Table of Content

12 June 2017, Volume 48 Issue 6

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DEVELOPMENT AND APPLICATION OF HIGHLY ACTIVE ULTRA DEEP DIESEL HDS CATALYST RS-2100 AND RS-2200

2017, 48(6):  1-6. 

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Reactant-active phase Optimization & Cost-effective Key Technology，ROCKET, was created through the analysis of the key factors affecting catalyst activity and stability. The highly active RS-2100 (NiMo) and RS-2200 (CoMo) catalysts with a high cost performance ratio were developed based on ROCKET technology and characterized by high hydrodesulfurization (HDS) activity, excellent stability, low bulk density and low cost. Industrial application results show that the RS-2100 and RS-2200 catalysts are capable of long-term continuous and stable operation for production of ultra-low sulfur diesel (ULSD) meeting National V emission standard, indicating the strong market competitiveness of the catalysts.

EFFECT OF SUPPORTS ON PERFORMANCE OF SLURRY-BED COBALT-BASED F-T SYNTHESIS CATALYST

2017, 48(6):  7-13. 

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Cobalt-based catalysts supported on silica and alumina were prepared respectively and tested by a slurry-bed Fischer-Tropsch synthesis reactor. These catalysts were characterized by N2-physisorption, H2-TPR, CO chemisorption, XRD, SEM, pyridine adsorption infrared spectroscopy and reduction degree. The results show that the silica support with larger pore size and acid-free benefits the dispersion of Co, larger surface area and reduction degree of the catalysts, resulting in higher activity and C5+ selectivity. It is found that for silica support catalyst the larger the pore size, the larger the dispersion and surface area of metal Co; the weaker the acidity, the higher the C5+ selectivity. The results indicate that support does not affect the catalyst deactivation rate, but the initial reaction rate of silica catalyst is significantly higher than the alumina catalyst.

STUDY ON ACCESSIBILITY AND CATALYTIC ACTIVITY OF Y ZEOLITE MODIFIED BY Ce-SPECIES

2017, 48(6):  14-19. 

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Ce-NaY zeolites with different cerium content were prepared by liquid phase ion exchange. The micro structure, textual properties and total acid content of the Y zeolites containing Ce were characterized by XRD, N2 adsorption and NH3-TPD. The influence of cerium on the acidity was studied by in-situ FTIR and the acid accessibility index (AAI) of Y zeolites before and after Ce modification were determined by different probe molecules. The micro-activities (MAT) of NaY/Ce-NaY zeolites were evaluated using Dagang light diesel as test feed. The results indicate that the original cage constructions of Y zeolites did not change after modification of cerium, while the crystal particle of Ce-NaY zeolites became smaller, and the pore structure turned to be more developed. With the introduction of more cerium, the extra-framework alumina reduced and the dealumination was suppressed, the AAI of Lewis acid gradually reduced and Bronsted acid AAI significantly increased, the MAT of REY zeolite is related with Ce content. The introduction of suitable amount of Ce species is very beneficial to improve the acid catalytic activity of the sieves.

DEVELOPMENT AND APPLICATION OF LOW COKE AND EFFICIENT CONVERSION RFCC CATALYST

2017, 48(6):  20-24. 

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The catalytic cracking catalyst with low coke-making and high heavy oil conversion was prepared using new matrix material and acidity modification technology. The catalytic cracking catalyst was characterized by means of nitrogen adsorption/desorption and temperature-programmed desorption of ammonia (NH3-TPD) techniques. The catalytic cracking performance of the catalyst was evaluated in a FCC riser reactor. The results indicated that compared with the catalyst in using, the prepared catalyst had the advantages of higher surface area, mesoporous volume, lower strong acid sites and higher weak acid sites. Laboratory evaluation results showed that compared with the catalyst in using, the heavy oil yield and coke yield of the prepared catalyst decreased by 1.37 and 0.26 percentage points respectively. The industrial application results showed that the catalyst possessed the characteristics of strong heavy oil conversion ability and good coke selectivity.

REGENERATION PERFORMANCE OF C5/C6 ISOMERIZATION CATALYST NNI-1

2017, 48(6):  25-29. 

