Table of Content

12 October 2013, Volume 44 Issue 10

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ADVANCES IN CATALYTIC PROCESSING OF PARAFFIN FOR PROPYLENE PRODUCTION

2013, 44(10):  1-7. 

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Catalytic conversion of paraffin to light alkenes is a new route for maximizing propylene production. Existing problems of steam pyrolysis were summarized. Research advances in catalyst and reaction behavior of catalytic pyrolysis and catalytic oxidation was reviewed, respectively, including discussion on current situations and developing tendency. It seems that in order to enhance alkene yields and further decrease dry gas yield the development of new zeolite catalysts which allow paraffin to crack at lower temperature is the main target of catalytic pyrolysis. In addition, it is essential for commercialization of catalytic oxidation to intensify studies on catalytic mechanism and catalysts with low temperature activity and high selectivity and strengthen the process research at the same time.

STUDY ON ENRICHMENT OF VANADIUM BY HYDRO-UPGRADING OF TAHE ATMOSPHERIC RESIDUE

2013, 44(10):  8-12. 

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THAR with high concentration of vanadium is a kind of heavy oil difficult to be processed. It was found that hydro-upgrading process could concentrate the vanadium in bottom fractions. Based on the properties of THAR, the effect of hydrotreating conditions, such as hydrotreating temperature, initial hydrogen pressure and reaction time, on vanadium distribution in product and light fraction yield were investigated. The results show that vanadium is mainly enriched in residue through hydrotreating, and the higher temperature and longer reaction time were conducive to the enrichment of vanadium, but could make light oil yield decrease. However, no apparent effect of initial hydrogen pressure on distribution of vanadium and light fraction yield is found. The suitable hydro-upgrading conditions are: T = 425 ℃, P H2 =3.0 MPa, and reaction time 45 min. Under these conditions, the distribution ratio of vanadium in the light oil is only 0.44%, but the distribution ratio in the residue is up to 95.57%. The vanadium content in the hydrotreated residue is as high as 1323 μg/g. The yields of the light fraction and residue are 61.29% and 20.32%, respectively.

STUDY ON WEAR CHARACTERISTICS OF ENGINE FUELED WITH BIODIESEL

2013, 44(10):  13-17. 

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Bench tests were conducted for evaluating the wear characteristics of diesel engine fueled with biodiesel and No. 0 petro-diesel, respectively. The wear and morphologies of the engine were analyzed before and after the bench test. The results indicate that the wear extent of moving parts of the engines such as cylinder liner, piston, piston ring, connecting rod, connecting rod bearing, camshaft and fuel injection pump was all in normal range for the two diesels, but the wear of biodiesel engine is slightly less than that of petro-diesel engine. SEM analysis of the cylinder liner and piston ring also shows that the anti-wear performance of biodiesel is better than that of petro-diesel because of higher viscosity and better lubricity of biodiesel which more easily form a film on the cylinder wall.

INFLUENCE OF ULTRASONIC PRETREATMENT ON ASPHALTENE STRUCTURE BEFORE AND AFTER HYDROTREATING

2013, 44(10):  18-22. 

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The effect of ultrasonic pre-treatment, followed by hydrotreating, on the status of association and structure of asphaltene was examined. The results indicate that ultrasonic treatment can change the asphaltene structure, but not the content of chemical elements. The structure changes caused by ultrasonic pre-treatment include the reduction of association number and increase of the branching degree through opening the naphthenic ring of asphaltene. Ultrasonic treatment reduces the molecular weight and the structure parameters of asphaltene, such as RT, RA, RN, CA and Dy. The distribution and types of hydrogen atoms are also changed. The molecular weight and parameters of fA, CAP, n, RT, RA, CA, Dy, BI of hydrotreated asphaltene increases because the occurrence of bridge bond rupture, dealkylation and condensation during the residue hydrotreating, while σ, H/C, nsw and X/n are decreased. These changes in structure and reactivity of asphaltene are helpful to residue hydrotreament. The functions of ultrasonic pretreatment are reinforced by hydrotreating. The structure of hydrotreated asphaltene was more complicated and the associating number of molecule even reaches 7 to 11.

HYDROGEN PRODUCTION FROM METHANOL STEAM REFORMING OVER CuZnAl CATALYSTS

2013, 44(10):  23-27. 

