Table of Content

12 October 2014, Volume 45 Issue 10

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INFLUENCE OF HYDROTREATING DEPTH ON PROPERTIES OF LCO

2014, 45(10):  1-7. 

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The influence of hydrotreating depth on the properties of diesel with low-sulfur and low-aromatic was investigated by simulating two-stage hydrotreating technology using two separate fixed-bed microreactors and different light cycle oils (LCO) feeds. The first reactor was packed with Ni-W sulfide catalyst, and the second reactor was packed with Pt-Pd noble metal catalyst. By adjusting the space velocity and reaction pressure, diesels with various hydrotreating depths were obtained. The results show that after deep hydrotreating, the density, refractive index, and the content of sulfur, nitrogen, and total aromatics decrease, while the hydrogen content and cetane number (CN) increase. The aromatic content of hydrotreated diesel is linearly related to the chemical hydrogen consumption, refractive index, density, and CN. The slope and intercept of the linear fitting of aromatic content and CN are different for various LCO, closely relating to the hydrocarbon compositions and the carbon number distributions. The intercept represents the CN of diesel after full aromatic saturation, and the slope reflects the contributions of aromatic saturation to CN. For feed LCO-I with 88 % of aromatic content, the CN will increase 0.26 units for every 1 percentage point reduction in aromatic content, and will reach up to 42.0 units after aromatic saturation in full. For the hybrid diesel LCO-II with 31% of aromatic content, every 1 percentage point reduction of aromatic content will increase the CN of 0.66 units.

RESEARCH ON ADSORPTION CAPACITY OF RFS09 SOX TRANSFER AGENT

2014, 45(10):  8-11. 

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The investigation of the adsorption capacity of RFS09 SOx transfer for simulated FCC regeneration flue gas was conducted in a small-scale fluid bed unit. The experimental results indicate that SO2 removal rate of SOx transfer is step down at some time point with the extension of running time. The accumulated adsorption capacity indicates a gradually increasing trend with running time. It increases quickly at the beginning of reaction and then goes up slowly. The absorption capacity per weight of SOx transfer in unit time decreases gradually and steps down at some time point. The accumulated absorption capacity of the SOx transfer increases with increase of loading, but it is not a simple amount of amplification. The research results indicate that there is an economic usage amount of SOx transfer in commercial unit for the largest SO2 accumulation absorption capacity per weight of SOx transfer.

SYNTHESIS AND CHARACTERIZATION OF NEW MICRO-MESOPORE MATERIALS BETA-KIT-6

2014, 45(10):  12-16. 

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The synthetic procedure of a new micro-mesopore material Beta-KIT-6 was described in detail. The materials synthesized were characterized by X-ray diffraction, N2 adsorption-desorption, scanning electron microscope, transmission electron microscope, nuclear magnetic resonance and infrared spectroscopy to understand more clearly the microporous materials Beta-KIT-6, including crystal type, specific surface area and pore size, morphology, channel structure as well as coordination forms of Al species, which laid a strong foundation for future development and application of Beta-KIT-6.

INFLUENCE OF ASPHALTENE CONTENT ON HYDROTREATING PROCESS

2014, 45(10):  17-20. 

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The reaction characteristics of different asphaltene content on hydrotreating process were studied in an autoclave with decalin as a solvent. The results show that the <200 ℃ fraction and coke yield increase; The denitrogenation rate, saturated and aromatic contents in hydrotreated residue decrease; while the asphaltene conversion, desulfurization rate and resin content in hydrotreated residue have a maximum. The molecular weight of hydrotreated asphaltene is less than that of the primary asphaltene, indicating the removal of the alkyl side chains and unit chip of asphaltene in hydrotreating process. The increase of asphaltene content is unfavorable for asphaltene hydrotreating when the reactant is only asphaltene in reaction system.

STUDY ON THERMOPHILIC AEROBIC FERMENTATION OF OILY SLUDGE

2014, 45(10):  21-27. 

