Table of Content

12 January 2015, Volume 46 Issue 1

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STUDY ON HYDROTREATING REACTIVITY OF YICHANG RESIDUE I. CHARACTERIZATION AND HYDROTREATING REACTIVITY OF YICHANG RESIDUE

2015, 46(1):  1-5. 

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Hydrocarbon constituents and structure parameters of Yichang residue were analyzed，and compared with that of Saudi-Arabian light crude residue by Fourier transform ion cyclotron resonance mass spectrometer and NMR techniques. The residue hydrotreating properties were tested in a pilot plant. It is found that compared with Saudi-Arabian residue, Yichang residue shows the properties of lower in sulfur, vanadium and aromatics content，but higher in nitrogen, nickel，and resin content. Its molecules are relative larger with high degree branching structure. A large amount of molecules contain nitrogen atoms. Under the same operation conditions and catalyst grading system, Yichang residue represents a significant lower Conradson carbon residue removal activity by hydrotreating (HCCR), compared with light Saudi Arab residue.

STUDY OF SULFUR COMPOUNDS IN MTBE

2015, 46(1):  6-9. 

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The sulfides in MTBE and their formation mechanisms during MTBE production were analyzed. It is found that all sulfur compounds in MTBE are from the refined LPG, one of stocks for synthesis of MTBE. The sulfides include thiols, thioether and disulfides. Thiols and disulfides are directly from refined LPG，while thioethers are attributed to the thioetherfication reaction of thiols with isobutene by catalysis of strong acidic cation exchanged resin. It is recognized that the analysis of sulfur compounds in MTBE can be helpful to estimate the operation problems and to further reduce sulfur content in LPG and MTBE during deep desulfurization processes.

EFFECT OF METAL IONS ON THERMAL OXIDATION STABILITY OF JET FUEL

2015, 46(1):  10-14. 

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The effect of transition metal ions on thermal oxidation stability of jet fuel was investigated. Jet fuels with different concentration copper, iron and zinc using their naphthenates as metal precursors were used. The test results indicate that the existence of transition ions of copper, iron and zinc appreciably affects the dynamic thermal oxidation stability. The impact extent on dynamic thermal oxidation stability of jet fuels follows the sequence: copper＞iron＞zinc. The results are benefit to prevent jet fuel to be contaminated by metal ions in the production and transportation.

PREPARATION AND PERFORMANCE STUDY OF DRAG REDUCTION POLYMER BY ETHYLENE/DODECENE COPOLYMERIZATION

2015, 46(1):  15-19. 

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Using ethylene and dodecene as polymerization monomers, a drag reduction copolymer of ethylene/dodecene was synthesized by solvent polymerization with n-Hexane as a solvent. The composite TiCl4/MgCl2 was used as a main catalyst and Al(i-Bu)3 as a cocatalyst. The structure and crystalinity of the copolymer produced were characterized by 13C-NMR and XRD techniques. The drag reduction performance of copolymer was evaluated in a self-designed indoor loop evaluation system with 1L reactor containing 600ml mixture of dodecene and n-hexane at -2℃. Under the optimum polymerization conditions: 0.4g main catalyst, n(Al)/n(Ti) of 80, V(dodecene)/V(n-Hexane) of 2/3, m(dodecene)/m(ethylene) of 912, the drag reduction rate is 45.45%. Compared with dodecene homopolymer, the crystallinity of the copolymer of ethylene/dodecene is significantly decreased due to the participation of ethylene, which helps to improve effective concentration of the copolymer in the oil, and to reduce the amount of drag reduction solution.

PREPARATION, CHARACTERIZATION AND EXTRACTIVE DESULFURIZATION PERFORMANCE OF 1- METHYL -3- BUTYL IMIDAZOLIUM TETRAFLUOROBORATE

2015, 46(1):  20-24. 

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An environment friendly ionic liquid (IL) 1-methyl-3-butyl imidazoliumtetrafluroborate ([BMIM]BF4) was synthesized by green synthesis method. The investigations of preparation method and the extractive desulfurization performance were conducted. The intermediate product [BMIM]Cl was obtained firstly by nucleophilic substitution reaction of N-methyl imidazolium and 1-chlorobutane under solvent-free condition, and then the product reacts with NaBF4 to get the target product ([BMIM]BF4). The molecular structure was confirmed by characterization of UV、FT-IR、MS and13C-NMR. The effect of extraction time, extraction temperature, sulfur compound type (BT or DBT), ratio of IL to model oil on extractive desulfurization was presented. The multistage extraction of DBT model oil with IL [BMIM] BF4 and its regeneration were studied. The results indicate that at the conditions of extraction temperature 40 ℃, 30min, and IL to oil volume ratio 1:2, the extraction desulfurization rate is 54.4% in single stage. While by 3 stage extractions, the sulfur removal rate is up to 90% and the IL can be recycled.

