Table of Content

12 October 2012, Volume 43 Issue 10

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STUDY ON THE RESIDUE HYDROTREATING ACTIVITY OF NiV/Al2O3 CATALYST

2012, 43(10):  1-4. 

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A series of NiV/Al2O3 catalysts with different Ni/(Ni+V) atomic ratios were prepared by pore saturation impregnation method. The catalysts were characterized by Raman spectrometry and H2-TPR technique. The hydrodemetallization (HDM) and hydrodesulfurization (HDS) activities of the prepared NiV/Al2O3 catalysts after sulfidation were assessed using Kuwait atmospheric residue as feed. Results showed that the existence of nickel could promote the agglomeration of vanadium and reduce the interaction between vanadium and alumina support. It can be concluded that a positive synergetic effect of nickel and vanadium existed in catalyst having Ni/(Ni+V) atomic ratio of 0.25, its HDM activity was much higher than those of the other NiV/Al2O3 catalysts, and its HDS activity was also slightly higher.

STUDY ON THE CATALYTIC PERFORMANCE OF Ti-MCM-41 IN FULL RANGE FCC GASOLINE UPGRADING

2012, 43(10):  5-10. 

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A series of mesoporous hydrodesulfurization catalysts were prepared using MCM-41 and Ti-MCM-41 as support respectively, Co and Mo as active components. The prepared catalysts were characterized by XRD, FT-IR, Py-IR, UV-Vis and N2 adsorption. Results indicated that the surface acidity of MCM-41 was slightly increased with Ti species introduced, while the surface area and pore volume were decreased. The effect of Ti species on the hydrodesulfurization (HDS) performance of these catalysts was studied on a fixed-bed reactor system using full range FCC gasoline as feed. Evaluation results showed that the HDS activity of catalyst was improved significantly with Ti species introduced. The framework Ti species could inhibit olefin saturation, while the non-framework Ti species could be helpful to increase HDS activity, moreover, synergistic effect existed between these two types of Ti species, thus the catalyst having Si/Ti mole ratio of 14.1 exhibited the best HDS selectivity.

SYNTHESIS OF NANO-TITANIUM DIOXIDE BY COMBUSTION METHOD RAPIDLY AND ITS PHOTO-CATALYSIS PERFORMANCE

2012, 43(10):  11-15. 

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With titanium trichloride as oxidant, ascorbic acid as reducing agent and incendiary agent, the synthesis of titanium dioxide by combustion method was carried out rapidly and the prepared samples were characterized by FT-IR, XRD, UV-Vis and SEM. Under the optimal titanium trichloride to ascorbic acid molar ratio of 1: 0.6, the prepared cream white nano-titanium dioxide had an average particle size of 28 nm. Using this titanium dioxide as photo-catalytic catalyst, 0.01 g/L methylene blue solution as simulated wastewater, the effect of catalyst dosage, H2O2 amount, system pH value and the rotation speed of centrifuge on the degradation of methylene blue was investigated. Test results showed that the optimum treating conditions were as follows: a catalyst dosage of 3 g/L, H2O2 to methylene blue solution volume ratio of 1:20，system pH value of 9 and centrifuge rotation speed of 2 000 r/min; treating under such conditions for 240 min, the 0.01 g/L methylene blue solution was degraded to colorless.

EFFECT OF SULFIDATION PRESSURE ON THE ACTIVITY OF CoMo/Al2O3 HYDRODESULFURIZATION CATALYST

2012, 43(10):  16-21. 

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A commercial CoMo/Al2O3 hydrodesulfurization (HDS) catalyst was sulfurized in a fixed-bed micro-reactor under various pressures. The sulfurized catalyst samples were characterized by high-resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS), as well as HDS activity evaluation. The TEM results show that the number of stacking layers and the length of MoS2 nano-particles increase with the sulfidation pressure, which is helpful to weaken the interaction of metal-support. The XPS results show that the sulfur content and the sulfidation degree of the sulfurized catalyst increase with the sulfidation pressure, which benefits the improvement of catalyst activity. Moreover, supplemental sulfidation may happen during the HDS reaction due to reaction pressure is higher than sulfidation pressure sometimes, and it is shown from the XPS results of catalysts reacted under 4.0 MPa for 18 h. The evaluation data of catalyst performance agree well with the characterization results, under a reaction temperature of 360 ℃ and a reaction pressure of 4.0 MPa, catalysts exhibit high activities, the maximum HDS rate reaches 99.5%.