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The effect of the anaerobic-aerobic fermentation and the function of addition of fowl manure as nutrients on the stabilization and harmlessness of oily sludge as well as composted sludge recycling were studied during the investigation of the possibility of thermophilic aerobic fermentation of oily sludge. It is shown by the results that the dewatered oily sludge mixed with additional fowl manure nutrients can be effectively fermented and stabilized by thermophilic aerobic method with an efficiency of oil removal about 60% or more. However, the oil removal by anaerobic- aerobic fermentation is not significantly better than by direct aerobic fermentation; the composted sludge can partly replace the nutrients and bulking agent during oily sludge aerobic fermentation. It is suggested that the optimized parameters of oily sludge aerobic fermentation are: air supplying rate from 0.025 m3/ (m3?h) to 0.05 m3/ (m3?h), the volumetric ratio of oily sludge to fowl manure nutrients of 3:1.

PRETREATMENT STUDY ON NORTHEN XINJIANG HIGH ACID SUPER HEAVY CRUDE OIL

2014, 45(10):  28-32. 

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The demulsifier screening was conducted for Northen Xinjiang high acid super heavy crude oil and the deacidification coupled with desalting pretreatment with it were studied. The influence factors on the deacidification and the desalting were investigated. Experimental results show that SXF2040 demulsifier is better for Northen Xinjiang crude oil. The optimal conditions for the deacidification of Northen Xinjiang crude are 70 ℃，400 r/min, reaction time 3 min, demulsifier to crude ratio 0.3, and settling time 30 min. At these optimal conditions, the deacidification rate reaches 94.6%. The acid number of the treated crude is 0.23 mgKOH/g, meeting the standard of low acid crude oil. While at the following conditions: SXF2040 demulsifier dosage of 20 μg/g, 130 ℃，water injection rate of 10%，combined electric strength of 400，-800，-1 200 V/cm and the corresponding processing time of 12 min, 10 min and 8 min，respectively, after deacidification-desalination two stage pretreatment, the acid number of the crude reaches a low acid value of 0.08 mgKOH/g, salt content less than 3 mg /L and the content of sodium is reduced to 1.75 μg/g.

CHANGES OF RESINS AND ASPHALTENES OF LIAOHE HEAVY OIL AFTER THERMAL REACTION

2014, 45(10):  33-36. 

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Liaohe heavy oil was heated for 2 hours in an autoclave at 350℃, 375℃ and 400℃, respectively. Saturates, aromatics, resins and asphaltenes were separated from oil sample. Elemental analysis, VPO molecular weight determination, IR analysis and H-NMR analysis for asphaltenes and resins were conducted. The results show that as increasing reaction temperature, the ratio of (asphaltenes and saturates) / (resins and aromatics) increases, the stability of the colloidal system of the heavy oil decreases. After thermal reaction, the molecular skeleton structure of resins and asphaltenes is not basically changed, but the breakage of side chain causes a reduction of molecular weight. Above 375℃, as the side chain is completely broken out, the degree of association of the asphaltenes enhances, thus its molecular weight increases.

RESEARCH ON MODIFICATION OF RESIDUAL OIL BY MICROWAVE

2014, 45(10):  37-40. 

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The effect of microwave radiation parameters（temperature，power and time） on viscosity reduction，desulfurization, group composition, removal of metal impurities was studied using Saudi Arabian medium crude residue（SZ）as a raw material. The results show that in the experimental condition range，viscosity of radiated product first decreases and then increases with increasing of temperature and radiation time; While it decreases with increase of the power. Sulfur content goes down gradually with the increase of the power. Saturated hydrocarbon and metal (Ni，V) contents basically remain unchanged; The content of aromatic hydrocarbon increases slightly; Resin and asphaltene decrease. Finally, the influence rule of the nature of three kinds of residues: SZ, Saudi Arabian light crude residue (SQ) and Jinling residue (JL) on the viscosity reduction treated by microwave was investigated. The results show that the more the asphaltene in feeds，the better the effect of viscosity reduction.