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The performance of NNI-1 Pd/molecular sieve catalyst applied in 0.2 Mt/a C5/C6 isomerization unit of SINOPEC Hainan Refining & Chemical Co. Ltd.，before and after regeneration was introduced. The NNI-1 catalyst was run for 3 periods and then regenerated ex-situ. The total time of operation for the first and second periods was 7 years. The inlet temperature of isomerization reactor was controlled under 250 ℃, while the temperature rise of catalyst bed was maintained in the range of 10-15 ℃; the RON of isomerized oil reached 78, 6 units higher than the feed; the C5 average isomerization ratio was 58.15%, and C6 average isomerization ratio was 73.32% with a 2,2-dimethylbutane selectivity of 14.78%. While at the EOR of the third period the RON increase of isomerized oil was less than 1 unit; the average isomerization ratio of C5 reduced to 43.96% and isomerization ratio of C6 was 51.42% with a 2,2-dimethylbutane selectivity of 2.42%, indicating that NNI-1 catalyst was no longer meet the needs of production. After regeneration ex-situ, the NNI-1 catalyst was run again for almost one year. In the case of high load operation, the inlet temperature of reactor maintained at 240 ℃, the temperature rise of reactor bed reached 18.7 ℃, the RON of isomerized oil recovered to 78, the average isomerization ratio of C5 recovered to 60.87% and C6 to 70.22% with the 2,2-dimethylbutane selectivity of 15.49%. The performance of the catalyst after regeneration indicates the well recovery in reactivity and stability meets the need of production.

STUDY ON REACTION RULES OF COMPOUNDS IN S Zorb PROCESS

2017, 48(6):  30-34. 

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The reaction rules of hydrocarbons, sulfides and nitrides in S Zorb process were studied. It is shown that some of the olefins are hydrogenated, small amount of hydrocarbon cracking reactions and denitrification reactions occur during desulfurization reactions in S Zorb process. When the FCC gasoline with olefin of 22.83% and sulfur of 325 μg/g is used to produce clean gasoline with sulfur content less than 10 μg/g by S Zorb process, the olefin saturation rate is 15.16%, the hydrocarbon cracking rate is 1.19%, and RON loss is less than 0.8. The removal rate for both mercaptan and thioether is close to 100%. 2-methyl thiophene and 3-methyl thiophene are the main residual sulfur compounds in refined gasoline. The aniline compounds in FCC gasoline are the primary nitrides. Its removal rate is 32.4% for this feed in S Zorb process.

PREPARATION OF BIODIESEL BY SUB/SUPERCRITICAL ALCOHOLYSIS

2017, 48(6):  35-38. 

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The sub/supercritical methanol were used for preparation of biodiesel fuel through alcoholysis of vegetable oils. The reaction conditions were optimized by orthogonal test. The influence of promoter on the transesterification reaction was investigated. The results show that the effect of reaction conditions without promoter on the yield of vegetable oil methyl ester has the following order: LHSV > temperature > alcohol/oil mole ratio > pressure. The addition of promote can significantly lower the reaction temperature and pressure and increase space velocity, and can produce the qualified biodiesel fuel in line with the national standared BD100（GB/T 20828-2007） under these mild conditions.

INFLUENCE OF DISTILLATION RANGE ON DISTRIBUTIONS AND PROPERTIES OF HYDROCRACKING PRODUCTS

2017, 48(6):  39-43. 

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Based on the composition analysis of the hydrocracking products with different distillation range, it is found that the aromatic hydrocarbons show a volcano type distribution and are mainly concentrated in the middle distillate; the yields of distillates are affected by changes of the cutting point moving forward or backward. The aromatic potential of heavy naphtha, cetane index of diesel decreases with IBP reduction, and the smoke point of jet fuel and BMCI value of tail oil increases, while the cracking performance of the tail oil has a little change. The effect of FBP increase on naphtha aromatic potential is not obvious, but the smoke point of jet fuel and cetane index of diesel increases greatly. It is concluded that the adjustment of distillation range of the product can highly optimize the compositions of hydrocracking products to response to market changes better.

EFFECT OF HYDROCRACKING TAIL OIL AS HYDROGEN DONOR ON COKING PRODUCT DISTRIBUTION

2017, 48(6):  44-48. 

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The capacities of hydrogen supply and hydrogen abstraction of hydrocracking tail oil and vacuum residue from CNOOC refining branch in Huizhou refinery were determined. The delayed coking laboratory and pilot plant test were performed using the residue and the residue with 10% hydrogen cracking tail oil. The pilot plant test results show that at the conditions of 500 ℃ and 0.15 MPa, compare with residue only, the total yield of naphtha, diesel and waxy oil increases 4.2 percentage points; the yield of coke and dry gas reduces 3.1 and 1.1 percentage points，respectively after the addition of hydrocracking tail oil as hydrogen donor.

MECHANISM OF WEAR FAILURE PROCESS OF SYMCHRONIZER

2017, 48(6):  49-53. 