PREPARATION AND CHARACTERIZATION OF SOLID SUPERACID SO₄^2-/SnO₂-Ta₂O₅ BY O/W MICROEMULSION METHOD

2012, 43(10):  22-28. 

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A type of solid superacid catalyst SO42-/SnO2-Ta2O5 was prepared by O/W micro-emulsion method in SDBS/ethanol/cyclohexane system, and the physicochemical properties of the prepared solid superacid samples were characterized by XRD, FT-IR and TG-DTA. The catalyst preparation conditions was optimized by orthogonal experiment and the optimum conditions were obtained as follows: a SnCl4 solution concentration of 0.1 mol/L, the mass ratios of SnCl4 solution: SDBS: ethanol: cyclohexane were 500︰1︰0.5︰15, Ta2O5/SnCl4 mass ratio of 0.06, an aging time of 24 h, the concentration of sulphuric acid impregnating solution was 3.0 mol/L and calcination at 550 ℃ for 3 h. The catalytic performance of this SO₄^2-/SnO₂-Ta₂O₅ catalyst prepared under optimum conditions was evaluated using esterification of acetic acid and n-butanol as probe reaction, its esterification rate reached 99.3%. As compared with catalyst prepared in conventional water system, catalyst prepared in SDBS micro-emulsion system exhibited better catalytic activity and stability.

STUDY ON THE EXTRACTION SEPARATION OF SATURATED HYDROCARBONS FROM FCC SLURRY

2012, 43(10):  29-34. 

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Dual-solvent extraction of FCC slurry oil was performed with furfural as main solvent, n-octane as second solvent, the operation conditions, components of raffinate and its cracking performance were investigated. The optimal operation conditions were obtained as follows: extraction temperature in the range of 50～70 ℃; using 1st stage material mass ratios of m(furfural): m(slurry): m(n-octane)=2.0:1.0:1.5, 2nd stage of m(furfural): m(raffinate phase)=0.67:1.00, 3rd stage of m(furfural): m(raffinate phase)=1.20:1.00; the entire process involved 8 extraction steps (1st step as 1st stage, 2nd-4th steps as 2nd stage, 5th-8th steps as 3rd stage) with an additional solvent enrichment step added between the 4th and 5th step. Under such optimal extraction conditions, using FCC slurry oils from Sinopec Jiujiang Petrochemical Company and Sinopec Guangzhou Petrochemical Company as feed respectively, the mass fractions of saturated hydrocarbons in raffinates were 77% and 74%, respectively; the yields of saturated hydrocarbons reached 95.23% and 91.58%, respectively. The separation of saturated hydrocarbons from aromatics was successful, and the raffinate exhibited excellent cracking performance, it could be used as a high quality FCC feedstock.

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RESEARCH ON THE DISTRIBUTIONS OF SULFUR ON ADSORBENT FOR REMOVING SOx AND NOx AFTER CATALYTIC CRACKING REACTIONS

2012, 43(10):  35-39. 

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An investigation was carried out on a fixed-fluidized bed reactor system to study the distributions and forms of sulfur deposited on adsorbent for removing SOx and NOx in flue gas through catalytic cracking, and the catalytic cracking performance of the adsorbent was studied as well. Results show that during catalytic cracking reactions, more than 80% of the sulfur deposited on the adsorbent could be desorbed and distributed into liquid product, cracking gas, pre-fluidized water and atomizing/stripping water with mass fractions of 2.6%, 41.5%, 27.2% and 2.8%, respectively. The sulfur in liquid product is mainly existed as alkyl thiophene, thiophene, mercaptan and thioether; the sulfur in cracking gas is existed as H2S; the sulfur in condensed water is mainly existed as SO42-, SO32-, S, S2O32- and S2-. However, it seems that the presence of adsorbent do not have significant effect on the catalytic cracking of hydrocarbons.

