Table of Content

12 April 2015, Volume 46 Issue 4

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DEMULSIFICATION TECHNOLOGY FOR EMULSIFIED CRUDE OIL FROM ACIDIZING WELLS IN TAHE OILFIELD

2015, 46(4):  1-6. 

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Studies indicated that the reason for demulsion difficulty of Tahe emulsified crude oil was closely related to residual chemicals, solid particles, resins and asphaltenes in the crude oil. Therefore, we developed a demulsifying technology were for the crude, including excellent performance chemicals, such as demulsifiers, wetting agents, and neutralizer as well as the supporting treatment technologies of washing and electrostatic field. The results show that the washing pretreatment of oil could reduce the dosing of chemicals and provide a lower load for the subsequent process, and benefits for the smoothly running of electric dehydrator. After washing, the subsequent chemical demulsification and electrostatic dehydration technologies can reduce the water content to less than 1%, satisfied with the requirement of Tahe oilfield.

RESEARCH ON HYDROTREATMENT OF OIL SANDS BITUMEN

2015, 46(4):  7-11. 

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The oil sands bitumen is an inferior raw material with high density, high viscosity, and high content of metal and carbon residue（CCR）. The impact of reaction temperature and reaction time on hydrotreating performance of oil sands bitumen was investigated with an autoclave and ebullated bed hydrotreating catalyst to find the optimal hydrotreating conditions. The test results show that as the temperature and reaction time increases, contents of Fe, Na, Ni, V, and CCR decrease. High temperature promotes the removal of metal and reduction of carbon residue. The best reaction conditions are: a temperature of 430 ℃ and a reaction time of 80min. Under the best conditions, the removal rates of Fe, Na, Ni, V reach 99.97%，99.99%，98.11%，99.61%, respectively. And the reduction rate of carbon residue is 72.61%. It is concluded that the ebullated bed hydrotreating is an effective technology for deep processing oil sands bitumen.

EFFECT OF Cr3+ ON Ni AND V TRAPPING FROM CRUDE OIL UNDER MILD HYDROGENATION CONDITIONS

2015, 46(4):  12-15. 

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In order to trap the heavy metal Ni and V in Oman crude oil and reduce their influence on the subsequent processing, With NaBH4 as a H2O reducing agent for producing H2, CrCl3 ? 6 H2O was used as a metals trapping agent to investigate the effect of metal capture agent amount, reaction temperature and reaction time on the metal capture in the hydrogen atmosphere. Results show that the optimal conditions are: a temperature of 150 ℃, NaBH4 and CrCl3 of 0.07 % and 0.12%, respectively, reaction time of 3 h. The trapping rates of Ni and V reach 71.23% and 46.47%, respectively under the best conditions. The mechanism of trap effect explore results shows that under the hydrogenation condition, the outer ring of etioporphyrin nickel is hydrogenated, the N-Ni bonds are broken and Ni2+ is removed from the prophyrin ring. Compared with Ni2+, Cr3+ has a stronger binding energy and Cr3+ replaces Ni2+ and generates more stable metal complex.

NOVEL APPROACH FOR OXIDATIVE DESULFURIZATION OF THIOPHENE IN MODEL GASOLINE WITH HETEROGENOUS FENTON SYSTEM

2015, 46(4):  16-21. 

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The XO-Fe2O3/γ-Al2O3 (X: La, Ce, Co and Cu) catalysts in Fenton system (catalyst + oxidant H2O2) were prepared and characterized by XRD, SEM and BET techniques. The oxidation removal of thiophene in model gasoline (n-octane solution) with heterogeneous Fenton system was tested to investigate the effect of kind of metals, n(H2O2)/n(S) and catalyst dosage. The characterized results demonstrate that the catalysts have meso-pore structures. The desulfurization tests indicate that the catalyst Fe2O3/γ-Al2O3 promotes the production of ?OH radical from H2O2 to oxidize the thiophene, thus improves the removal of thiophene. The addition of second metal can improve the catalytic activity of Fe2O3/γ-Al2O3. Among of them, Cu is the best one. Under the conditions of temperature 333K, catalyst dosage 0.2g, n(H2O2)/n(S)=7.40 and reaction time 120 min, 95.3% of thiophene can be removed. The S content in product is reduced to 9.4μg/g, which meet the ultra-deep desulfurization object.

