Table of Content

12 July 2012, Volume 43 Issue 7

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A CONSIDERATION ABOUT ENGINEERING DESIGN COPING WITH STRUCTURAL CHANGE OF GLOBAL CRUDE SUPPLY AND DEMAND

2012, 43(7):  1-7. 

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The changing in global crude supply-demand structure and developing trend are analyzed. During the 11th five-year plan period, SINOPEC Engineering Incorporation (SEI) has designed or retrofitted a number of new and existing refinery or petrochemical complex projects having different characteristics, four typical overall processing flows among them are reviewed. To further demonstrate the impact of selecting appropriate heavy oil upgrading scheme on plant profit, four heavy oil processing schemes involved novel technology and combined process are studied from perspective of liquid products production and investment return, techno-economically. Besides, coping with the change of crude supply structure, the incorporation of petroleum substitute fuel production in modern refinery is also discussed. The technical schemes of direct liquefaction of coal to oil and combined direct/indirect liquefaction of coal to oil are compared. Finally, some countermeasures for engineering design to cope with the change of crude supply-demand structure are proposed.

CATALYTIC PERFORMANCE STUDY OF HYDROCRACKING CATALYST RHC-3 UNDER HIGH PRESSURE AND ITS COMMERCIAL APPLICATION

2012, 43(7):  8-11. 

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New hydrocracking catalyst RHC-3 was developed for hydrocracking unit to produce tail oil used as steam cracking feedstock. The flexibility of processing inferior feedstock under high pressure by RHC-3 catalyst was studied in a hydrocracking pilot plant. Test data showed that good product slates and product properties were obtained by using RHC-3 catalyst, particularly the properties of tail oil were improved significantly. The application results of RHC-3 catalyst in a 2.0 Mt/a high pressure hydrocracking unit indicated that good quality tail oil with low BMCI value and high alkane content was produced; meanwhile, the yield of tail oil could be kept at a high level.

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ISOMERIZATION AND AROMATIZATION OF n-OCTANE OVER VARIOUS MOLECULAR SIEVES SUPPORTED NICKEL CATALYATS

2012, 43(7):  12-16. 

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Nickel supported catalysts were prepared by impregnating nickel on SAPO-11, USY and ZSP-3 molecular sieves. BET, XRD, NH3-TPR and pyridine adsorption-desorption FT-IR were used to characterize the prepared catalysts. The hydroisomerization and hydroaromatization performance of these catalysts were evaluated with a micro-reactor using n-octane as model compound. Test results indicated that among the three catalysts, Ni/SAPO-11 showed the highest isomerization selectivity and good aromatization selectivity, but its conversion was the lowest; Ni/ZSP-3 showed the highest conversion and aromatization selectivity, yet its isomerization selectivity was the lowest; Ni/USY showed moderate isomerization selectivity and conversion, however, its aromatization selectivity was poor. Using ZSP-3 molecular sieve modified by rare earth cations as support, the surface acid center distributions of catalyst were altered, resulting in an enhancement of catalyst selectivity to isomerization and aromatization.

A STUDY OF Zn-Pt-Re/ZSM-5 AROMATIZATION CATALYST

2012, 43(7):  17-22. 

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The influences of Zn, Pt and Re contents on the acidity and aromatization performance of Zn-Pt-Re/ZSM-5 catalyst were studied. The effect of reaction conditions, such as reaction temperature, pressure and volume space velocity (LHSV) on the performance of Zn-Pt-Re/ZSM-5 catalyst was investigated in a continuous flow micro-reactor using n-hexane as probe molecule. Test results showed that with the increase of Zn content in catalyst, the amount of Br?nsted (B) acid sites increased and Lewis (L) acid sites decreased gradually. The existence of Pt and Re (esp. Re) in catalyst was beneficial for increasing the amount of B acid sites. It was found that the alkane aromatization was the synergetic effect of B acid and L acid, and the aromatics yield could be enhanced when B/L ratio was about 0.2. There was a very good corresponding relationship between aromatics yield and the changing trend of medium-strong acid amount of catalyst. High reaction temperature was favored to aromatization reactions, an aromatics yield of over 95% could be obtained when the reaction temperature was over 450 ℃. However, high reaction pressure and high LHSV had negative effect on the conversion and aromatics yield. The optimum reaction conditions for aromatization of n-hexane over Zn-Pt-Re/ZSM-5 catalyst were obtained as follows：a reaction temperature of 450 ℃，a reaction pressure of 1.0 MPa and LHSV of 1.0 h-1.

