Table of Content

12 February 2015, Volume 46 Issue 2

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DEVELOPMENT OF BLOCKAGE REMOVING AND INHIBITING AGENT FOR TAHE HEAVY OIL WELLS

2015, 46(2):  1-6. 

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Heavy oil well blockage occurs frequently in dilution exploration process in TAHE oilfield, which influences the production seriously. The SARA analysis of the blockage indicates that about 57% of it is asphaltene. This work investigates, based on the analysis, the solubility properties of the plug in different mediums and develops a new composite blockage removing and inhibiting agent RPDA-02. Its saturation solubility for the blockage is up to 2.0 g/g, much higher than the reference agents. The blockage inhibition performance of RPDA-02 shows that the inhibition time for asphaltene deposition is more than 60 days. The field test shows that temperature changes have little impact on the performance of RPDA-02. A continuous agent injection process is developed based on the conditions of the oilfield, which can well solve the problem of blocking and has no undesired effect on the subsequent processing of produced liquid.

STUDY ON HYDROTREATING REACTIVITY OF YICHANG RESIDUE II. CATALYST AND OPERATION CONDITIONS

2015, 46(2):  7-11. 

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Based on the characterization and hydrotreating reactivity of Yichang residue, a new hydrotreating catalyst for reduction of Conradson carbon residue (HDCCR) was developed by adopting Ni-Mo active metals and optimizing pore structure of the supports and adjusting the impregnation process, and adding promoter. The experimental results show that the residue hydrotreating layered catalyst system with the new HDCCR catalyst displays the higher HDCCR, HDS and HDN activities compared with the system with original HDCCR Co-Mo catalyst. Under the same reaction conditions, the Carbon residue reduced rate increases by 3.3%, HDN rate increases 7.9%. It is found that high reaction temperature, high hydrogen partial pressure and low volume space velocity improves HDCCR, HDS and HDN activities and thus improves the hydrotreated residue quality.

STUDY ON GASOLINE BLENDING COMPONENTS AND BLENDING FEATURES

2015, 46(2):  12-17. 

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Gasoline is a complex mixture of hydrocarbons composed by a variety of different monomer composition. Monomer hydrocarbon compositions of the main gasoline blending components in gasoline pool as well as alkylation gasoline alone are discussed. The octane number distribution of three gasoline blending components,i.e. S Zorb gasoline, reformate and alkylate, and the monomer hydrocarbons making a larger contribution to the octane number are also analyzed. The regularity of gasoline blending is analyzed in detail. It follows that the gasoline formulations with different monomer hydrocarbon composition can be made at the same octane number and total aromatic content. In addition, the gasoline with different boiling range can also be blended on the premise of equal vapor pressure.

STUDY ON BIOSURFACTANT PRODUCED BY PSEUDOMONAS SP. LKY-5 AND ITS STABILITY

2015, 46(2):  18-21. 

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The Pseudomonas sp. LKY-5 produces biosurfactant during biodegradation process of dibenzothiophene. This work optimizes the carbon sources for biosurfactant production, verifies the biosurfactant by thin-layer chromatography, and then determines its physicochemical properties, and investigates the influence of temperature, pH and inorganic ions on the active stability of biosurfactant. The results show that the biosurfactant produced is rhamnolipid, and peanut oil is the optimal carbon source for the production of biosurfactant with a yield of 0.15 g/L. The critical micelle concentration (CMC) and hydrophile-lipophile balance (HLB) value of biosurfactant are 180 mg/L and 12.3, respectively. Twenty-four hours diesel emulsification ability is 61%. The biosurfactant is stable at conditions of 30~80 °C, pH of 6~13, and can tolerate the environment of 200 g/L NaCl (or MgCl2) or 20 g/L CaCl2.

STUDY ON INFERIOR DIESEL HYDROTREATING AND HYDROCARBON GROUP COMPOSITION ANALYSIS OF NARROW FRACTIONS

2015, 46(2):  22-26. 