INFLUENCE OF SURFACTANT AND COMMON ION EFFECT ON THE ADSORPTION OF CAPROLACTAM

2012, 43(10):  40-44. 

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The adhesion of caprolactam on the surface of ammonium sulfate crystal was studied by adding various kinds of surfactant and common ion compounds into the mixed system of caprolactam and ammonium sulfate. Test results show that cationic surfactants (DTAB, DTAC, CTAC) and fluorine cationic surfactant can reduce the amount of caprolactam adhered on ammonium sulfate significantly; the addition of Na2SO4, NH4Cl, CTAB and dodecyl betaine made the adsorption of caprolactam become irregular. In an industrial system containing caprolactam, ammonium sulfate and crystallization mother liquid, adding a little of DTAB into the system could effectively reduce the amount of caprolactam adhered on ammonium sulfate particles.

PRELIMINARY STUDY ON THE PYROLYSIS OF OIL SHALE UNDER DIFFERENT MEDIUMS

2012, 43(10):  45-48. 

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The pyrolysis of oil shale from Minhe Basin under three different medium conditions (shale retort, with deionized water and with alkalic saturated potassium chloride solution) was investigated using autoclave simulation device. The formation of shale oil and shale gas in the three-series was analyzed and compared. Test results show that as compared with shale retort, under aqueous medium more shale oil can be produced. With deionized water medium, the average yield of shale oil increases from 83.66 mg/g (shale retort case) to 210.15 mg/g, yet it seems to suppress the formation of shale gas; in alkalic saturated potassium chloride medium, both average yields of shale oil and shale gas go up, the former increases form 83.66 mg/g to 186.16 mg/g and the latter increases from 7.56 mL/g (shale retort case) to 9.08 mL/g.

MECHANISM ANALYSIS OF Ti-MODIFIED ALUMINA SUPPORT

2012, 43(10):  49-54. 

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A series of Ti-modified alumina samples having various TiO2 contents was prepared. The dispersion state of TiO2 on the alumina support was characterized by TEM, XRD and XRF. Furthermore, the effect of TiO2 on the surface hydroxyl groups of alumina support was studied by FT-IR. Results show that Ti species is dispersed on the alumina surface uniformly. The IR absorption peak of alumina at wave number of 3 725 cm-1 is related to weak acidic hydroxyl group bridged with octahedral Al3 + and tetrahedral Al3+, with the loading of TiO2, the H+ of this bridged hydroxyl is substituted by Ti species firstly, followed by substituting H+ of other hydroxyl groups gradually. It can be seen that in wave number range of 1 000—2 000 cm-1 the related medium strong and weak Lewis acid sites of alumina are affected by Ti-modification in certain aspect.

RESEARCH ON THE THERMAL EXPANSION COEFFICIENT OF ELECTRICAL INSULATING OIL

2012, 43(10):  55-59. 

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Thermal expansion coefficients of insulating oils from various crude sources and different brands are studied in laboratory by ASTM D1903 method. Results show that the thermal expansion coefficients of most mineral insulating oils are in the range of 0.000 72 —0.000 80, having the trend of increase with the temperature slightly. For insulating oils from the same crude source and with great different viscosities, the thermal expansion coefficient of the high viscosity oil is smaller, and the low viscosity one is larger. For insulating oils with same viscosity level, the naphthenic base oil exhibits the least thermal expansion coefficient, followed by intermediate base oil and paraffinic base one is the most. For insulating oils from the same crude base, their thermal expansion coefficients decrease with the increase of aromatic contents.

CAUSE ANALYSIS OF HIGH REACTOR PRESSURE DROP IN FCC NAPHTHA HYDRODESULFURIZATION UNIT AND COUNTERMEASURES

2012, 43(10):  60-63. 

