Table of Content

12 September 2014, Volume 45 Issue 9

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STUDY ON EFFECT OF ALKANE STRUCTURE ON HYDROISOMERIZATION SELECTIVITY

2014, 45(9):  1-4. 

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The hydroisomerization reactions of alkanes, single or mixed ones, with different structure on zeolite catalyst were studied. It is found that the chain lengths of alkanes have an obvious influence on the hydroisomerization selectivity of alkanes and that there is a mutual influence on isomerization reaction even between alkanes with different chain length and between normal and iso-alkanes. The data show that the longer the chain of the alkane, the more difficult to reduce the pour point of the alkane. The results indicate that long-chain n-alkanes can influence the reaction activity of the short-chain ones. The iso-alkanes in the mixed feed only influence the isomerization reactivity of the n-alkanes, but have an impact on the product distribution. At close conversion rate, the iso-product distribution of mixed material is more beneficial to reduce the pour point than that of the individual alkane.

STUDY ON DEACTIVATION KINETIC MODEL FOR RESIDUE HYDRODEMETALLIZATION CATALYST

2014, 45(9):  5-9. 

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The catalyst deactivation during the HDM process can be divided into 3 stages. Based on the operation data of vacuum residue hydrogenation in STRONG ebullated bed, a catalyst deactivation kinetic model was established and then verified. The results show that in the initial stage, the reaction temperature accelerates catalyst deactivation and in the mid-term operation the activity of catalyst mainly depends on metal deposition. The verification test proves that the model fits well with the experiment data, indicating the good reliability and accuracy of the model for residue HDM catalyst deactivation in ebullated bed.

STUDY ON GASOLINE ADSORPTIVE DESULFURIZATION OF RESIN-BASED MODIFIED SPHERICAL ACTIVATED CARBON

2014, 45(9):  10-15. 

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Strong acidic polystyrene-based cation exchange resin （D001）was used as carbonization precursor to prepare metal-loaded modified spherical activated carbons (SACs) for fuel adsorptive desulfurization. The modification procedures included metal loading through metallic cation exchange in metal-containg salt solutions (Cu2+，Ni2+，Fe3+ nitrates) , carbonized by calcinations followed by activation with CO2. TG, XRD, SEM and BET characterizations show that after carbonization and modification the SACs remain the spherical shape having large pore volume and specific surface area. The metallic particle disperses over the carbonized surface as the activated centers for adsorptive desulfurization. The desulfurization capacities of SACs were investigated by model gasoline (MG) composed of thiophene dissolved in cyclohexane. The results reveal that the effect of the type of metal loaded on adsorption capacity was the order Fe＞Ni＞Cu. The adsorption capacity decreases with temperature rising from 20 ℃ to 60 ℃. The first-order and second-order kinetic equations both fit the adsorption mass transfer process well. The SACs can be regenerated by ultrasonic ethanol solvent elution and heat treatment. After 3 times regeneration, the reactivated carbon still has a good adsorption capability of thiophene.

OXIDATIVE DESULFURIZATION OF FCC GASOLINE BY MOLYBDOPHOSPHATE-BASED IONIC LIQUID

Wang HaoJie He JianXun Zheng ShuanChen Zou Yu

2014, 45(9):  16-19. 

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An ionic liquid based on molybdophosphate was synthesized and tested for oxidative desulfurization of FCC gasoline. The effect of catalytic oxidation time, dosage of hydrogen peroxide, dosage of catalyst and reaction temperature on the model gasoline desulfurization was studied. Under the optimum process conditions obtained, the FCC gasoline desulfurization performance of the catalyst was investigated. The results show that When catalytic oxidation time of 90 min, reaction temperature of 60 ℃, n (catalyst)/n (S) = 0.04, n (H2O2)/n (S) = 4, simulated gasoline desulfurization rate can reach 91.6%. While for FCC gasoline, desulfurization rate can be 87.8% at the same conditions. The catalyst has a good cycle performance and the average desulfurization rate of four cycles is 84.9%.