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The influence of hydrotreating temperature on the inferior FCC diesel oil was investigated at 12.0 MPa, volume space velocity of 0.5 h-1 and hydrogen to oil volume ratio of 800 in a three 300mL hydrogenation fixed bed in series. Raw material oil and the hydrotreated diesel oil were cut into narrow fractions, and the variation of hydrocarbon group compositions of the narrow fractions with distillation range was studied. The results show that at the optimum hydrotreating temperature of 370 ℃, the density of hydrotreated diesel is 0.865 1 g/cm3，the sulfur and the total aromatics content are 27.51 μg/g and 12.8%, respectively and the cetane index increases 15 points. Over 92% of bicyclic and tricyclic aromatic hydrocarbon of every narrow fraction is removed. It is found that most of single-ring aromatics and tricyclic naphthenic is concentrated in 285~350 ℃fraction range, which is required further hydro-upgrading to reduce the density and improve cetane number of inferior diesel oil.

SYNTHESIS AND DESULFURIZATION PROCESS WITH CHELATED IRON OF NEW COMPLEXING AGENT

2015, 46(2):  27-32. 

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A new complexing agent SG containing sulfonic group and carboxylic group is synthesized using chlorosulfonic acid and glutaric acid. The ternary complex iron desulfurization system is prepared with SG, EDTA, citric acid and Fe3+. In a continuous desulfurization device, the effect of liquid to feed gas ratio, running time and filler height on the desulfurization efficiency of the ternary system is studied. The effect of air flow rate, regeneration time and temperature on the regeneration for the ternary system is also investigated. The optimum desulfurization conditions are approached as follows: the liquid/feed gas ratio of 0.134, the packing height of 0.4 m, the temperature of 40℃ and pH of 8.0. In this case, the H2S content of the feed gas is reduced from 227.679 g/m3 to 0.011 g/m3, the removal rate is up to 99.99%. The regeneration rate is up to 93.24% at the optimum regeneration conditions: the air flow of 125 L/h, the regeneration time of 30 min, the regeneration temperature of 30 ℃ and pH of 8.0.

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EXPERIMENTAL STUDY ON DESULFURIZATION OF MTBE BY ALKALI WASHING AND EXTRACTIVE DISTILLATION

2015, 46(2):  33-37. 

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Methyl tert-butyl ether (MTBE) is an important high octane additive for the production of clean gasoline. It is necessary to reduce sulfur in MTBE to less than 10μg/g to meet increasingly stringent standard for motor gasoline. According to the weak acidity property of mercaptan, this work uses an alkali washing-extractive distillation combination process for MTBE desulfurization. The S content is reduced from 132.5 μg/g to 76.2 μg/g in alkali washing stage at conditions of NaOH of 28%, NaOH/MTBE mass ratio of 0.015, alkali washing temperature of 35℃, alkali washing time of 6s, separated temperature of 35℃, separation time of 5min. The MTBE after alkali washing then undergoes three-stage extraction distillation by DMF at 80℃, distillation time of 25min, solvent/oil mass ratio of 1.5. The results show that the sulfur content of MTBE can be further reduced to 8.7μg/g and the total liquid yield of the combined process is 99.64%. The solvent after six times regeneration recycle can still reduce the sulfur in feed to less than 10μg/g. The regeneration conditions are: N2 stripping with space velocity of 60h-1 at 100℃.

COMPOSITION AND ALKALINE WASH DECHLORINATION OF TIRE TOP LINE OIL

2015, 46(2):  38-42. 

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The distributions of hydrocarbon and non-hydrocarbon compounds as well as the method of dechlorination pretreatment of the tire top line oil were studied. The tire top line oil was accurately cut into 10 narrow fractions, then the elements, hydrocarbons, the main chloric components and the chlorine distributions in each narrow fraction were investigated by micro coulometry and GC-MS analysis. Alkali wash method was used for dechlorination pretreatment of the top line oil. The influence of reaction temperature, reaction time and NaOH solution to tire top line oil volume ratio was tested by orthogonal test. The results show that saturated hydrocarbon and chlorine content decreases along with the temperature rise of distillation range, while aromatics content decreases. The distribution of unsaturated hydrocarbon content is more uniform. The dechlorination rate is 59.70% at the optimized conditions: reaction temperature of 100 ℃, reaction time of 4 h, NaOH solution to tire top line oil volume ratio of 1.5:1.