CORMMERCIAL APPLICATION OF NEW CATALYST TAILORED FOR MIP PROCESS

2015, 46(1):  25-27. 

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The commercial application of the new formula catalyst tailored for MIP process in the 2.8 Mt/a RFCC unit of PetroChina Huhhot Petrochemical Company was introduced. Compared with the original catalyst, the new catalyst has better heavy oil cracking ability, better coke selectivity, and higher light oil yield. LPG and slurry yield show a downward trend as the new catalyst inventory increases. The new formula catalyst is helpful to produce more propylene as well.

INDUSTRIAL APPLICATION OF AMBERLYST 35 RESIN CATALYST IN FCC LIGHT GASOLINE ETHERIFICATION

2015, 46(1):  28-33. 

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The industrial applications of the positive ion resin catalyst Amberlyst 35 in FCC light gasoline etherification unit of A and B companies were introduced. The results indicate that the catalyst has outstanding characteristics of high activity and simple starting-up. Both A and B company can produce low olefin and premium etherified gasoline over the catalyst. By a three-stage etherification，the total conversion rates of isoamylene are 97.59%，95.54% and the selectivities of tertiary amyl methyl ether (TAME) are 93.48%, 97.15% under the working conditions of case I and case II , respectively in company A. The total conversion rate of isoamylene is 97.21% and the TAME selectivity is 87.15% in company B.

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APPLICATION OF DOMESTIC CATALYSTS IN HYDRO-UPGRADING UNIT OF JINXI PETROCHEMICAL COMPANY

2015, 46(1):  34-38. 

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The combination of hydrotreating catalyst FF-36 and hydrocracking catalyst FC-50 were first used in the hydro-upgrading unit of Jinxi Petrochemical Company. The sulfurization and passivation procedures of the catalysts are introduced. The operating conditions, product qualities and energy consumption of the unit using domestic catalysts were compared with the imported composite catalysts. The results show that under somewhat higher operation severity conditions the HDS rate, HDN rate and CN increment are 1.6%, 2.6% and 8.9 points of the new catalysts higher than that of the reference catalysts, respectively. The energy consumption difference is small.

PREPARATION AND DESULFURIZATION PERFORMANCE OF ZnO-AC（ACTIVE CARBON） SORBENT

2015, 46(1):  39-43. 

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A desulfurization adsorbent ZnO-AC（active carbon）was prepared by kneading method. The sorbent was characterized by XRD, BET and Py-IR and its adsorptive desulfurization performance was evaluated in a 10 mL high pressure fixed bed micro-reactor using hydrotreated FCC gasoline as a feedstock. The results show that the C3-B adsorbent (30% active carbon) has a good desulfurization activity and stability. At 380 ℃，1 MPa, LHSV of 1.0 h-1, H2/Oil of 100:1, the sulfur content can be reduced from 78.2 μg/g of the feed to less than 10.0 μg/g of the product with only 0.9 octane number loss. The sulfur removal rate is 87.1%. The quality of the gasoline product meets the standard of national phase V gasoline.

CONVERSION OF C10 AROMATICS TO LIGHT AROMATICS ON NANO ZSM-5 ZEOLITE

2015, 46(1):  44-47. 

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The conversions of tetramethylbenzene and diethylbenzene, the main components in C10 fraction, to light aromatics on nano-ZSM-5 were studied in a pulse micro-reactor. The results show that at low temperature, isomerization of tetramethylbenzene is the main reaction, while at high temperature, the reaction is changed to dealkylation and transalkylation. The space velocity affects the competition of the two kinds of reactions of tetramethylbenzene. As to diethylbenzene, the dealkylation is the main reaction. If the maximum amount of BTX is the reaction goal, low space velocity and low temperature are the optimum reaction conditions for both of the reactants. The optimum reaction conditions can be used for lightening the C10 aromatics fraction in industrial unit.