FIELD TEST FOR VISCOSITY REDUCTION OF TAHE HEAVY OIL BY HYDROTHERMAL CATALYTIC MODIFICATION

2014, 45(9):  20-23. 

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The field test for viscosity reduction of Tahe TH12196 heavy oil by hydrothermal catalytic process was conducted in the pilot plant of Northwest Oilfield Company, Sinopec using a catalytic viscosity reducer developed by Research Institute of Petroleum Processing. The results show that the viscosity of Tahe oil is reduced by 54.5% after catalytic modification at the conditions of reaction time of 6h, 160℃ and the viscosity reducer dosage of 1.5%, 51.4% more than that of hydrothermal method, while similar to the results of laboratory. After the modification, the heavy components are decreased and the light ones are increased. The breakage of weaker chemical bond between molecules leads the composition changes of heavy oil, resulting in smaller aggregations and irreversible viscosity reduction.

EXPERIMENTAL STUDY ON STEAM GASIFICATION OF PETROLEUM COKE

2014, 45(9):  24-29. 

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In order to investigate the steam gasification characteristics of petroleum coke, the effect of coke particle size, water vapor flow rate, temperature, pressure and oxygen content on the steam gasification of coke was studied in a fixed bed gasification reactor. The results show that, when the petroleum coke particle size is smaller than 380 μm and more than 96 μm, and the steam flow rate is in a range of 0.85—4.60 g/min, the effect of internal and external diffusion on the steam gasification of petroleum coke reaction are essentially eliminated. On the premise of elimination of the influence of internal and external diffusion, the gasification reaction rate of petroleum coke presents the increased trend with the reaction temperature and pressure increasing. The influence of temperature on petroleum coke gasification rate is much larger. It is displayed that the content of H2 is decreased while the content of CO is increased. When oxygen is added to the reaction system, petroleum coke not only gives off heat with petroleum coke burning but also reacts with generated hydrogen and carbon monoxide, which has a huge influence on the reaction conditions and product distribution. Therefore, to ensure the gasification reaction quickly and efficiently, optimizing reaction conditions and developing supporting equipment are highly desirable.

COMPARISON OF COKING PROERTIES OF HEAVY PETROLUEM RAW MATERIALS

2014, 45(9):  30-35. 

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Based on the coking test of vacuum residue, FCC slurry and ethylene tar in domestic laboratory, the benefits of three kinds of raw oils processed by delayed coking were simulated. The results show that the benefits of unit decline in different degree when the vacuum residue oil blending with FCC slurry and ethylene tar are processed. However, the analysis shows that the benefit of refinery processing FCC slurry and ethylene tar is better than the two raw materials are directly sold as products. The reason lies in more low value common petroleum coke produced when FCC slurry oil and ethylene tar with vacuum residue oil are co-processed. By analyzing the compositions and structure of three raw oils, and coking mechanism, the feasibility of processing ethylene tar in industrial delayed coking unit is discussed. The ways and measures for production of high quality petroleum coke with ethylene tar are proposed.

EX-SITU REGENERATION OF KF-848 HYDROTREATING CATALYST AND COMMERCIAL APPLICATION

2014, 45(9):  36-39. 

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The ex-situ regeneration of KF-848 hydrotreating catalyst was conducted in Jiangsu Kechuang Petrochemical Co. Ltd. and commercial application of the regenerated catalyst in refinery of Liaoyang Petrochemical Company，CNPC was introduced. The performance of the catalyst in pilot plant and in industrial unit shows that the regenerated catalyst has a high activity of hydrodesulfurization, hydrodenitrogenation and aromatics hydrogenation. The activity of the regenerated catalyst reaches above 95% of fresh catalyst. It is proved that ex-situ regeneration technology is effective and successful. Compared with the performance of fresh KF-848 and before the shutdown, the average temperature of the reactor using the regenerated catalyst is lower by 7~10℃; the pressure drop is improved. The N content of the product is less than 10 mg/g.

PREPARATION，CHARACTERIZATION AND HYDRODENITROGENATION ACTIVITY OF Ni2P/TiO2-SiO2 CATALYST

2014, 45(9):  40-46. 