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A series of CuZn and CuZnAl catalysts were prepared by co-precipitation method. The catalytic performance of these catalysts for methanol steam reforming was investigated. The catalysts were characterized by BET, XRD, H2-TPR and N2O chemisorptions to explore the effect of the introduction of Al into CuZn catalyst. The results show that with the moderate ratio of Cu/Zn, the addition of Al can enlarge the specific surface area of CuZn catalyst and promote the dispersion and stability of Cu species on the catalyst surface and that the Cu50Zn40Al10 catalyst exhibits the highest catalytic activity for methanol steam reforming in the tested CuZnAl catalysts. The methanol conversion reaches 100% and the hydrogen yield is up to 97.7% under the reaction conditions: T=250 oC and P=1.0 MPa, H2O/CH3OH=1.5 molar ratio, VHSV=0.56 h-1. The Cu50Zn40Al10 catalyst has the excellent catalytic stability for methanol steam reforming during 200 h on stream and the methanol conversion has been kept at around 97%, much better than that of Cu50Zn40.

STUDY ON CETANE NUMBER IMPROVEMENT OF LCO BY HYDROTREATING

2013, 44(10):  28-32. 

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The improvement of cetane number (CN) was studied over Ni-Mo-W catalyst in the light cycle oil (LCO) hydro-upgrading processing in pilot plant. The effect of the processing parameters on improving cetane number of LCO was investigated. The results indicate that 7-13 cetane number increment is observed under 6.4 MPa and other suitable operation conditions. The main factor influencing the increment of cetane number of LCO is the aromatics saturation reactions. Other operation parameters, such as temperature, LHSV and H2 to oil ratio have also a significant influence. The suitable reaction conditions are helpful to increase CN of diesel fraction through aromatics saturation.

INTEGRATION AND REGULATION OF VACUUM DEEP- CUT TECHNOLOGY Ⅰ. INTEGRATION OF EQUIPMENT TECHNOLOGY FOR VACUUM DEEP-CUT

2013, 44(10):  33-38. 

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The importance of deep vacuum distillation technology is prominent because of inferior heavy oil is rolled out and atmospheric residual oil is difficult to be directly used as a raw material of RFCC. The atmospheric and vacuum distillation units are optimized as a whole in this paper. The tower internals technologies of the NS stripping plate, NS vacuum tower feed distributor, NS dedicated grille packing of washing section, NS dual flow compound tray, NS resistance wall jet type liquid distributor, NS layer tower liquid collector and a complete set of equipment of direct contact heat transfer technology are integrated. Based on the integrated technologies, the operation conditions can be optimized such as increasing atmospheric column distillation rate, improving separation effect of flash distillation section, and vacuum degree and temperature of flash distillation section in vacuum tower, reducing entrainment, reducing backflow in flash distillation section, creating micro wet distillation in vacuum tower bottom and improving cutting clarity. The deep-cut vacuum distillation with low cost and low energy consumption is achieved.

STUDY ON HYDRODESULFURIZATION PROCESS OF DIESEL ON UNSUPPORTED CATALYST

2013, 44(10):  39-45. 

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Nowadays, deep hydrodesulfurization (HDS) of diesel fractions has become one of the most important approaches for production of clean fuels, as increasingly stringent quality standards of diesel fuel has been made all around the world. In the present work, operation conditions such as temperature, hydrogen pressure, liquid hourly space velocity (LHSV) and H2/oil volume ratio during the deep HDS of FCC diesel on an unsupported Ni-Mo-W catalyst were investigated, and activity of Ni-Mo-W catalyst was compared with a commercial NiMo/Al2O3 catalyst. The results show that reaction temperature, pressure, H2/oil ratio and LHSV made great influence on HDS efficiency of diesel fraction, and The reaction conditions of temperature 340 ℃, pressure 6.0 MPa, LHSV 1.5 h-1, and H2/oil ratio 600 were clarified to be the appropriate conditions for Shenghua FCC diesel hydrotreating on the unsupported Ni-Mo-W catalyst. The sulfur removal of the FCC diesel on the unsupported catalyst was 99.84%, and the nitrogen removal efficiency can reach up to 99.96%, much higher than that of the reference catalyst.

STUDY ON TECHNOLOGY PROCESS OF TREATING TREATMENT ACID GAS INCLUDING HIGH AMMONIA IN SULFUR RECOVERY UNIT

2013, 44(10):  46-50. 

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This paper presents the technique features of sulfur recovery unit in Sinopec Jinling petrochemical company. Based on brief introduction of principle of acid gas treatment and ammonia incineration, the three main factors which affect ammonia burning in oven were analyzed in detail. The problems in the ammonia bearing gas treatment in 50kt/a sulfur recovery unit and possible countermeasures were discussed. Some of practical technical solutions and experiences for long stable operation of treating the ammonia bearing acid gas were also introduced. By above countermeasures, SO2 emission is decreased to 424 mg/m3, friendly to environment. The NOx emission can be effectively controlled to less than 55 mg/m3.

INDUSTRIAL APPLICATION OF RS-1100 CATALYST IN DIESEL HYDROREFINING UNIT

2013, 44(10):  51-54. 