COAL GASIFICATION PRINCIPLE AND ITS TECHNOLOGY DEVELOPMENT DIRACTION

2015, 46(4):  22-28. 

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The complexity of coal constituent and the variety of downstream processes lead to variety of coal gasification technologies. Domestic coal gasification technologies nowadays were analyzed in this paper based on the coal gasification principle. It is thought that the slag flow bed is the main development direction of coal gasification technology, which possesses the advantages of high gasification reaction efficiency, high carbon conversion rate and is the best green process. The pyrolysis layer in moving bed leads to higher methane content in product gas and is good for coal to manufacture nature gas, but the problems of lower gasification intensity and alkali metals enrichment in the bed occur；Fluidized bed pyrolysis-gasification process can also raise methane content in its product gas. The gasification intensity is higher than that of moving bed if reasonable particulate size of feed coal is used. There are various problems for the other gasification technologies and need to continue to research and development or think carefully about industrial application.

ADVANTAGE OF MIP SERIES TECHNOLOGIES IN IMPROVING TOTAL LIQUID YIELD

TANG Jin-lian Jin-lian congli cheng

2015, 46(4):  29-32. 

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Data of liquid yield from representative running MIP unit was analyzed and compared with FDFCC, FCC and TSRFCC processes. The statistical data show that MIP technologies have higher total liquid yields with higher gasoline and liquefied petroleum gas (LPG) yields, lower dry gas and slurry yields in processing hydrotreated heavy oil, hydrotreated gas oil and atmospheric residue. Relative to other technologies, the liquid yield of MIP is 2 percent higher at least with higher ratio of gasoline to diesel oil of MIP process. The MIP gasoline is lower in olefin and sulfur content and higher or equivalent octane number to other process. That can mainly attribute to the unique two reaction zones in one riser reactor, each having suitable reaction condition for the different reaction of hydrocarbons. The suitable reaction condition in each zone intensifies the heavy oil conversion and decreases dry gas and coke yields so that total liquid yield is increased.

SIMULATION OF CUTTING DEPTH OF DISTILLATION TOWER OF DELAYED COKER

2015, 46(4):  33-39. 

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The naphtha end point(x) from delayed coking distillation tower is taken as the independent variable representing the depth of separation. The relationships between x and energy consumption, steam product, product distribution are examined based on the process flow sheet，using the technology of process simulation and data regression. A general method of determining the optimal x is developed, considering the total economic benefit or total energy loss. The application of the method in a 4.2 Mt/a delayed coker can improve the benefit of the unit about 7.679 million Yuan/a.

INFLUENCE OF NICKEL PRECURSORS ON STRUCTURE AND ACTIVITY OF UNSUPPORTED Ni-Mo-W CATALYSTS FOR DIESEL HYDROTREATING

2015, 46(4):  40-45. 

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A series of Ni-Mo-W composite oxides were prepared through hydrothermal synthesis method by changing nickel precursors. The influence of nickel precursors on structure and activity of unsupported catalysts was investigated and the composite oxides were characterized by BET, XRD and SEM. Unsupported catalysts were prepared through wet-mixing-kneading method, and the fluid catalytic cracking (FCC) diesel was used as a feedstock for activity evaluation of the unsupported catalysts in a 20 ml high-pressure hydrotreating unit. The experiment results show that the composite oxides from nickel nitrate have less BET surface area and pore volume. While crystal phase of Ni-Mo-W composite oxide from basic nickel carbonate precursor tends to be amorphous, and particle size is smaller than that from nickel nitrate precursor. The experiments also reveal that surface area and pore volume of the composite oxide synthesized by basic nickel carbonate precursor are improved a lot. The activity evaluation results show that the catalyst prepared by basic nickel carbonate with larger pore volume & lower surface area performs the highest activity of hydrodesulfurization (HDS), hydrodenitrogeneration (HDN) and aromatics saturation. The sulfur and nitrogen removal rate reaches to 99.91% and 99.94%, respectively.

SYNTHESIS AND EVALUATION OF ZSM-5 ZEOLITE CATALYST FOR MTP

2015, 46(4):  46-50. 