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TiO2-SiO2 composite support was prepared by sol-gel method，and the supported nickel phosphide catalysts, Ni2P/TiO2-SiO2，were prepared by incipient wetness impregnation and in situ H2 reduction method. The samples were characterized by N2 adsorption-desorption, XRD, TPR， NH3-TPD and FT-IR. Their hydrodenitrogenation (HDN) performance was evaluated in a continuous-flow fixed-bed reactor using quinoline as a model molecule to investigate the effect of the active component loading, Ni/P molar ratio and Ti/Si molar ratio. The results show that TiO2-SiO2 composite support has a larger specific surface area. The Ni2P/TiO2-SiO2 catalyst precursor has a better reducibility, which helps the formation of Ni2P phase. Ni2P phase appears for the Ni2P/TiO2-SiO2 catalyst at n(Ni)/n(P)≤1.0. The optimal HDN activity occurs for the Ni2P/TiO2-SiO2 with Ti/Si molar ratio of 1/2，Ni/P molar ratio of 1.0 and the loading of (NiO+P2O5) of 25%.

INFLUENCE OF REDUCTION TEMPERATURE ON CATALYTIC ACTIVITY AND MICROSTRUCTURE OF PD/C CATALYSTS PREPARED BY COLLOIDAL METHOD

2014, 45(9):  47-51. 

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A series of Pd/C catalysts for hydropurification of terephthalic acid were prepared using sol-gel process. The effect of reduction temperature on the microstructure and activity of the catalysts were investigated by means of SEM, TEM, EDS, physisorption, chemisorption and HPLC. The results show that the activity and dispersion of Pd sharply decreases with the increase of reduction temperature. The conversion ratio of 4-CBA is close to 100% at reduction temperature of 10℃ and the dispersion of Pd also reaches the highest. The Pd particles at this condition are fine and equally distributed with average size of about 6.45 nm. However, a lot of larger particles with size of 15-20 nm gather at the surface at reduction temperature of 30℃. The amount of Pd on the catalyst surface reduced at 30℃ is about five times the amounts of Pd on the surface reduced at 10℃. Higher temperature generally causes the breaking of hydrogen bond between polyoxyethylene group and water, leading to a great reduction of solubilization capacity, which further results in the growth of Pd grain and the decrease of activity of Pd/C catalysts because of increased collision probability of Pd colloids.

PREPARATION OF Cu(Ⅱ)-Ce(Ⅳ) BIMETAL ION-EXCHANGED 13X ZEOLITES AND THEIR DESULFURIZATION PERFORMANCE

2014, 45(9):  52-56. 

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Desulfurization adsorbents of Cu(Ⅱ)-Ce(Ⅳ) bimetal ion-exchanged 13X zeolites，and Cu(Ⅱ)/13X ion-exchanged and Ce(Ⅳ)/13X ion-exchanged were prepared, respectively. The prepared adsorbents were characterized by XRD and N2 adsorption-desorption. Desulfurization performance of the desulfurization adsorbents for dimethyl disulfide, dimethyl sulfide, and tert-butyl mercaptan was investigated. The results indicate that compared with results of the adsorbents before modification the specific surface area and total pore volume of the prepared desulfurization adsorbents decrease, while the average pore diameter and the number of mesopore increase. The Cu(Ⅱ)-Ce(Ⅳ) bimetal ion-exchanged 13X zeolites exhibit good desulfurization performance, better than the results of single metal-exchanged adsorbents Cu(Ⅱ)/13X and Ce(Ⅳ)/13X, due to the synergistic effect between the two cations. Regeneration performance of spent desulfurization adsorbents was investigated and the results demonstrate that the regenerated adsorbents have a perfect desulfurization performance, and the desulfurization rate of the adsorbents after first regeneration is 98% of the fresh adsorbents.

OXIDATIVE DESULFURIZATION OF FCC GASOLINE BY MOLYBDOPHOSPHATE-BASED IONIC LIQUID

2014, 45(9):  57-61. 