EFFECT OF MODIFICATION METHODS ON Fe-ZRP MOLECULAR SIEVE

2014, 45(10):  41-46. 

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Fe-ZRP zeolites were synthesized through solid state ion exchange, ion exchange and impregnation method. The zeolites were characterized by XRD, XPS, SEM and pyridine adsorption IR spectra to investigate the physico-chemical properties and the distributions, compositions and transfer cases of iron in the ion exchanged zeolites. The catalytic performance of zeolites by different methods and the functions of Fe2O3 loading introduced by solid ion exchange were examined as well. The results show that the surface Lewis acid and weak acid content are increased, resulting more total acid. The amount of Bronst acid is reduced in cases of impregnation and solid ion exchange. A less effect on total acid amount by liquid ion exchange is observed. Three forms of iron: isolate Fe3+ species, iron oxide clusters and α-Fe2O3 particles are found in the samples. Iron is mainly on the skeleton by liquid ion exchange method; while only part of iron are exchanged into the skeleton and more surface α-Fe2O3 particles are formed by solid state ion exchange. As increase of Fe2O3 loading, the areas and volumes of micro-pores of zeolites decrease due to the occupation of part of micropores by iron oxide. Ion exchanges low down the crystallinity of the zeolite for local excess acid. The change of acid is not linear with increase of iron. The threshold of loading amount is 2%-3% of iron that does not make particles gather. Lewis acid amount exists a maximum value within the loading amount tested.

INDUSTRIAL APPLICATION OF SMC-1 CATALYAT IN 1.80 Mt/a MTO UNIT

2014, 45(10):  47-51. 

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The methanol to olefin (MTO) catalyst SMC-1 developed by China Shenhua CTL and Chemical Company Ltd, was successfully used in Shenhua Baotou 1.80Mt/a MTO unit. The operation of the unit is stable and the unit processing capacity is up to 100% design load. The industrial application indicates that methanol conversion is 99.96% and selectivity of ethylene plus propylene is 79.24%. The total selectivity of ethylene, propylene, and hydrocarbon of C4 is up to 90.25%. The methanol conversion, selectivity of light olefin, and attrition resistance properties are equal to the comparative catalyst, while the coke yield is lower.

EFFECT OF CALCINATION TEMPERATURE ON PERFORMANCE OF SILICALITE-1 FOR VAPOR PHASE BECKMANN REARRANGEMENT OF CYCLOHEXANONE OXIME

2014, 45(10):  52-56. 

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Silicalite-1 was synthesized by hydrothermal method. The catalytic performance of Silicalite-1 treated by different calcination temperatures in vapor phase Beckmann rearrangement of cyclohexanone oxime was investigated. Silicalite-1 catalysts were characterized by XRD, IR, BET and thermal analysis. The results show that the calcination temperature has an important effect on the conversion of cyclohexanone oxime and the stability of the Silicalite-1 catalyst, but no obvious influence on the selectivity of caprolactam. With the increase of calcination temperature, BET surface area of molecular sieve does not change significantly, while external surface area first increases and then decreases. The ratio of micropore volume to the total volume is on the decline. The Silicalite-1 calcinated at 400°C exhibits an excellent activity and stability in vapor phase Beckmann rearrangement reaction.

PREPARATION, CHARACTERIZATION OF LARGE SURFACE AREA INERT Al2O3 AND PERFORMANCE OF NiO/INERT-Al2O3 CATALYST

2014, 45(10):  57-62. 