INDUSTRY OPERATION AND REGENERATION OF TRANSALKYLATION AND DISPROPORTIONATION CATALYST

2012, 43(7):  23-26. 

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The operation of transalkylation and disproportionation catalyst under high space velocity and low hydrogen to hydrocarbon (H2/HC) ratio at the aromatics complex unit of CNOOC Huizhou Refinery was introduced, as well as the regeneration of this catalyst. Processing feedstock with relative high C10+ aromatics content and after running about 2 years under high space velocity and low H2/HC ratio conditions, the coke deposited on the catalyst was as high as over 39%, thus the activity of the catalyst dropped significantly. The deactivated catalyst was stripped by hydrogen, and then followed by burning coke under low oxygen atmosphere and removing coke under high oxygen atmosphere, about 35.80 t of coke was eliminated. The catalytic performance of the regenerated catalyst was good, which indicated that said catalyst possessed good regeneration property.

EFFECT OF Zn MODIFIED ZRP ZEOLITE CATALYST ON THE AROMATIZATION OF CATALYTIC CRACKING NAPHTHA

2012, 43(7):  27-32. 

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The effect of zinc modified ZRP zeolite catalyst on the aromatization of FCC naphtha was studied using a fixed bed micro-reactor, and the function of zinc on the aromatization reaction was investigated. Through analyzing the surface acidity of catalyst prior and post to Zn modification from pyridine adsorption FT-IR spectra, the aromatization reaction mechanism of FCC naphtha over Zn/ZRP zeolite catalyst was proposed. Test results showed that the aromatization performance of ZRP zeolite catalyst was improved significantly by Zn modification. By discussing the reaction mechanism, it was found that the aromatization of FCC naphtha over ZRP zeolite catalyst was mainly through hydrogen transfer reactions, yet over Zn/ZRP zeolite catalyst was mainly through cyclization and dehydrogenation reactions assisted by hydrogen transfer reactions, besides, cracking, oligomerization and isomerization reactions were implicated as well. [Zn(OH)]+ active sites having both B/L acid functions might exist in the channels of Zn/ZRP zeolite to meet the requirements of aromatization reaction in various stages, thus the aromatization performance of ZRP zeolite catalyst was enhanced by Zn modification.

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EFFECT OF PHOSPHORUS ON THE INTERACTION BETWEEN ACTIVE COMPONENT AND CARRIER OF NiMo/Al2O3 CATALYSTS

2012, 43(7):  33-37. 

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Temperature-programmed reduction (TPR) and X-ray photoelectron spectroscopy (XPS) were used to characterize a series of NiMo/Al2O3 catalysts prepared by impregnation method. The interaction between active component and carrier and the effect of phosphorus on the interaction of NiMo/Al2O3 catalysts was studied. Test results indicated that various interactions (week and strong) among active components Ni/Mo species and γ-Al2O3 carrier existed, and the interaction also happened between Ni species and Mo species. Adding phosphorus into NiMo/Al2O3 catalyst could weaken the interaction between active component and carrier. Catalysts samples prior and post to sulfurization were analyzed by XPS and the existence of Al species interacted with active component was verified. Furthermore, Al2p binding energies in various samples were determined, as well as the effect of phosphorus on the interaction between Mo species and the carrier could be determined quantitatively by the XPS results of sulfidized samples.

STUDY ON THE ADSORPTION EQUILIBRIUM PARAMETERS AND MASS TRANSFER COEFFICIENTS OF C8 AROMATIC ISOMERS ON ZEOLITE X

2012, 43(7):  38-43. 

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The saturated adsorption capacities and equilibrium constants of C8 aromatic isomers were determined through static adsorption method at 177 ℃ and 0.8 MPa, using barium exchanged X zeolite as adsorbent. The breakthrough curve of individual C8 aromatic isomer was obtained by pulse experiments. The lumped mass transfer coefficients of C8 aromatics were calculated through curve fitting by Aspen Plus software. Simulating experiments were carried out to separate p-xylene, o-xylene, m-xylene and ethylbenzene for validation. Results showed that the simulated curves of all these components were in well accordance with the data from experiments.