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A new high efficient heavy oil conversion catalyst A was developed and commercialized for a RFCC unit with a capacity of 3.5 Mt/a. The lab results showed that the slurry and coke yield reduced; the total liquid yield increased slightly and the propylene yield increased significantly. The commercial application results show that compared with the results of the original catalyst，using the feed with same properties, the metal content on the equilibrium catalyst decreases, propylene yield increases by 1.07 %, slurry yield lowers by 2.91% , RON of FCC gasoline increases by 0.59, the NOx concentration at CO incineration flue gas furnace outlet decreases slightly.

RELATIONS OF DEWAXED OIL COMPOSITION AND PERFORMANCE OF BASE OIL

2014, 45(9):  62-67. 

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To explore the relationship between the hydrocarbon compositions of dewaxed oil and viscosity index and yield of base oil，the lube latent content and MS characterization of the narrow VGO fractions of four crude oils were analyzed. It is found that the yield and viscosity indexes of P+N components and related group hydrocarbon compositions as well as the yields of light and intermediate aromatic hydrocarbons can well be predicted by analyzing the group compositions of the dewaxed oil. The findings can replace tedious column separation process of lube latent content analysis method to increase the probability of high-quality crude oil screening.

RAW MATERIAL SELECTION AND OPTIMIZATION FOR HIGH-QUALITY APIⅠ BASE OIL PRODUCTION

2014, 45(9):  68-71. 

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Based on the lab and unit operation data of raw materials for APIⅠbase oil production, the optimized solutions are suggested. The yield of high quality APIⅠbase oil is increased by selecting the raw material, independent transporting and processing, and reasonable mixed refining. The ratio of high quality API Ⅰ base oil in total base oil output of SINOPEC is also increased.

STUDY ON PERFORMANCE OF ELECTRIC BREAKDOWN OF TRANSFORMER OIL WITH DIFFERENT COMPOSITIONS IN DC FIELD

2014, 45(9):  72-77. 

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The breakdown characteristics of transformer oils in DC electric field are one of the key factors to decide the safe operation of equipment. In this paper, the breakdown voltages test methods of transformer oils at home and abroad are briefly introduced. In HVDC electric field, the relevance of electric field uniformity and breakdown voltage, and the performance of electric breakdown of transformer oils with different hydrocarbon compositions as well as the relations between types of aromatics and their content and breakdown characteristics in uneven DC field are investigated. The results show that in uneven electric field, breakdown voltage of transformer oils has a great correlation with their hydrocarbon composition. The higher the aromatic hydrocarbon content in transformer oil, the lower the breakdown voltages in positive and negative polarity. Under the same electrode gap, the negative polarity breakdown voltage is higher than the positive polarity breakdown voltage of transformer oils. The breakdown voltage of transformer oils increases in direct ratio with the increase of electrode gap. The content of polycyclic aromatic hydrocarbons is the key factor affecting DC breakdown voltage of transformer oil; while monocyclic aromatics do not negatively affect the DC breakdown voltage.

STUDY ON TRIBOLOGICAL PERFORMANCE OF LITHIUM GREASE USING ULTRAFINE SILICON MATERIAL (SI-AL TYPE) AS ADDITIVE

2014, 45(9):  78-84. 

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A four-ball friction tester was used to investigate the tribological properties of lithium base grease using ultrafine silicon material (Si-Al type) as additive. The steel ball wear surface was characterized by optical microscope, scanning electron microscope (SEM) and energy dispersive spectrometer. The results show that anti-wearing ability is improved significantly but no effect on the antifriction performance. Compared with base grease, when the Si-Al additive is 0.5%, the wear scar diameters are reduced 22.37%,48.97% at loading of 392 N and 588 N, respectively, indicating the best anti-wear effect. After surface modification, the Si-Al additive powder is easier to dissolve in oil, but the tribological performance of the modified powder did not significantly change. Results of SEM and EDX show that in the process of long wear, a lubricating film mainly composed of SiO2,Fe2O3,Al2O3 is formed on the wear surface which has more notable tribological properties.

MECHANISM OF BIOCHEMICAL EXCESS SLUDGE REDUCTION BY WET AIR OXIDATION

2014, 45(9):  85-89. 

