, showing better stability than micropore ZSM-5 sieve.

ISOMERIZATION OF n-PENTANE CATALYZED BY IONIC LIQUIDS [BMIM] Cl-AlCl3

2017, 48(2):  79-83. 

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In order to study the catalytic isomerization performance of ionic liquid, the acidity of synthesized ionic liquid [BMIM]Cl-AlCl3 were characterized by acetonitrile adsorption FT-IR spectra and UV-vis spectra. The effects of AlCl3 mole fraction, types and amount of initiator, reaction temperature and catalyst/oil mass ratio on pentane isomerization were also investigated. The results show that the acidities of ionic liquids are enhanced with the increase of AlCl3 mole fraction. When the AlCl3 mole fraction and 1-chlorobutane volume fraction is 0.70 and 8%, respectively, the conversion of n-pentane and yield of isoparaffin can reach to 88.1% and 74.8%, respectively at the conditions of 120℃ and catalyst/oil mass ratio of 1:1.

STUDY ON PROPERTIES OF CALCIUM ALKYLSALICYLATE WITH DIFFERENT SUBSTITUENT STRUCTURE

2017, 48(2):  84-89. 

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Using olefins with different chain length and salicylic acid as raw materials, calcium salicylates with different alkyl structure were synthesized by alkylation and calcification. The performance differences of the products in high temperature detergency, oxidation resistance, sludge dispersion properties, anti-foam property, anti-emulsification property and colloid stability were investigated. The results show that the change of alkyl carbon number of the calcium alkyl salicylate is the main reason for performance differences. The calcium alkyl salicylates with alkyl carbon number of 12 to 18 possess better high temperature detergent resistance, oxidation resistance, sludge dispersion property and colloid stability. When the alkyl carbon number is 20-22, the calcium alkyl salicylates have better resistance to foaming and anti-emulsifying abilityies.

HYDRODYNAMIC CHARACTERISTICS IN BUBBLE COLUMNS

2017, 48(2):  90-93. 

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The changing rules of gas holdup, Sauter mean diameter (SMD) of bubbles, slip velocity between gas and liquid phases of nitrogen-kerosene system in a cold bubble column with a diameter of 45 mm were investigated. The experimental results show that in the bubble coalescence control region, the average gas holdup increases as the velocity of the gas and liquid phase increases, the SMD of bubbles increases with increasing the gas velocity, but decreases with the increased liquid velocity. Under the same conditions, compared with the results in smaller column, larger reactor has the stronger bubble coalescence effect and larger bubble diameter, while the gas holdup is reduced.

INFLUENCE OF PRE-LIFTING ON GAS-SOLIDS FLOW IN CIRCULATING FLUIDIZED BED

2017, 48(2):  94-100. 

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The effects of operating conditions of superficial gas velocity, system storage capacity, butterfly valve opening, pre-lifting gas volume on solids circulation rate in a cold apparatus of circulating fluidized bed were investigated using air and FCC equilibrium catalyst, and the causes of influence were also analyzed. Meanwhile, this paper conducted a thoroughly comparative study about the impacts of pre-lifting outlet on solid fluxes as well as axial and radial solids concentration distribution inside the bottom section of riser. The micro-flow pattern in the gas-solids confluent zone was proposed. The results show that the solids circulation rate increases with increasing gas velocity and more intensive gas-solids contact. The pressure needed for supporting gas-solids flow in riser is from storage vessel and butterfly valve. Increasing particle reserves and decreasing butterfly valve pressure drop also helps boost solids circulation rate. Injection of pre-lifting gas helps to push solids upwards in case of particle deposits at the bottom. When the solids flux provided by storage vessel is large enough, increasing pre-lifting outlet position could change the gas-solids flow structure in the gas-solids confluent zone by preventing solids downwards and pushing solids upwards. Besides, the different pre-lifting structures have limited influence on solids concentration in either axial or radial distributions in riser.

STUDY ON METAL DETERGENT TURBIDITY MEASUREMENT BY SCATTERED LIGHT TURBIDIMETER

2017, 48(2):  101-106. 

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Turbidimeter HACH2100AN and M-151 were used to investigate the turbidity of metal detergents of calcium alkylbenzene sulfonate, calcium sulfurized phenate, calcium alkyl salicylate and calcium naphthenate. It is found that the turbidity values of detergents change as the concentration of detergent increases in the samples: increasing, decreasing, and having maximum point when HACH2100AN turbidity instrument is used. The most increase of turbidity values occurs when the instrument is in open mode and the sample concentration is 20%，the turbidity measured is close to the real value. In addition, the effect of base oil types and operation temperature of samples on measured turbidity was also explored. The results show that the type of base oil has larger effect on turbidity measured, while the temperature has only little influence. The reliability of HACH2100AN testing method is verified by the colloid sizes data of metal detergent in lube oil.

COMPOSITIONS AND STRUCTURES OF PETROLEUM ACIDS IN FENGCHENG HEAVY CRUDE

2017, 48(2):  107-113. 

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Petroleum acids in Fengcheng heavy crude were separated by potassium hydroxide-ethanol aqueous solution extraction. The compositions and structures of petroleum acids were determined by elemental analysis, IR, NMR, ESI-MS, UV and Fluorescence Spectrum. The results show that the petroleum acid in Fengcheng heavy crude is mainly composed of dimers of mono-carboxylic acids with an average molecular weight of 665, the empirical formula is C43.51H78.47O3.78 with a hydrogen-carbon mole ratio of 1.80. The contents of naphthenic acids and aliphatic acids occupy 79.84% and 20.16%, respectively. The contents of naphthenic acids with different structures (including 1-3 ring naphthenic acids, 4-ring naphthenic acids/aromatic carboxylic acids, 5-ring naphthenic acids/benzonaphthenic carboxylic acids with one ring, 6-ring naphthenic acids/benzonaphthenic carboxylic acids with 2-ring) are close to each other, ranging from 11.00% to 18.88%. Trace amount of 3-4 ring aromatic in petroleum acids are also observed.