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Fine grain NaZSM-5 zeolites with wide range of Si/Al ratio were prepared by using proper amount of template, tetraethyl orthosilicate（TEOS）and water. The effect of preparation parameters on the performance of the catalysts containing ZSM-5 was studied by XRD，SEM，NH3-TPD，BET techniques and MTP test. The optimal conditions for synthesis of ZSM-5 zeolite are: n(TPA+)/n(SiO2) of 0.16-0.18，H2O/SiO2 mass ration of 14-16, Si/Al ratio of 500 and crystallization temperature of 130～150 ℃. The catalysts containing ZSM-5 were obtained by extrusion, acid exchange and calcination, and evaluated for MTP. The results indicate that the catalyst containing ZSM-5 with Si/Al ratio of 500 has a good performance of MTP. The methanol conversion is higher than 99%, and the propylene selectivity can be maintained at about 45%.

STUDY OF PHOTOCATALYTIC OXIDATION DESULFURIZATION OF THIOPHENE WITH TiO2/SBA-15

2015, 46(4):  51-54. 

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TiO2/SBA-15 photocatalysts were synthesized by impregnation method using tetra-n-butyl titanate (TnBT) as titanium source. The properties of the catalyst were characterized by XRD and BET. The results show that TiO2/SBA-15 catalyst keeps the structure of the support SBA-15. The photocatalytic oxidative desulfurization performance of the catalyst was investigated using thiophene isooctane solution as a simulated oil and H2O2 as an oxidant under UV light irradiation. The process conditions of the reaction were determined by static experiment. The optimum reaction conditions are as follows: 50 ℃，120 min, catalyst dosage of 2 g/L(feed), the O/S molar ratio of 8.5:1. Under the conditions, the desulfurizition rate of simulated oil is up to 88.2%, indicating that TiO2/SBA-15 has a good performance of photocatalytic oxidation desulfurization.

COAL TAR HYDROCRACKING OF ZEOLITE-CONTAINING CATALYST PREPARED BY TUNGSTEN FROM DIFFERENT SOURCES AND MODIFIED BY PHOSPHORUS

2015, 46(4):  55-61. 

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Ni-W hydrocracking catalysts were prepared by co-impregnation method on the carrier consisted of ZSM-5, USY zeolites and Al2O3 using ammonium metatungstate and phosphotungstic acid as tungsten source, respectively and then modified by phosphorus. The catalysts were characterized by BET, NH3-TPD, Py-IR, XRD, XPS and HRTEM techniques. The hydrocracking performance of the catalysts was evaluated in a fixed-bed reactor, using a hydrotreated diesel fraction obtained from middle/low-temperature coal coking process. The catalyst using phosphotungstic acid as tungsten source exhibits a higher sulfidation degree of W and Ni, resulting in higher hydrocracking activity. The total aromatics contents in the hydrocracked products are decreased by 7.06% and the total saturated hydrocarbon contents are increased by 6.70%, compared with the catalyst using ammonium metatungstate as tungsten source. The addition of phosphorus increases the strength of weak and moderate strong acid, improves the B acid ratio and the sulfidation level of W and Ni of the catalyst prepared using ammonium tungstate as tungsten source, thus enhances its hydrocracking activity. On the P modified catalyst, the total aromatics content in the hydrocracked products was decreased by 7.90% and the total saturated hydrocarbon contents are increased by 7.54%.

CAUSES OF DEACTIVATION OF CLAUS TAIL GAS HYDROGENATION CATALYST AND COUNTERMEASURES

2015, 46(4):  62-66. 

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The factors that affect the activity of hydrogenation catalyst for Claus tail gas from sulfur recycling unit in Quanzhou Petrochemical Co.，Ltd.，were analyzed in aspect of sulfur settlement, carbon deposition, hydrothermal ageing, sulfation, incomplete pre-sulfidation or sulfur loss, and channeling. The causes of catalyst deactivation and the countermeasures for maintaining catalyst activity were proposed. It is found that unreasonable design of the gas distributor is the main reason, which causes uneven gas distribution in hydrogenation reactor and the channel flow in the catalyst bed under high load operation due to the low bulk density of the hydrogenation catalyst. The measures of plugging partial openings of gas distributor and laying protective ball on the top of the catalyst bed can effectively suppress the channeling and stabilize the catalyst activity and operation under high load.