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The RS-1100 catalyst has been applied in the 1.6 Mt/a diesel hydrorefining unit of SINOPEC Cangzhou Petrochemical Company. Industrial application results show that RS-1100 catalyst has excellent hydrodesulfurization activity though the feedstock quality is worse than that of design and the average reaction temperature is 22 ℃ lower than the design value. The product meets the national Ⅲ standard of diesel oil. The RS-1000 provides a powerful technical support for diesel quality upgrading.

SYNTHESIS OF DECALIN BY ONE STEP HYDROGENATION OF NAPHTHALENE ON UNSUPPORTED NiMoW CATALYST

2013, 44(10):  55-60. 

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The synthesis of decalin by hydrogenation of naphthalene was studied using sulfided unsupported NiMoW catalyst in a continuous flow high-pressure micro-reactor. The catalyst was characterized by XRD and HRTEM. The characterization results show that the characteristic peaks of Ni3S2 and MoS2/WS2 exist on the sulfided unsupported NiMoW catalyst and the length of MoS2/WS2 crystal is about 5-10 nm with 3-5 stacking layers, while the crystal of reference supported NiMoW catalyst is 3-5nm long and 1-3 layers, respectively. The conversion of naphthalene is 100% and the selectivity of decalin is 99.1% on the sulfided unsupported NiMoW catalyst under the conditions of 240℃, 6.0MPa, Sv 1.0h-1, and the selectivity of decalin on reference catalyst is only 46%. It is revealed that the conversion of naphthalene and yield of decalin increase with the increase of temperature and pressure and with the decrease of liquid hourly space velocity (LHSV) on the sulfided unsupported NiMoW catalyst.

STUDIES ON CATALYTIC ACTIVITY OF HIERARCHICAL ZSM-11 WITH INTERGROWTH MORPHOLOGY

2013, 44(10):  61-66. 

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Hierarchical ZSM-11 zeolites with different SiO2/Al2O3 and different crystal size were used as active components of cracking catalysts and compared with commercial cracking catalysts (ZSM-5 as an active component). These active components were characterized by means of XRD, SEM, N2 adsorption, NH3-TPD and FT-IR. The results indicate that ZSM-11 zeolites possess pure crystal phase with high crystallinity, special intergrowth morphology as well as hierarchical pore structure. When tested in a micro fixed-bed reactor using Fushun vacuum gas oil (VGO) as a feedstock, catalysts based on ZSM-11 exhibit both better conversion ability for heavy oil and higher selectivity to high-value products (C3=+C4= and light fractions) than ZSM-5 catalyst. Particularly, the ZSM-11 sample with SiO2/Al2O3 ratio of 50 shows the superior performance than the other samples. In addition, as the crystal size decreases to 200 nm, the catalyst presents both enhanced conversion ability and selectivity to light oil but lower selectivity to light olefins.

IMPROVEMENT OF AROMATIZATION AND OIEFIN-REDUCTION CATALYST FOR FCC HEAVY GASOLINE

2013, 44(10):  67-72. 

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The aromatization and olefin-reduction catalyst M had been applied in commercial unit for desulfurization and olefin-reduction process of FCCG heavy fraction. To overcome the shortcomings of lower liquid yield and shorter cycle length at higher reaction temperature, a series of modification procedures were taken to improve the activity and stability of the catalyst M. A modified catalyst M-II was then successfully developed by improving manufacture of HZSM-5 and the ratio of the active metals. The results of the performance test of M-II, compared with that of catalyst M, show that aromatics increases more than 1.3 % and RON is 0.7 higher than M at the close reduction level of olefin.

DEACTIVATION AND REGENERATION OF Hβ-Al2O3 ALKYLATION CATALYST

2013, 44(10):  73-78. 

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The nano- Hβ molecular sieve was prepared by hydrothermal method，and the composite Hβ-Al2O3 alkylation catalysts were prepared by mechanical kneading. The causes of the Hβ-Al2O3 catalysts deactivation were investigated by means of TG, BET, NH3-TPD and Py-IR. The effect of regeneration conditions on the performance of the regenerated catalysts was examined, and the coke combustion kinetics of the deactivated catalyst was also investigated. The results show that the carbon deposition is the main reason of catalyst deactivation, which blocks up the micropores and covers quite a number of moderate intensity L acid center of the catalyst. The suitable regeneration conditions of the deactivated catalyst are: temperature 450 ℃, air flow 50 ml?min-1for the 5mL catalyst tested. Two stages with different carbon removal rate can be seen during the regeneration process and can be described respectively in two kinetic equations.