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A STUDY OF TWO-STEP SYNTHESIS OF METHYL METHACRYLATE FROM ISOBUTENE

2012, 43(7):  44-47. 

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Compound oxide catalyst for isobutene selective oxidation to methacrolein (MAL) and supported noble metal catalyst for MAL oxidative esterification to methyl methacrylate (MMA) were prepared, and a new process for two-step synthesis of MMA from isobutene was developed. For isobutene to MAL process, under a reaction temperature of 380 ℃ and a reaction pressure of 0.03 MPa, the average conversion of isobutene and the average selectivity of MAL reached 93.7% and 92.3%, respectively. For MAL to MMA process, under a reaction temperature of 90 ℃ and a reaction pressure of 0.27 MPa, in batch reaction mode, the MAL average conversion and the average selectivity of MMA was 93.35% and 83.50%, respectively; under two-stage continuous operation mode, the MAL average conversion and the average selectivity of MMA was 93.24% and 80.06%, respectively.

INFLUENCE OF VARIOUS ADDITIVES ON THE REACTION PERFORMANCE OF RESIDUE HYDROTREATING

2012, 43(7):  48-51. 

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The influence of additives on the product distribution of residue hydrotreating process was studied by adding additives having various functional groups into residue feedstock. Test results showed that the influences of different additives on the hydrotreating reaction performance were mainly embodied on the yields of light oil and resid (>500℃). Adding dodecyl benzene sulfonic acid (DBSA) with acidic functional groups exhibited the best positive effect: the light oil yield and residue conversion increased significantly as compared with base case, coke yield increased slightly; followed by oleic acid. However, adding p-tert-butyl catechol (TBC) with acidic functional groups and fatty amine with basic functional groups showed little positive effect. When adding polysorbate-80 with neutral groups, negative effects, such as higher coke yield, lower light oil yield and less residue conversion were observed. These phenomena should be attributed to the changing of asphaltene existing state in the residue feedstock, the increase of asphaltene solubility and colloid stability by adding additives.

STUDY ON THE CHANGING OF COMPOSITION AND STRUCTURE OF ASPHALTENE DURING RESIDUE HYDROTREATING

2012, 43(7):  52-56. 

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Residue oil hydrotreating experiments were carried out on a pilot plant unit to investigate the effect of reaction temperature and hydrotreating severity on the composition and the molecular structure of asphaltenes in the treated residue samples. Results showed that with the increase of reaction temperature or the depth of hydrogenation, the asphaltene content in the treated residue sample decreased; the sulfur, nickel and vanadium contents of asphaltene dropped, but the nitrogen content gave an increase trend. The average molecular structural parameters of asphaltene in the obtained samples were calculated from the spectrum of 1H-NMR and 13C-NMR. Results showed that with the increase of reaction temperature, the fraction of paraffins decreased and the fraction of aromatics increased; however, with the increase of hydrogenation depth, the fraction of paraffins increased and the fraction of aromatics decreased.

EFFECT OF ACETATE ESTER ON THE PHASE STABILITY OF METHANOL–STRAIGHT-RUN GASOLINE BLENDS

2012, 43(7):  57-61. 

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Effect of a series of acetate ester co-solvents on the phase stability of methanol–straight-run (SR) gasoline blends was studied by testing the phase separate temperature of these blends. Results show that methyl acetate, ethyl acetate, propyl acetate, butyl acetate, amyl acetate and isoamyl acetate all have positive effect on the phase stability of a series of methanol–SR gasoline blends with various blending ratios (M15, M30, M50 and M65) in the temperature range of -27 ℃ to 36 ℃, and this effect enhances with the increase of carbon number in the oxyalkyl of acetate ester. The effect of alkoxy isomerization on the phase stability of methanol–SR gasoline blends was studied by comparing the phase stabilities of these blends containing butyl acetate, amyl acetate and isoamyl acetate respectively.

A PERFORMANCE STUDY OF SBS MODIFIED PAVING ASPHALT FROM TAHE CRUDE OIL

2012, 43(7):  62-67. 