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DEVELOPMENT OF OIL-SOLUBLE VISCOSITY REDUCER FOR PIPELINE TRANSPORTATION OF SHENGLI HEAVY OIL

2015, 46(4):  67-71. 

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The heavy oil of Shengli oilfield has a high viscosity and is difficult to transport. A new type of oil-soluble viscosity reducer RPJN-SL is developed, which has a viscosity reduction rate (VRR) of more than 55% for Shengli heavy oil. The mechanism of the oil-soluble viscosity reducer （VR）is studied by dynamic light scattering and X-ray diffraction. The results show that the VR molecules interact with the aggregate micelle of asphaltene and resin to reduce the micelle size and the internal force between micelles so as to depress the viscosity of the heavy oil and reduce the order of the asphalt aggregate structure as well. The influencing factors studied show that the VRR rises with increasing the concentration of VR, and is not affected by temperature and shearing. The oil-soluble viscosity reducer RPJN-SL can fulfill the demands of pipeline transportation.

TRIBOLOGICAL PROPERTIES OF MERCAPTOBENZOTHIAZOLE ALCOHOL AS ADDITIVE IN RAPESEED OIL AND HYDROTREATED OIL

2015, 46(4):  72-77. 

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A lubricant additive 3-(benzo[d]thiazol-2-ylthio)-2-ethoxypropan-1-ol (TBE) was synthesized using fatty alcohol and a mercaptobenzothiazole as starting materials. The tribological properties of TBE alone and TBE/TBP (tributyl phosphate) composite additive in rapeseed oil (RSO) and hydrotreated base oil with 5Cst (5Cst) were investigated using a four-ball friction tester. The results show that the synthesized TBE has some tribological properties, and the response effect in RSO is better than in 5 cst. On the other hand, the addition of TBE and TBP simultaneously in base oil can get synergies. TBE/TBP has better extreme pressure, anti-wear and friction properties than the single additive, and the best mass ratio of TBE/TBP composite additive is 7:3 or 5:5. The response performance of TBE/TBP composite additive in RSO is also better than in 5Cst.

CONDUCTIVITY AND TRIBOLOGICAL PROPERTIES OF IONIC LIQUID AS GREASE ADDITIVES

2015, 46(4):  78-82. 

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New ionic liquids were prepared by the way of in-situ formation between lithium salts and polyether（PAG） and used as lubricating grease additives. The electricity compound grease was prepared by mixing PAO40 base oil with traditional or the new ionic liquid and a thickener polytetrafluoroethylene (PTFE). The conductivity and tribological properties of traditional ionic liquid and new ionic liquids as additives were studied. It is observed that the addition of additives reduces significantly the volume resistivity and contact resistance of the electricity compound grease, but the conductivity and that the scar width and the friction coefficient are both reduced, reflecting the excellent antifriction and anti-wear performance of the greases adding the additives. The improvement of tribological properties should attribute to the formation of the chemical reaction ?lm due to the reactions of anion of the additives with metal surface. The results demonstrate that the new ionic liquids which are easily prepared can significantly improve the electrical conductivity and tribological properties of the grease.

DEVELOPMENT OF ENVIRONMENTALLY FRIENDLY EMULSION FOR COLD-ROLLED SILICON STEEL AND ITS TRIBOLOGICAL PROPERTIES

Li Yan Sun Jianlin Chen Jingyue

2015, 46(4):  83-87. 

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Enviromentally-friendly silicon steel rolling emulsion with high lubricating property was developed using enviromentally friendly base oil and additives. The lubricating performance was analyzed by MRS-10A four-ball tester and 4-high cold-rolling mil and compared with the KD traditional emulsion. The results show that relative to the traditional KD emulsion, the developed cold-rolling emulsion shows a higher lubricating performance, a better annealing cleanliness, and that the minimum rolling thickness is decreased by 13.3%. After rolling, silicon steel strip shape and surface quality is more ideal. It is concluded that the developed enviromental emulsion can meet the need of the high speed silicon steel cold- rolling process .