STUDY ON BENZENE OXIDATION CATALYZED BY Sn MODIFIED TS-1

2013, 44(10):  79-82. 

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The benzene catalytic oxidation performance of TS-1 modified by NH4AC and 0.5wt% Sn was studied. The zeolite was characterized by XRD，N2 adsorption - desorption，XRF，NH3-TPD，IR technologies. And the results indicate that the Sn can modulate the pore structure and surface acidity of TS-1. Mesopores are formed from micropores，extra surface area is increased, and a portion of strong acid sites are transformed into weak acid centers. The conversion of benzene on the zeolite with 0.5% Sn reaches 21.20%; phenol and hydroquinone yields are greatly improved by 3.7 times and 7.2 times after the modification , respectively.

INFLUENCE OF STORAGE ON DIESEL LUBRICITY

2013, 44(10):  83-88. 

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By High Frequency Reciprocating Rig test (HFRR), the relationship of the changes in lubricating properties of diesel products with sulfur content，polycyclic aromatics content before and after storage were studied. Resins were separated from diesels by solid phase extraction (SPE), and then studied on their lubricating property. The acidity and the varieties of basic nitrogen compounds in diesels were analyzed before and after storage. The results show that the lubricating properties of diesels with low solidification point is easy to become worse after storage. However, large changes in lubricating properties after storage will appear for the diesels with low content of sulfur and polycyclic aromatic. One reason that leads to the better lubricating property is the increase of acidity and the basic nitrogen compounds with lower hydrogen deficient number (z value) after storage. The lubricating properties of diesels will become worse after resins were separated out.

STUDY ON FRICTIONAL BEHAVIOR OF ENGINE OIL AND ADDITIVES BY MINI-TRACTION MACHINE

2013, 44(10):  89-93. 

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Mini-traction machine is an effective tool to evaluate the frictional behavior of lubricants and additives in elastohydrodynamic lubrication (EHL), mixed lubrication (ML) and boundary lubrication (BL) with appropriate testing conditions. The device also has an excellent ability to differentiate various lubricants and additives. Frictional behaviors of several additives were studied by MTM tester. Test results show that anti-wear property of ZDDP can be much affected by diverse anti-wear additives in fully formulated engine oil. Crystalline sulfonate is sufficiently helpful to reduce the coefficient of traction under BL condition, while it doesn’t show any improvement on the coefficient of traction in EHL and ML lubrications. The frictional properties and effective range of various friction modifiers also have much difference and need to be carefully balanced in practical use.

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ESTABLISHMENT OF TRANSFORMER OIL OXIDATION STABILITY TEST BENCH UNDER HIGH VOLTAGE AC AND DC FIELD

2013, 44(10):  94-98. 

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A transformer oil oxidation stability test bench under electric field was designed and established. Simulation tests for evaluating transformer oil oxidation stability under high voltage DC or AC field were conducted respectively for several kinds of transformer oils. Test results show that distinguished oxidation stabilities of different transformer oils under the different types of electric field can be obtained using the test bench. Transformer oils possess different oxidation stabilities under different types of electric fields. Anti-oxidation performance under DC field is better than that under AC field, while with no electric field is the best.

MASS ANALYSIS TECHNIQUE FOR DETERMINATION OF SALT CONTENT IN CRUDE OIL

2013, 44(10):  99-102. 

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A high efficiency mass analysis technique has been established for the determination of salt content in crude oils. The oil is extracted by 10 ml of the mixture of ethanol/water (1/3, v/v) in a thermostatic shaking table for 3 hours and then detected by coulometric titration method. The test parameters, such as extract time and extract reagent, are optimized. Under the optimal conditions, the recoveries of standard addition in samples are in the range of 98％-101％ with RSDs of (10 times parallel tests) less than 3% and the lower limit of detection is 0.1 ?g/g．Finally，this method is applied to the analysis of salt in real samples and the results compared with that of the method of SY/T 0536 indicate that the relative deviation of the new method is less than 6%.

ESTABLISHMENT OF LUBRICATING OIL FINGERPRINTS BY PYROLYSIS GAS CHROMATOGRAPHY- MASS SPECTROMETRY

2013, 44(10):  103-106. 

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Fingerprint of lubricating oil is the integrated embodiment of its integrity and fuzzy matter and can be used as an effective means of lubricating oil quality control. The application of pyrolysis gas chromatography-mass spectrometry in building fingerprints of lubricating oil was studied. The factors influencing the stability of fingerprints, such as preprocessing method, pyrolytic form, gas chromatography-mass spectrometry conditions, were examined. The fingerprint library of lubrication oils was then built with typical results of the fingerprints of lubricating oils tested. Some lubricating oils were used as samples to check the accuracy of the established fingerprint and the result exceeded 99%.