STUDY ON SODIUM REMOVAL PROCESS AND MICROACTIVITY OF CATALYTIC CRACKING CATALYST

2015, 46(2):  43-48. 

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The effect of calcination temperature, washing times and ammonium salt concentration on the sodium content and the microactivity (MAT) of the catalytic catalyst was studied. The catalysts with different sodium content were prepared by using zeolites with different sodium content. The sodium oxide in the catalysts was removed by post-treatment of calcination and ammonium salt washing. The results reveal that the sodium contents of the catalysts remain stable with the increase of calcination temperature under the same washing conditions when the calcination temperature is lower than 450 ℃. The same results are also for the catalysts washed with different concentration of ammonium sulfate at fixed calcinations temperature. But twice calcinations and washing can reduce the sodium oxide content of the catalysts to the level of industry catalyst. Small changes of MAT are observed for the catalysts washed by ammonium salt and calcinated between 300℃ and 400℃. As the calcination temperature increases to 500 ℃ or even higher, both of specific surface area and activity are significantly decreased. An empirical formula between catalyst activity and sodium content is established for prediction of catalyst performance.

STUDY ON OXIDATIVE DESULFURIZATION OF SIMULATED OIL USING PHOSPHOTUNGSTIC ACID/SEMI-COKE AS CATALYST

2015, 46(2):  49-53. 

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Oxidative desulfurization of benzothiophene（BT，DBT and 4,6-DMDBT） in simulated oil was investigated using hydrogen peroxide as oxidant, Span60 as emulsifier, N-Methyl pyrrolidone as extractant and phosphotungstic acid/semi-coke (HPW/Sc) as catalyst. The catalysts of phosphotungstic acid (HPW)/semi-coke (Sc) were characterized by FTIR. The effect of HPW loading amount, reaction temperature, reaction time, and aromatics, olefins and nitrogen compounds on desulfurization rate was studied. The results show that the sulfur removal efficiency of DBT reaches above 99% using the catalyst with 30% HPW loading at the conditions of temperature of 60 ℃, reaction 60 min, amount of catalyst 1.0%, n(H2O2)/ n(S)=3, amount of Span60 emulsifier 0.36%，and the oxidative activity of the model sulfur compounds follows the order of DBT＞4,6-DMDBT＞BT. The benzene in the test oil can promote DBT desulfurization, while quinoline and cyclohexene inhibit the removal of DBT.

EFFECT OF PREPARATION METHOD OF COMPOSITE SUPPORT ON PHYSICOCHEMICAL PROPERTY OF HYDROCRACKING CATALYST

2015, 46(2):  54-57. 

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Using β，Y molecular sieve and amorphous silica alumina (ASA) as raw materials for composite support preparation, hydrocracking catalysts with composite supports prepared by different methods were made to see the effect of support on physicochemical properties. It is discovered that the surface area, pore volume and average pore size of the catalyst with composite support made in-situ are lower than that of the catalyst with mechanical mixed molecular sieve and ASA composite support. The conversion rate, naphtha selectivity and chemical raw material yield are lower than the latter at the conditions of 360 ℃，8.0 MPa，LHSV of 2.0 h-1 and H2/oil of 1000 using hydrotreated Daqing VGO as feed , but higher liquid yield than the latter.

PERFORMANCE OF METHANOL AROMATIZATION ON NICKEL MODIFIED HZSM-5 CATALYSTS

2015, 46(2):  58-63. 