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The inert Al2O3 with α phase and high surface area was synthesized from Al(NO3)3?9H2O and urea by microwave radiation. The preparation conditions were studied. The NiO/inert-A12O3 catalyst with large surface was prepared by impregnation and its performance of selective hydrogenation for the diene in the model gasoline was evaluated using a micro-reactor. By means of XRD, BET, NH3-TPD and SEM, the synthesized inert-A12O3 and its catalyst were characterized. The results show that the morphology of the inert α phase A12O3, to a certain extent, is the fragment shape structure with surface area greater than 200m2/g. The suitable synthesis conditions are: mole ratio of Al(NO3)3?9H2O/urea 2.5-3.0, the microwave power of 600W, the radiation time about 10 minutes. After the catalyst with 9.87% NiO on the inert-A12O3 is activated with H2, its hydrogenation conversion and selectivity for the diene in the model gasoline achieve both about 100% at atmosphere pressure, 80 ℃, LHSV of 6 h-1, H2/oil ratio of 100/1.

APPLICATION OF NOxGETTER DENITRIFICATION AGENT TO CATALYTIC CRACKING UNIT

2014, 45(10):  63-66. 

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The denitrification agents consisted of NOxGETTER-NP and NOxGETTER from JOHNSON MATTHEY were applied to FCCU of Luoyang branch , SINOPEC. The NOxGETTER is the base agent with NOxGETTER-NP as a combution promoter containg bi-metals including Pd. The nitrogen contents in feeds tested are 3 017.2，2 211.1，1 818.3 μg/g, respectively. The test is devided into 3 stages：adding NOxGETTER-NP into regenerator alone，and adding NOxGETTER-NP plus NOxGETTER keeping between 1% and 2% of the inventory, respectively. The carbon content on regenerated catalyst are low of 0.003 4, 0.008 4, 0.009 4 percentage points, respectively for 3 stages, compared with the blank caliberation. The combustion effect is good, no partial burning or tail firing. The average contents of NOx in three export flue gas are 194.5，97.6，49.7 mg/m3 with denitrification ratios of 58.14%,78.99% and 89.3%, respectively. The effect of denitrification is signifcant and the cost is 3.4，9.4，18.9 Yuan/kg, respectively .

EFFECT OF HEAT REMOVAL OPTIMIZATION ON OPERATION OF FCC MAIN FRACTIONATOR

2014, 45(10):  67-71. 

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The FCC main fractionator usually has 2~3 pump-around (PA) heat exchanger. The lower PA has a higher temperature, indicating more valuable energy available. The effect of the heat removal optimization from the top and middle tower PA of the main fractionator on the operation was simulated using PRO/II simulation software. It is found that the increase of the energy recovery from the PA heat exchanger at the tower top and the first PA heat exchanger at the middle tower leads to an increase of the vapor and liquid phase load on the plate of the column. The model also indicates that under the conditions of stable heat recovery from the tower top PA, more heat removal from the middle tower PA needs more heat removal from the lower part of PA of slurry, resulting in lower total heat removal from the slurry (including upper part of PA of slurry), and higher yield of gasoline and diesel，while the slurry reduces slightly. The increase of heat removal from the tower top PA leads to a larger loading of both of gas and liquids phases at the lower part of the column, which makes the heavier component go up and more heavy components in gasoline and diesel products.

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OPTIMIZATION OF S Zorb UNIT OPERATION

2014, 45(10):  72-76. 

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The characteristics of S Zorb unit, in SINOPEC Jinling Petrochemical Company, are described. This article analyzed the factors influencing the production of low sulfur gasoline, loss extent of octane number as well as increase of liquid yield and reduction of energy consumption and suggested measures for optimization of operation parameters of feed quality controlling and reactor, regeneration and stabilization systems. By measures suggested, compared with base case, the gasoline quality is raised with sulfur less than 5?g/g, the energy consumption is less than 33.44 MJ/t, and the octane number loss of clean gasoline is only 0.3-0.7 units. The gasoline yield increases 0.23%.

DEVELOPMENT AND COMMERCIAL APPLICATION OF FULL HYDROGENATION TECHNOLOGY FOR PRODUCTION OF LUBE BASE OIL

2014, 45(10):  77-82. 