PREPARATION AND PERFORMANCE OF Cu-SiO2 CATALYST FOR H2 PRODUCTION FROM METHANOL ON VEHICLE

2015, 46(1):  48-52. 

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Using copper nitrate and sodium water glass as materials, the Cu-SiO2 catalyst was prepared by co-precipitation method. The performance of Cu-SiO2 for methanol decomposition was studied in a fixed down-flow reactor. The influence of reaction temperature and WHSV were investigated. The evaluation results show that the Cu-SiO2 without pre-reduction by H2 gives a high catalytic activity for methanol decomposition, and exhibits a good regeneration property. At 300℃, WHSV of 0.79h-1 and atmospheric pressure, the conversion of methanol increases from initial 75.8% to 85.6% at 48h, and then remains at about 85% within 144h. The main products are hydrogen and carbon monoxide. A few of methyl formate and other products are also found. The influence of the temperature and WHSV on the activity of the catalyst is significant, but small on the products distribution. The test results indicate that the catalyst (Cu-SiO2) has a good applicability for the hydrogen production from the methanol on vehicle.

JET FUEL PRODUCTION BY UPGRADING COBALT-BASED LOW-TEMPERATURE FISCHER-TROPSCH SYNCRUDE

2015, 46(1):  53-58. 

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The properties of low-temperature cobalt-based Fischer-Tropsch syncrude and the technologies for production of jet fuel from the syncrude were introduced. The process scheme was involved in reactions of oligomerization, alkylation, aromatization, hydrocracking and hydroisomerization. By the designed process scheme, the jet fuel yield of up to 65.7% and gasoline of 18.3% are obtained by simulated calculation, the qualities of the two products meet the specifications of Jet A-1 and national phase V gasoline, respectively.

APPLICATION OF FCCG SELECTIVE HYDRODESULFURIZATION CATALYST REGULATION TECHNOLOGY

2015, 46(1):  59-61. 

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The commercial results of FCCG selective hydrodesulfurization catalyst regulation technology（RSAT）based on the RSDS-II process in Qingdao refinery show that the sulfur content of FCC gasoline can be dropped to less than 50μg/g, meeting the standard of national phase IV gasoline, or less than 10μg/g, meeting the phase V standard with less RON loss. In the late case, the ON loss is 0.4 point less than RSDS-II process, indicating the better selectivity of RAST technology. The commercial data over the long run time demonstrate that the product quality remains stable, though the sulfur content of material varies in a large range (391～1 580 μg/g), which is to show that the RSAT technology can meet the requirement of gasoline quality upgrading.

APPLICATION OF GARDES TECHNOLOGY IN FCC NAPHTHA HYDRODESULFURIZATION UNIT

2015, 46(1):  62-67. 

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The application of GARDES technology developed by PetroChina Petrochemical Institute and China University of Petroleum (Beijing) in FCC gasoline hydrodesulfurization unit of Daqing Petrochemical Company Refinery was introduced. The results show that the diene value of FCC gasoline is less than 0.45 gI/(100g) after prehydrotreating. The mercaptane sulfur content of LCN is less than 3μg/g, which can be blended into gasoline directly without alkali sweetening process. The sulfur content of FCC gasoline after HDS is decreased from 97~ 103μg/g to 26μg/g, the sulfur removal rate is 74 %. The mercaptane sulfur content in final product is less than 10μg/g, and the average octane loss is only 0.3 point. The GARDES technology can produce clean national phase IV standard gasoline.

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TRANSFORMER OIL COMPOSITION AND DETECTION DEVIATION OF ANTIOXIDANT CONTENT AND DETECTION METHOD OPTIMIZATION

2015, 46(1):  68-73. 

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The standard curves of relations of actual value and measured value are established based on transformer oils with different hydrocarbon compositions to investigate the different measured results of antioxidant content in the oils. The results show that the measured values change with aromatic content and the detection deviation is largely depends on the aromatic content in oils. To optimize the measuring method, low aromatic content base oil (CA value 0.23%) is used to establish calibration curves for detecting antioxidant content of samples. The correction factors and the modifier formula are established to calculate the correct value. The deviation between the correct value and the theoretical value is less than 0.005 point. The optimization greatly improves the accuracy of the detection method.

DETERMINATION OF ANTIOXIDANT IN LUBRICATING OIL BY DIFFERENTIAL PULSE VOLTAMMETRY

2015, 46(1):  74-77. 