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The performance of modified HZSM-5 catalysts with different loadings of nickel on the aromatization of methanol was investigated in a continuous fixed bed microreactor using pure methanol as raw material. The catalysts were characterized by BET, XRD, Py-FTIR, and NH3-TPD techniques. Results show that the introduction of nickel species results in the formation of new Lewis acid sites. Furthermore, the total acid amount of the HZSM-5 catalyst increases gradually, especially the weak acid, with increasing amount of nickel. The total aromatic yield decreases first and then increases, followed by decrease again with the Ni loading. The introduction of nickel species may change the path from the hydrogen transfer aromatization to the dehydrogenation aromatization. In addition, aromatic hydrocarbons generated are mainly C7~C9 aromatics, while C6 and C10+ aromatics are relatively few. Meanwhile, by-products such as methane and COx increase gradually with the increase of nickel loading, which is probably in correlation with the enhancement of methylation of methanol caused by nickel species.

DIFFUSIVITY BEHAVIOR OF HEAVY OIL IN MODEL CATALYSTS

2015, 46(2):  64-70. 

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Using F127 as template agent, tetraethyl orthosilicate as silicon source, a series of mesoporeous silica FDU-12s as model catalysts were synthesized under different conditions for investigation of diffusivity of asphaltene. The catalysts were characterized by BET，XRD，TEM，SEM techniques. The influence of assemble temperature and crystallization temperature on the pore size of the materials was investigated. The diffusivities of asphaltene in the catalysts with different pore size were studied. The results show that rising the crystallization temperature can only enlarge the pore mouth size of FDU-12 molecular sieves without the increase of cage diameter, while lowering the assemble temperature has a opposite effect. Increase of entrance pore size and cage size of FDU-12 enhances the effective diffusivity; however, the decrease of specific surface due to excessive increase of pore size can reduce effective diffusivity.

ANALYSIS OF COMMERCIAL APPLICATION AND FLEXIBILITY OF DCC-PLUS PROCESS

2015, 46(2):  71-75. 

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On the basis of DCC technology, CNOOC Dongfang Petrochemical Co., Ltd. has adopted the DCC-plus technology developed by RIPP for increasing propylene yield and decreasing dry gas and coke yields since Feb. 2014. To meet the actual production requirements, adjustment and improvement are conducted on the original designed DCC-plus unit for olefin production to produce more gasoline and diesel. The commercial results indicate that the total liquid yield of DCC-plus unit reaches 82.23%, and the propylene yield is 8.07% under the moderate operation condition using atmosphere residue of the mixed Lufeng / Weizhou crude oil as feedstock, and the commercial performance shows that DCC-plus process has a good flexibility of product slate.

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EFFECT OF ONLINE DECOKING TECHNOLOGY ON LONG-TERM OPERATION OF COKING FURNACE

2015, 46(2):  76-78. 

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Urumqi petrochemical Co.,CNPC adopts the online decoking technology for its 1.2 Mt/a delayed coking device. This text introduces the situation of heating furnace. The online decoking technology prolongs the furnace running time, but has some adverse effect on the heating furnace, such as thermocouple falling off, tube surface oxidation peeling, tube entrance capebolt loosing，heating furnace outlet flange bolt fatigue. Some suggestions are proposed to solve these damages.

SYNTHESIS AND PROPERTIES OF LIQUID SULFUR-CONTAINING PHENOL ESTER ANTIOXIDANT

2015, 46(2):  79-83. 

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A liquid sulfur-containing phenol ester antioxidant (KY505) was synthesized by transesterification of methyl 3-(3,5-di-ter-butyl-4-hydroxyphenyl) propionate and 2-(phenylthio ) ethanol. The structure of the product was analyzed by IR and NMR. Then the solubility and anti-oxidation performance of the product was inspected. The results indicate that the antioxidant ability of KY505 is outstanding, and the oil solubility of KY505 is better. The oxidation induction period increases by more than 50%, compared with antioxidants, like hindered phenol type, phenol ester type and thio-phenyl type antioxidant.