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A full hydrogenation process consisted of high pressure hydrotreating, iso-dewaxing and hydrofinishing is developed by Fushun Research Institute of Petroleum and Petrochemical and adopted in industrial unit to produce high viscosity index lube base oil. It has advantages in process simplicity and low investment. APIⅡ and Ⅲ grade lube base oils as well as low aromatic solvent naphtha and white oil can be produced under appropriate conditions. The commercial results show that the products have good qualities and high added values, bringing obvious better economic benefit to the enterprise.

PREPARATION AND PERFORMANCE OF NONYL DIPHENYLAMINE

2014, 45(10):  83-86. 

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Nonyl diphenylamine as a high base number antioxidant was synthesized by alkylation of diphenylamine with C9 olefins in the presence of solid Lewis acid catalyst in the laboratory. The product was isolated and characterized by NMR, TLC, and chromatography to determine the structure of these products and the content of the different components. The antioxidant performance in base oil was evaluated by means of RBOT and PDSC. It shows that the synthesized antioxidant contains tri-substituted (I) diphenylamine (II), disubstituted diphenylamine (III), monosubstituted diphenylamine (IV) and the unreacted diphenylamine. The total base number(TBN) order of these Component is Ⅳ>Ⅲ>Ⅱ>Ⅰ,the product prepared in lab has a higher TBN, better resistance to oxidation and less remaining diphenylamine compared to existing product.

CORRELATION OF PROPERTIES AND COMPOSITIONS OF HYDROTREATED LUBE BASE OIL

2014, 45(10):  87-91. 

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The properties and hydrocarbon compositions of 9 kinds of hydrotreated lube base oils were analyzed and their structure parameters were calculated by n-d-m method. The relationships between the structure and the hydrocarbon composition of hydrotreated base oil with density, refractive index, average molecular weight were explored. At the same time, the correlation of the alkane, cyclanes content in lube base oil with viscosity index and oxidation stability was tested. The results show that the density of the base oil has a positive correlation with the RT and RA; the refractive index has an approximate positive correlation with the structure parameters (CA, CN) and a negative correlation with CP; the average molecular weight has a positive correlation with aromatic and alkane content, and a negative correlation with the paraffinicity. The paraffin content has a positive correlation with the oxidation stability and viscosity index, but has a negative correlation with the naphthene content.

NUMERICAL SIMULATION OF GAS-PHASE FLOW FIELD IN FOURTH STAGE SEPARATION SYSTEM IN FCCU

2014, 45(10):  92-97. 

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Based on the Reynolds Stress Model, the three-dimensional gas-phase flow fields of two kinds of the fourth stage separation systems in FCCU were simulated. The characteristics of gas flow fields in the two systems were especially analyzed. The results show that in the material storage tank of the traditional structure, the gas flows upward at some areas, which is not conducive to particle sedimentation. Reverse flow exists in the dipleg. Bias flow happens in the cyclone separator, by which particle transportation is affected. The unreasonable structure design is the main reason for particle plugging. However, in the improved one, the air flow is relatively slow, favorable to particle sedimentation. In the dipleg, the pneumatic transportation is influenced by the periodic secondary vortex that can wear the wall. The flow field in the cyclone separator is stable enough for particle separation. Particle plugging can be avoided effectively in the improved structure. The comparison of the gas flow field in the two structures provides valuable guidance for designing efficient fourth stage separation system.

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RAPID QUANTITATIVE PHASE ANALYSIS TECHNOLOGY FOR DESULPHURIZATION SORBENTS AND ITS APPLICATION

2014, 45(10):  98-104. 

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The phase composition database of S Zorb sorbents has been established using Rietveld quantitative phase analysis method. The database covers almost all possibilities of S Zorb sorbent occurred in china. The rapid phase quantitative analysis models are established for fresh, spent, and regenerated sorbent respectively, which have good accuracy and repeatability. The alarm models were building for the Zn3O(SO4)2 phase of the spent and regenerated sorbents, and for the NiO phase of spent sorbents. The rapid phase quantitative analysis technology has successfully applied in an S Zorb industrial unit, which is helpful to optimize the operating parameters and to promote the long-periodic stable running of unit.