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The improvement of sludge dewater ability is essential to the volume reduction of waste activated sludge (WAS). The wet air oxidation process is used for WAS degradation. It is found that the volatile suspended sludge is decomposed into small molecular organic compounds, such as soluble protein, carbohydrate, short-chain fatty acids and ammonia by wet air oxidation, which improves the sludge dewater ability significantly.

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ADVANCE IN ENHANCED EXCESS SLUDGE IN-SITU FERMENTATION AND ITS APPLICATION

Chao ZHANG

2014, 45(9):  90-94. 

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Biological treatment of wastewater produces lots of excess sludge, resulting in secondary pollution. Fermentation of excess sludge can produce short-chain fatty acids (SCFAs), which can be used as an additional carbon source of biological nutrient remover and is important to sludge reduction and wastewater treatment. Excess sludge can be treated by alkaline fermentation, surfactant fermentation, and co-fermentation with carbohydrate and so on to get fermented liquid rich in SCFAs without biological toxicity. Enhanced excess sludge fermentation in-situ produces SCFAs, 3 ~ 8 times more than the conventional fermentation technology. Enhanced fermentation of the excess sludge in situ and liquid reuse in right place can realize the comprehensive utilization of sludge in sewage plant and provide a new way of thinking for residual sludge treatment. This review introduces the technologies and the mechanism of enhanced excess sludge in-situ fermentation and summarizes the process parameters and application effect of fermentation liquid recycling.

COMPREHENSIVE TREATMENT TECHNOLOGY FOR ODOUR POLLUTION OF WASTE GAS IN REFINER Ⅰ.STUDY OF TREATMENT TECHNOLOGY FOR WASTE GAS FROM SOUR WATER TANK AND LIGHT PRODUCT TANK

2014, 45(9):  95-101. 

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Fugitive odor emission behavior from sour water tanks and product intermediate tanks were comprehensively monitored and evaluated in a typical refinery. The comprehensive measures including reducing emissions of exhaust gas in tanks area and the absorbing process by low temperature distillate oils followed by desulfurization are used. The main odor pollutant in the tanks area is hydrogen sulfide, methyl mercaptan, ethyl mercaptan and dimethyl disulfide as well as non-methane hydrocarbons (NMHC). It is found that the hydrogen sulfide concentration in sour water tank is 175—3.36×103 mg/m3, organic sulfur compound concentration is 112-1.39×103 mg/m3, NMHC concentration is（2.67-4.40）×105 mg/m3. After purified by absorbing processe of low temperature distillate oils and then desulfurization, hydrogen sulfide concentration can be below 1 mg/m3, and purification efficiency reaches up to 99.9%. The organic sulfur compound concentration is less than 0.6mg/m3, and purification efficiency is greater than 99.5%. NMHC concentration is lower than 2.35×104 mg/m3, and purification efficiency reached as high as 95.1%.

QUALITATIVE AND QUANTITATIVE ANALYSIS FOR INORGANIC ANIONS IN MDEA SOLUTION

2014, 45(9):  102-106. 

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The qualitative and quantitative inorganic anion analysis method by ion chromatography (IC) for MDEA solution was established. The multiple-step gradient model was affirmed being the best one to separate the inorganic ions in MDEA solution through comparison of different eluent patterns (such as degree model, step gradient model, multi-step gradient model). The quantitative external standard curves for analysis of F -, Cl -, Br -, NO3 -, SO4= anions in a mixed standard solution were established by multi-step gradient elution method, respectively. The linear correlation coefficients of above 5 inorganic anion concentration curves can reach more than 99% and the detection limit can be up to ≤10 g/L with high sensitivity. The results of repeatability and standard addition recovery tests show that the method has a high accuracy with the relative standard deviation less than 5% and the standard addition recovery rate between 95.9% ~105.6%. By the multi-step gradient elution method established, the concentrations of Cl -, NO3 -, SO4= inorganic anions in a MDEA solution used for a year or so are determined to be 1191.055, 3.155, 41.595 mg/L, respectively.