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The gearbox synchronizer wear failure process using CF-4 15w/40 lube oil was investigated on the self-developed WS2001 synchronizer oil adaptability test bench. The failure mechanism was studied by analysis of the shift-characteristic curve, friction factor curve and the SEM figures of friction pairs before and after test. The results indicate that the shift-displacement goes up with the number of shifts, which leads to synchronizer failure because the shift block wears aggravate, making it difficult to press the sleeve with the cone. During the shift process, new contact surface appears continually due to friction of pairs, leading to a stable friction torque and moderate changes in the friction coefficient. However, in this process the stable oil membrane with enough strength cannot be formed on the surface of the friction pairs, causing wear of friction pairs. The surface of the test pieces has a large wear, the visible wear surface and curled asperities appear on the copper slider, the surface of the cone show scratches, and the synchronizing ring is worn and peeled.

ANALYSIS OF TECHNOLOGIES AND APPLICATION FOR INCEASING JET FUEL IN REFINERY

Yong-Lin LI

2017, 48(6):  54-60. 

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To increase jet fuel and reduce diesel production was the key to refinery to adapt to changes in domestic oil market by adjusting product structure and improving product quality and operation efficiency. Increasing the kerosene yield of CDU and hydrocracker was the main way to increase the production of jet fuel. However, the jet fuel production was limited by the yield of No.1 side-line of atmospheric distillation tower and hydrocracking products solutions. This paper analyzed the current bottlenecks in jet fuel production of refineries, described the technologies for maximum production of jet fuel from conventional hydrocracking and SR diesel hydrcracking. Meanwhile, the technology application effect was summarized. Based on the above analysis, some suggestions were suggested.

OPTIMIZATION OF S Zorb UNIT IN PLANT PLAN FOR NATIONAL V GASOLINE PRODUCTION

2017, 48(6):  61-64. 

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To produce national V gasoline, the optimum scheme for the plant around S Zorb device was conducted. Through the comprehensive analysis of the hydrogen balance, product distribution as well as octane number, the optimal sulfur content in S Zorb feed was determined, making the benefit increase 5.2 Yuan RMB per ton crude oil. By optimizing the operating parameters of the S Zorb gasoline stabilization tower and recycling part of LPG in winter, the octane number loss reduces by 0.3. After optimizing processing routs for dry gas of S Zorb unit, the benefit increases 240 Yuan RMB per ton dry gas.

INFLUENCE FACTORS ON WAX ODOR AND PROCESS IMPROVEMENT

2017, 48(6):  65-68. 

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Factors influencing the odor of petroleum wax product and the chemical compositions of the materials which give odor of waxes produced in SINOPEC Jinan Company were discussed. According to quantitative analysis results of volatiles and identification thresholds of odor materials, the toluene and cyclohexane are determined as the main compounds from ketone-benzol dewaxing process and lube oil hydrofining process, which cause the odor of wax. The steam stripping under vacuum condition technology for deodorization was adopted based on the experiments and theoretical analysis. By the process, fully refined wax product with the odor less than 1.0 can be stably produced.

TECHNIQUES OF HIGH AROMATIC ENVIRONMENTAL FRIENDLY RUBBER OIL DERIVED FROM NAPHTHENIC VACUUM 3rd LINE DISTILLATE

2017, 48(6):  69-73. 

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The environmental friendly rubber oil with high CA value was produced in pilot plant by a combined process of high pressure hydrofining and furfural refining. The CNOOC naphthenic vacuum 3rd line distillate was used as a raw material. The results indicate that the environmental friendly rubber oil with CA value of 12% can be produced directly through hydrogenation process. While the rubber oil with the CA value as high as 27.2% can be obtained with high yield (31.0%) by the combined process of first hydrofining followed by furfural refining. The by-product of the raffinate oil can be used as ordinary rubber oil directly to the market or as feed for production of SBS rubber filling oil and food grade white oil.

INFLUENCE OF PROCESSING ROUTE OF LCO ON DIESEL/GASOLINE RATIO

2017, 48(6):  74-78. 

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Some new ideas for optimal use of LCO for a grassroots refinery were proposed. According to the composition features as well as the complexity of desulfurization of different fractions, LCO is divided into three narrow fractions, i.e. LLCO (light fraction of LCO, < 260 ℃), MLCO (middle fraction of LCO，260-340 ℃) and HLCO (heavy fraction of LCO，>340 ℃). LLCO is pumped to low pressure diesel hydrotreating unit, while MLCO and HLCO, rich in PAHs (polycyclic aromatic hydrocarbons), are processed in hydrocracking unit and residue hydrodesulfurization unit, respectively, to produce reforming and FCC feed. Therefore, the yield of gasoline and aromatic product increases while diesel production decreases. The results show that for optimized scheme, the production of gasoline, PX and benzene increases by 415.6 kt/a, 33.3 kt/a and 14.7 kt/a, respectively, while that of diesel decreases by 774.0 kt/a, and the diesel/gasoline ratio reduces from 1.38 to 1.04. Meanwhile, the refining margins rise by 6.93 Yuan per ton crude, bringing remarkable economic benefit.