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The differential pulse voltammetry method was used for determination of antioxidant type, remaining content, and the remaining life of the lube oil. The 0.1 mol/L KOH 92% ethanol-water solution was selected as the extraction liquid after the contrast test. The experiments provide the pulse signals of three kinds of antioxidants: 2,6-ditertbutylmethylphenol, the N-phenyl-a-naphthylamine, and zinc dialkyl dithiophosphate (ZDDP) for usage of qualitative analysis. The antioxidant decay curves of CF-4 and hydraulic 10 lubricants with aging time were obtained by simulated aging test. Thus the lube oil remaining residual life can be predicted based on the remaining content of antioxidant. The results show that the measurement method can be used not only for qualitative analysis of kinds of antioxidant in lubricating oils, but also for effective evaluation of the lubricating oil life and working state.

FEASIBILITY OF HOT HIGH-PRESSURE SEPARATION PROCESS IN ISOMERIZATION UNIT OF PX COMPLEX

2015, 46(1):  78-82. 

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Cold high-pressure separation process is now widely used in isomerization unit of PX complex, and results in an unreasonable energy consumption of PX complex. The advantages and the problems when using hot high-pressure separation process are analyzed. An accurate method for determination of isomerization product distribution is established. The hot high-pressure separation process is simulated by ASPEN PLUS, and the results indicate that recycle hydrogen concentration is almost not changed, compared with cold high-pressure separation process. Hot high-pressure separation process is proved to be feasible by industrial practice. The energy optimization scheme is proposed, and the simulation proves that the energy consumption of 370 kt/a PX complex can be reduced by 627 MJ/t.

STUDY AND APPLICATION OF ANALYTICAL METHOD FOR NOx IN RECYCLABLE OLEFIN-CONTAINING GAS

2015, 46(1):  83-88. 

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The method for NOx analysis in the recyclable olefin refinery gas was established. The solid absorption tube for pre-concentrating NO2 from gas sample and the special tube for NO oxidation to NO2 were prepared. The simulating gas containing trace NOx was prepared by the dynamic distribution equipment and used as an evaluation gas. Based on the quantitative parameters of the method and the interference of coexisting component determined by us of ion chromatography(IC) technique, a complete analytical method for NOx, consisting of pre-concentration solid absorption tube on-line and ion chromatography detection , was developed. The limits of determination for NO2 and NO of gas sample are 2 nL/L and 3 nL/L, respectively, when the sampl gas is 25 L. The analytical method of NOx can be well applied to determine the contents of NO2 and NO in the gas samples from dry gas concentration of ethylene cracking unit and steam cracking unit of Yanshan refinery.

BOILING RANGE DISTRIBUTIONS OF HYDROCARBON MOLECULAR COMPOSITIONS IN DIESEL BY GAS CHROMATOGRAPHY-TIME OF FLIGHT MASS SPECTROMETRY

2015, 46(1):  89-96. 

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A method for analysis of boiling range distribution of hydrocarbon molecular composition in diesel by gas chromatography-time of flight mass spectrometry (GC-TOFMS) was established. Carbon number distributions, average molecular weights and structures of hydrocarbon in different boiling ranges were studied. It is found that the average molecular weight of distillation range was influenced by aromatic content and degree of isomerization. The lower the aromatic content and the higher the isomerization degree is, the higher average molecular weight of the boiling range is. The boiling range distributions of hydrocarbon molecular compositions in diesel before and after hydrotreating were investigated. For hydrotreated diesel, boiling range distribution of saturated hydrocarbon is basically unchanged, but its concentration increases. Boiling range distribution of aromatic remains the same in low distillate fraction, whereas there is a concentration decrease in high distillate, which results in a higher average molecular weight of product than that of raw material diesel in high distillate fraction..

MONITORING BIODIESEL HYDROTREATING PROCESS CONDITIONS BY IR

2015, 46(1):  97-100. 

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The products of hydrotreated animal fats or vegetable oils were analyzed by IR spectrometer. The corrected height of the peaks at 2 925, 1 745, 1 710 cm-1 were used to calculate A1745/ A2925, a ratio of ester to alkane and A1710/ A2925 , a ratio of acid to alkane, which represent the contents of ester and acid in product, respectively. The results show that A1745/ A2925 and A1710/ A2925 are very effective to differentiate the hydrotreating depth, and can be used to screen the suitable reaction conditions for animal fats or vegetable oils hydrotreating processes.