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SBS modified paving asphalt samples from Tahe Crude oil were prepared by using suitable technique, and analysis results show that their properties well meet the requirements of JTG F40-2004 technical specification. It is observed that by adding stabilizing agent, a homogeneous micro-structure system of SBS and Tahe asphalt is formed, and thus, the storage stability of SBS modified Tahe asphalt is good. The results of conventional performance analysis indicate that Tahe SBS modified paving asphalt is less sensitive to temperature, and it possesses excellent high-low temperature performance. These paving asphalt samples were also evaluated by SHRP procedure. Test results show that Tahe SBS modified paving asphalt samples exhibit excellent performance of temperature response and resistance to fatigue cracking, which meet the performance grade of PG70-34 and PG76-34 respectively.

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THE VERIFICATION OF CONTINUOUS LIQUID-PHASE HYDROPROCESSING TECHNOLOGY BY SIMULATION CALCULATION

2012, 43(7):  68-71. 

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Based on the operation data from gas oil hydrotreating units, the impacts of excess hydrogen, recycle liquid ratio and stripping hydrogen on the operation of unit adopted continuous liquid-phase hydroprocessing technology are analyzed by simulative calculation. The calculation results show that a small amount of gaseous excess hydrogen in reactor can build up a relative high hydrogen partial pressure; the presence of recycle oil is helpful to reduce the rise of temperature along catalyst-bed; moreover, an appropriate amount of stripping hydrogen can dilute the H2S concentration in reactant significantly. Therefore, it is well founded that the functions of recycle hydrogen system in conventional hydrotreating unit are fulfilled by the continuous liquid-phase hydroprocessing technology, which indicates that the recycle hydrogen system in hydroprocessing unit might be canceled in future.

APPLICATION OF RVHT TECHNOLOGY FOR CLEAN GASOLINE PRODUCTION

2012, 43(7):  72-76. 

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The vacuum gas oil (VGO) hydrotreating technology (RVHT) developed by Research Institute of Petroleum Processing was applied with matching catalysts series in a 1.8 Mt/a VGO hydrotreating unit of Maoming Company, SINOPEC, by which the hydrotreated VGO with sulfur content less than 0.1% could be obtained using inferior feedstocks under mild reaction conditions. The results showed that with the integrated process of VGO hydrotreating and FCC by using the hydrotreated VGO as the feed for FCC units, the clean gasoline blending components meeting the Guangdong Ⅳ standard could be produced with good social and economic benefits.

TECHNOLOGY IMPROVEMENT AND APPLICATION IN THE LOCALIZATION OF S ZORB TECHNOLOGY

2012, 43(7):  77-80. 

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To eliminate the factors affecting the stable operation of FCC naphtha adsorptive desulfurization (S Zorb) units, based on the accumulated experience and know-how in refining and chemical engineering design, SINOPEC Engineering Incorporation applies various technology innovations and transplantations in the localization of the first seven S Zorb units, such as developing a dustfall device for reactor to prolong the service life of back-flush valve, improving regeneration system to solve the caking of adsorbent, arranging feed/reactant heat exchangers in parallel two-row to maintain continuous operation, and adopting lock hopper control system to ensure the transport of adsorbent smoothly. After completing design and construction, these units go on stream successfully and their operation cycles prolong significantly, furthermore, their adsorbent consumption and energy consumption are reduced as compared with base case, which indicates a new generation of S Zorb technology is developing to support the upgrade of gasoline quality.

ANALYSIS AND DISCUSSION ON CIRCULAR ECONOMY OF PETROCHEMICAL AND SALT CHEMICAL INTEGRATION

2012, 43(7):  81-85. 

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The characteristics of circular economy system based on the integration of petrochemical and salt chemical is discussed in depth, and the situations before and after the implementation of this project are analyzed. Adopting combined process to manufacture PVC, the ethylene in dry gas and the by-product hydrogen chloride all can be used, besides, the supply of electrolytic hydrogen is less. The improved chlorohydrine process for propylene oxide (PO) production can reduce the consumption of soda, seawater and propylene significantly; furthermore, the zero discharge of wastes from PO unit is realized. The comprehensive utilization of DCC dry gas and C4 resource can promote the added value of products. On the whole, by optimizing overall process planning and applying technology innovations, the objective goal of maximum utilization of various resources, less energy consumption and waste discharge could be reached.

THE DESIGN OF REFINING CONFIGURATION FOR PROCESSING HIGH-SULFUR INFERIOR CRUDES

2012, 43(7):  86-90. 