INDUSTRIAL APPLICATION OF EXPANSION BED-CATALYTIC DISTILLATION COMBINED PROCESS FOR LIGHT FCC GASOLINE ETHERIFICATION

2017, 48(6):  79-82. 

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A new process consisted of expansion bed-catalytic distillation series process (LNE-3) developed by PetroChina Lanzhou Petrochemical Research Center was applied to a 300 kt/a newly-built FCC light naphtha etherification unit in PetroChina Jilin Petrochemical Company. The industrial calibration results after running for 8 months showed that under full load operating conditions, the average conversion of tert-C5 and C6 olefins was 91.33% and 48.15%, respectively, the consumption of methanol was 3.21 t/h, the RON of etherified oil reached 98.5, the energy consumption was 1 107.878 MJ/t and the qualified etherified light gasoline was produced.

APPLICATION OF MIP TECHNOLOGY IN CATALYTIC CRACKING UNIT PROCESSING PARAFFIN FEEDSTOCKS

2017, 48(6):  83-87. 

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The revamping of FCCU followed by the application of MIP technology at Jilin Petrochemical Company was introduced. After revamping，the product distribution and gasoline properties are improved. The total liquid yield is increased by 0.3%, the olefin content in gasoline reduced by 5%. The RON increased by 1.6, up to 89, meeting the requirement for gasoline blending. Propylene content in LPG increased by over 3.0 percentage points. The properties of diesel and slurry become worse, indicating the effective use of hydrogen in the reaction process.

APPLICATION OF CERAMIC MEMBRANE FOR FILTRATING AND PURIFING SULFUR-CONTAINING SEWAGE FROM DELAYED COKING UNIT

Xue Tian zhang fuping

2017, 48(6):  88-92. 

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It is difficult to purify the sulfur-containing sewage of delayed coking unit using common technology. In response to this situation, a ceramic membrane with appropriate pore size was selected based on the particle size distribution of a refinery sulfur-containing sewage. A series of purification experimentations were done using single tube ceramic membrane. The filtration results show that the average size of the particle is above 0.5 μm and most of them are concentrated in the range of 20-250 μm. A ceramic membrane with filtering accuracy of 0.05 μm can meet the requirement, by which the average turbidity of sulfur-containing sewage from delayed coking is reduced by more than 99% after filtration and purification and the average oil removal rate is 96.51%, the permeability can be recovered to 0.3 mL/(m2?h?Pa). The industrial side line test shows that the average oil removal rate is more than 95%, solids content, such as coke powder, is less than 30 mg/L, and the turbidity reduced more than 98%. The purification device runs stably and the permeability recoveries well after regular cleaning.

SOOT DISPERSION PERFORMANCE OF HIGH - GRADE DIESEL ENGINE OIL

2017, 48(6):  93-97. 

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The soot sonication dispersion method for CJ-4 engine oil was established by simulation to relate the results of Mack T-11 engine test. The influence of different dosage ashless dispersants on the dispersion ability and shear stability was investigated. The results show that the ashless dispersants with different molecular structure have different dispersion abilities for soot dispersion. Good dispersion ability and shear stability can be observed at suitable dosage of the ashless dispersants and less influence on the oil shear ability is found. The CJ-4 diesel engine oil with the optimum amount of dispersant passes the Mack T-11 engine test.

REASONS OF INLET FILTER CLOGGING OF FCC SLURRY PUMP

2017, 48(6):  98-102. 

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Slurry pump is an important part of fluidized catalytic cracking (FCC) unit. The granularity of insoluble particles, pyrolysis behavior, morphology and elemental composition of the samples obtained from different positions in the FCC slurry pump in Shijiazhuang Company were characterized to investigate reasons that caused the clogging of the filter inlet of the slurry pump. Two kinds of cokes were found in the sludge deposition: small size coke powder and block particles. The results show that the small size coke in the sludge deposition of the pump inlet has a similar H/C atom ratio with the coke from coking unit, but significantly different from the coke blocks in the sludge, which is thought to be generated by FCC reaction, indicating that the small size coke powder in the sludge is the product of pyrolysis reactions of high temperature slurry. It is this coke powder produced due to the changes of operation conditions that causes the filter clogging.