REGENERATION OF WASTE LUBRICATING-OIL BY EXTRACTION-FLOCCULATION

2015, 46(2):  84-88. 

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By extraction-flocculation combined process, the regeneration of spent lube oil was investigated using cyclohexane-isopropanol mixed solvent as extraction agent and KOH solution as flocculant. The base oil fractions in the feed were recovered at the optimal process conditions: cyclohexane to isopropanol ratio of 1:2, KOH solution concentration of 15%, KOH solution to organic solvents ratio of 7:1, solvent to oil ratio of 2:1, refining temperature of 45℃, refining time of 30 min, and the base oil yield is 83.4％. The regenerated lubricating oil is clear light yellow in color, the viscosities at 40℃ and 100℃ are 17.58 mm2/s and 4.11 mm2/s, respectively. The base oil has the viscosity index of 139, the acid value of 0.023 4 mgKOH/g, flash point of 234 ℃, and the solidifying point of -17 ℃. The performance index of the reclaimed oil is dramatically improved.

STUDY ON GASSIMG TENDENCY OF TRANSFORMER OIL WITH DIFFERENT HYDROCARBEN COMPOSITIONS IN ELECTRICAL FIELD

2015, 46(2):  89-94. 

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Gassing tendency of transformer oil with different hydrocarbon compositions in AC, DC electrical field or AC/DC mixed electrical field are investigated according to the standard at home and abroad. The influence of additives on gassing tendency of transformer oils was observed at the same time. The results show that the aromatics content is the key factor, which decide gassing or absorbing gas of transformer oil. At the same temperature and electric field strength, the tendency of gassing or absorbing gas of oils in AC electric field is the largest, the AC and DC mixed electric field takes the second，and the smallest value of gassing or absorbing gas is in the DC electric field. The use of additives has no obvious effect on gassing tendency of oils in specified dosage range.

NUMERICAL STUDY OF PARTICLE-WALL ADHESION AND DEPOSITION IN DISCHARGE CONE OF CYCLONE TUBE

2015, 46(2):  95-101. 

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Based on theory and numerical simulation, a particle-wall adhesion model in vane cyclone tube was established to study the effect of throughput, temperature, particle concentration in gas feed and particle size on particle-wall adhesion in the discharge cone. Investigation shows that the shear velocity of flow near the wall is the critical factor for particle adhesion. With increasing the rate of feed, shear velocity of the gaseous flow near the wall increases greatly and the concentration of particles close to the wall rises, leading to more particle-wall adhesion. Operation parameters and solid properties affect the particle-wall adhesion. The influence of operation temperature is mainly through changing the Young modulus of particles, which declines significantly with operation temperature rising, resulting in more adhesion. Besides, the higher the particle concentration, the more collision and discharge cone scaling will occur. Particles of diameters between 1 μm and 10 μm are apt to deposit on discharge cone due to stay for a long time.

PREDICTION OF MPUITY CONTENT IN DEASPHALTED OIL OF TAHE ATMOSPHERIC RESIDUE BY COLUMN CHROMATOGRAPHY

2015, 46(2):  102-108. 

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Tahe crude oil is a heavy crude oil with high content of asphaltene, carbon residue, metal and high acid value. The corrosion of Tahe crude oil was investigated by the weight loss of hanging slice method. Tahe atmospheric residue after flashing was directly used as the solvent deasphalting raw material in this work. Tahe atmospheric residue was separated into six fractions and the structure parameters of the six fractions were calculated by the modified Brown-Ladner method. The results indicate that 53.89% of sulfur, 86.97% of nitrogen and more than 98% of Ni and V metals exist in resin and asphaltene. With the deterioration of the fractions, fA increases, while H/C, fN and HAU/CA decrease. There is a good correlation between the impurity removal rate under different chromatographic effluent yield and the results of solvent deasphalting process in pilot plant, indicating that the chromatographic separation method can be used to predict the impurity content of deasphalted oil with different yield of deasphalting process and to guide the solvent deasphalting process.