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In some OCT-M FCC naphtha hydrodesulfurization units, rapid rise of reactor pressure drop happened frequently, cause analysis was conducted, such as analyzing the compositions of coke sample from the reactor top part and feedstock as well. It is concluded that the accumulation of amorphous coke deposits on the top part of reactor is the main cause of building up high pressure drop, especially when OCT-M unit processing purchased FCC naphtha and/or FCC unit processing high aromatics blending feedstock. To solve the problem, when processing long-stored purchased naphtha, the naphtha should be pretreated by fractionation column of FCC unit to remove impurities, such as gum. Heavy aromatics feed is not suitable to be blended into FCC feedstock, it will increase the gum content and end point of FCC naphtha significantly, blending should be avoided.

COMMERCIAL TRIAL OF SULFUR TRANSFER ADDITIVE FOR REDUCING SULFUR DIOXIDE EMISSIONS IN FCC FLUE GAS

2012, 43(10):  64-68. 

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The commercial trial of a nontoxic sulfur transfer additive SFTS-1 for reducing sulfur dioxide emissions in FCC flue gas developed by China University of Petroleum (East China) was carried out at Petrochemical Plant of Shengli Oilfield Co. Ltd. SINOPEC and it was introduced in this paper. Trial results showed that compared with base case under similar feedstock properties and operation parameters, when said additive occupied 4% of the catalyst inventory and stabilized at this level for 6 d, the SO2 content in regeneration flue gas dropped from 1 300 mg/m3 to 245 mg/m3, keeping a sulfur removal rate of above 80%; then without adding additive for 11 d, the sulfur removal rate still could be remained at 69%. At the same time, no significant negative effect on product distributions and product properties was observed during the trial.

INDUSTRIAL APPLICATION OF STRAIGHT-RUN GASOLINE AND MIXED C₄ FEED NON-HYDROGENATION UPGRADING TECHNOLOGY

2012, 43(10):  69-72. 

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A 100 kt/a straight-run gasoline aromatization unit of Nanchong Refinery was revamped and expanded its capacity to 180 kt/a by adopting the straight-run gasoline and mixed C4 feed non-hydrogenation upgrading technology developed by Research Institute of Petroleum Processing. The data of more than one year operation show that compared with the base case, the product distributions improve, gasoline yield increases significantly, dry gas yield decreases and the energy consumption of the unit is lower, which demonstrates that this technology is better than the previous one. The straight-run gasoline and mixed C4 feed non-hydrogenation upgrading technology is a preferable technology for straight-run gasoline upgrading

RESEARCH ON DECLINING WATER SEPARATION CHARACTERISTICS OF JET FUEL CONTAINING ANTISTATIC AGENT AND COUNTERMEASURE

2012, 43(10):  73-76. 

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The cause of declining water separation characteristics after adding antistatic agent into jet fuel was analyzed and it was found that the existence of some entrained basic nitrogen compounds in feed was the main reason. To solve the problem, two measures were proposed and put into practice: increase the reaction temperature of removing mercaptan by hydrogenation process to 280℃; remain the reaction temperature at 240℃ and add a clay adsorption step. Results show that both measures are effective, by adopting either one the water separation characteristics of jet fuel with antistatic agent can meet the requirement of product quality standard (not less than 70).

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STUDY ON GASSING CHARACTERISTICS OF TRANSFORMER BASE OIL UNDER THERMAL STRESS AT LOW TEMPERATURE

2012, 43(10):  77-81. 

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The changes of the gaseous components dissolved in transformer base oil under thermal stress at low temperature were investigated by gas chromatography method. Test results show that under the conditions of transformer base oils having various aromatic contents and from different crude base, prior and post to vacuum degassing, the contents of dissolved gases in oil are related with the content of dissolved oxygen in oil, storage temperature and storage time directly. Prior to vacuum degassing, the contents of dissolved gases increase with the increase of aromatic content in oil; post to vacuum degassing, the contents of dissolved gases not seem to be had direct relationship neither with aromatic content nor crude base.

SYNTHESIS AND PERFORMANCE EVALUATION OF A MULTIFUNCTIONAL EXTREME PRESSURE ANTIWEAR ADDITIVE FOR GEAR OIL

2012, 43(10):  82-85. 