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Three mature combined refining configurations, delayed coking+CFB, RDS+RFCC and DAU+IGCC, for processing high-sulfur inferior crudes are summarized, and the limitations of these configurations are analyzed as well. During the design of overall process flow for refinery, several issues including enlarging refinery scale and processing various sources of crude, processing unconventional extra-heavy crude, conflict requirement between increase gasoline production and chemical feedstock supply, production of low sulfur products, and integration of oil and coal, should take into account, in this paper some feasible ideas and suggestions are proposed.

PREPARATION OF SULPHONATED ALKYLPHENOL AND ITS CORROSION INHIBITION PERFORMANCE

2012, 43(7):  91-95. 

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Sulphonated alkylphenol was synthesized with alkylphenol (A) and concentrated sulphuric acid (B), and the effect of reaction conditions on the sulphonation rate was studied. The structure of the prepared sulphonated alkylphenol was characterized by means of FT-IR．Rotary weight-loss method，digital camera，microscope and EDS were used to investigate the corrosion inhibition performance of sulphonated alkylphenol．Results showed that under the optimal reaction conditions of B/A mole ratio of 1.25，a reaction temperature of 60 ℃ and a reaction time of 2 h, the yield of sulphonated alkylphenol could reach 90.46%．Sulphonated alkylphenol used as corrosion inhibitors could suppress the corrosion of A3 steel by naphthenic acid effectively, due to the formation of a protected film on the steel surface. The corrosion inhibition rate reached 93.27% under the following conditions: sulphonated alkylphenol concentration of 1 000 mg/L, corrosive medium temperature of 280 ℃，with a stirring speed of 300 r/min and the residence time in corrosive medium was 6 h．

DEVELOPMENT OF SLURRY ANTIFOULANT FOR PETROLEUM PROCESSING

2012, 43(7):  96-98. 

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Based on analyzing the fouling mechanism of slurry oil in petroleum processing, several antifoulants were prepared including components for cleaning and dispersion, antioxidation, metal passivation and corrosion inhibition. The main cleaning and dispersion component was synthesized in lab using polybutadiene thiophosphoric acid and hexanediol as raw materials. The antifouling performance of the prepared antifoulants was tested. Results showed that using FCC slurry as feed under the testing conditions, with an optimum antifoulant dosage of 150 ?g/g, the antifouling rate of the optimum antifoulant reached 92.07％.

TEST METHODS FOR DETERMINING FREEZING POINT OF JET FUEL

2012, 43(7):  99-104. 

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The progresses, principles and correlations among methods for determining freezing point of jet fuel are presented. According to the appointment of the national standard ASTM D1655-07e for jet fuel, in United States test methods including conventional ASTM D2386-06, automatic phase transfer ASTM D5972-05, automatic laser ASTM D7153-05 and automatic fiber optic ASTM D7154-05, are all qualified to be used alternatively for determining freezing point of jet fuel, in which only ASTM D5972-05 and ASTM D7153-05 can be used as arbitration methods. The above four test methods are also being used for determining the freezing point of jet fuel in other countries, yet only ASTM D2386-06 and its equivalent can be used as arbitration methods. In China, based on the requirement of national standard GB 6537—2006 for 3# jet fuel, test method GB/T 2430-2008 and SH/T 0770-2005, which is equivalent to ASTM D2386-06 and ASTM D5972-05 respectively, are now used for determining the freezing point of jet fuel and GB/T 2430-2008 is the arbitration method. ASTM D5972-05, ASTM D7153-05 and ASTM D7154-05 are highly automatic instrumental methods developed recently; they are relatively easy to be operated and having good reproducibility. Other methods for measuring freezing point of jet fuel in research or under standardizing are also outlined briefly.

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GAS CHROMATOGRAPHY METHOD FOR DETERMINATION OF UNDERIVATIZED FREE FATTY ACID AND FATTY ACID METHYL ESTER

2012, 43(7):  105-111. 

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A gas chromatography (GC) method was developed for the determination of underivatized free fatty acid (FFA) and fatty acid methyl ester (FAME). Test results show that long/medium chain FFAs and FAMEs in sample could be separated by a single run, when using a CP-FFAP CB capillary column and with a heating procedure as follows: keep at starting temperature (180℃) for 0.5 min, using a heating rate of 3℃/min to reach 210℃, followed by heating to 250℃ with a rate of 10℃/min and keep for 30 min. The contents of every FFAs and FAMEs in the sample could also be determined accurately by employing two internal standards.