CORROSION RESEARCH OF NAPHTHENIC ACID IN DISTILLATES OF SHENGLI HIGH ACID CRUDE

2015, 46(4):  88-92. 

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Naphthenic acid in the distillates of 200—350 ℃ and 350—450 ℃ in Shengli high acid crude oil were separated and purified through alkaline-ethanol extraction. The structures and compositions of naphthenic acids were confirmed by means of element analysis method, steam osmosis pressure，hydrogen nuclear magnetic resonance (NMR) spectroscopy, and Fourier transform infrared spectroscopy techniques. The corrosion of A20 carbon steel in the two distillates was conducted at different temperatures. The results show that naphthenic acid is monocarboxylic, and the average molecular formulas of naphthenic acid in the distillates of 200—350 ℃ and 350—450 ℃ are C15.86H27.51O2.06 and C32.86H54.77O2.29, respectively. The corrosion ability of naphthenic acid is not only related to acid content, but also closely related with its structure. As the fraction becomes heavier, the branching degree of petroleum acid molecule increases from 0.197 to 0.292, and the electron-withdrawing property of the group connected with carboxyl groups in acid reduces, and the acidity decreases, resulting in a lower corrosion rate of carbon steel. At the same time, a larger space steric hindrance in branched acid molecules would lower the corrosion ability of naphthenic acid. The corrosion rate is increased as temperatures go up and the corrosion ability of the small molecular naphthenic acid is stronger.

APPLICATION OF ENERGY SAVING ROSE TECHNOLOGY IN PROPANE DEASPHALTING PROCESS

2015, 46(4):  93-96. 

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The 800kt/a propane deasphalting unit of a petrochemical company adopts the ROSE technology to utilize the potential energy and thermal energy from the effluents with high temperature and pressure. The extraction column and supercritical separation tower use high efficiency structured packings. The heat transfer oil is used for heating. An innovative structure of the heater and a high efficiency energy saving burner are used. Using the same vacuum residue and propane solution, the comprehensive energy consumption of 800 kt/a propane deasphalting unit adopting ROSE technology is 21.7% lower than that of the comparative 250 kt/a unit.

CHARACTERIZATION OF SPENT RESIDUE HYDROPROCESSING CATALYST BY COMBINED SEM TECHNIQUES

2015, 46(4):  97-102. 

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Residue hydroprocessing catalysts are susceptible to deactivation. One of the causes is metal deposition. Combination utilization of dot, line, and mapping analysis of scanning electron microscope (SEM), second electron (SE) image, back scatted electron (BSE) image, and energy dispersive spectroscope (EDS) can not only qualitatively but also quantitatively analyze the metal deposition to understand the changes of the catalyst properties. The results show that the distribution of Ni is relatively uniform along the cross section of the deactivated catalyst, meanwhile, V and Fe mainly deposite on the outside of the catalyst. Along the flow direction, the amount of deposited Ni and V decrease. Most of the metal deposition is on the demetallization catalyst bed.

STUDY ON MOLECULAR COMPOSITIONS OF HYDROCRACKING PRODUCTS AND CHANGING REGULARITY WITH CONVERSION DEPTH

2015, 46(4):  103-109. 

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Gas chromatography/mass spectrometry (GC/MS) and gas chromatography/field ionization time of flight mass spectrometry (GC/FI - TOF MS) were used to analyze the molecular compositions of hydrocracking products. The composition properties of products and the changes of composition with conversion depth were investigated. The results show that the carbon number of normal paraffin is mainly between C18 and C40. With the conversion depth increasing, the iso-paraffin increases rapidly and the normal paraffin has little change. The contents and compositions of alkanes in the feedstocks have a significant influence on the BMCI value and cold- flow properties of the unconverted oil. The cyclo-paraffin hydrocarbon compounds in the whole distillate products, the mass fraction of monocycloalkane with the carbon number from C5 to C13 is the highest, compared with other cycloalkanes. One to three-ring cycloalkanes with carbon number of side-chain above 7 undergo an alkyl chain cracking and tend to be the cycloalkanes with lower side-chain carbon number. Aromatic hydrocarbons mainly distribute in the fractions below 350 ℃with alkylbenzene, indane and tetralone as main configulations, but little compounds exist in the form of benzene.