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A multifunctional extreme pressure antiwear additive (MEAD) for gear oil was synthesized using phosphorus pentoxide, alkyl alcohol and polyisobutene succimide as raw materials. The structure of the additive was determined by FT-IR, its oil solubility, anti-corrosive capability, sludge dispersion and tribology performance were tested by oven oxidation, four-ball and SRV tests, as well as compared with conventional extreme pressure antiwear additive. Test results indicate that MEAD additive holds excellent performance of antirust, sludge dispersion, load bearing, anti-wear and friction reducing stability.

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ENERGY CONSUMPTION ANALYSIS AND OPTIMIZATION OF A REFINING ENTERPRISE

2012, 43(10):  86-91. 

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Based on analyzing the comprehensive energy consumption of Maoming Oil Refinery, using process system integration optimizing approaches，optimizing the transformation, utilization and recovery of industrial energy in the whole plant were carried out. Some optimized solutions and measures for saving energy were proposed and mostly were realized, such as improvements in some main refining units, heat integration among units, proper using low-temperature heat, revamping storage-transportation and steam power system. Successful results were achieved, in 2011, the total crude processing capacity reached 14.5 million tons with processing loss of 0.38% only, the comprehensive energy consumption of the whole plant was reduced to 2 071 MJ/t, in which saving electricity more than 20 million kWh and steam 255 kt.

INFLUENCE OF WATER TREATMENT AGENT ON THE EFFICIENCY OF INTERMITTENT ACTIVATED SLUDGE TREATMENT SYSTEM

2012, 43(10):  92-96. 

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The effect of reaction time, concentration of bactericides (isothiazolone and 1227), corrosion and scale inhibitor (ATMP) on the efficiency of intermittent activated sludge treatment system was investigated by a batch activated sludge reactor. Results showed that the existence of such water treatment agents in simulated wastewater could decrease the COD removal rate, NH3-N removal rate and oxygen consumption rate of the system, as well as inhibit the growth of heterotrophic bacteria. On the whole, the influence of residual water treatment agents on the biochemical treating effect of intermittent activated sludge treatment system was related with the types of chemical agent, its concentration and reaction time.

CHARACTERIZATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN HEAVY GAS OILS BY COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY COUPLED TO TIME-OF-FLIGHT MASS SPECTROMETRY

2012, 43(10):  97-102. 

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Method for characterization of polycyclic aromatic hydrocarbons (PAHs) by comprehensive two-dimensional gas chromatography (GC×GC) coupled with time-of-flight mass spectrometry (TOF MS) was established and applied in the detailed characterization of PAHs in heavy gas oil. Qualitative and semi-quantitative analyses of PAHs and alkyl substituted PAHs were carried out by the proposed method based on retention time, mass spectra and the NIST library of standard substances. Furthermore, the effects of structure and substituted alkyl on the hydrogenation of PAHs were investigated. Results show that the hydro-conversions of various PAHs are varied apparently due to their different structures, different sites and number of alkyl substitution. Owing to the high resolution power and enhanced sensitivity, GC×GC is a powerful tool to characterize target compounds in complex matrixes, and it will play an important role in the characterization of petroleum at molecular level.

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MECHANISM ANALYSIS OF LOW EFFICIENT DEMULSIFICATION OF ZHETYBAI CRUDE AND SELECTION OF OPTIMIZED HIGH EFFICIENT DEMULSIFIER

2012, 43(10):  103-106. 

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During the demulsification and dehydration of Zhetybai crude, poor demulsification effect including high consumption of demulsifier and thick middle layer of emulsion happened, thus cause discussion was carried out based on mechanism analysis. It can be seen that the main reasons of poor demulsification are related to Zhetybai crude having high wax and salt content, the existence of certain mechanical impurities and the demulsifier used onsite was low efficient. To improve the demulsification and dehydration process of Zhetybai crude, a high efficient demulsifier, BKP-62, was developed and compared with the onsite one. Lab test results show that the dehydration performance of BKP-62 demulsifier is much better, besides, from the test results of interfacial tension, BKP-62 exhibits significant higher interfacial activity than that of the onsite one, which indicates that its demulsification and dehydration performance should be much better.