PETROLEUM PROCESSING AND PETROCHEMICALS

ANALYSIS OF COKE ON FIXED BED RESIDUE HYDROTREATING CATALYSTS

2016, 47(10): 1-5.

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The compositions and types of the coke deposited on commercial hydrodesulfurization (HDS) catalyst RMS-30 and hydrodemetallization catalyst RDM-32 run for 450 days in fixed bed residue hydrogenating unit were characterized by SEM-EDX, TG-MS, FT-IR, XRF, C and S elemental analysis. The results show that along the radial direction from the surface to the center, the coke content on both two catalysts is decreased gradually, especially HDS catalyst. HDS catalyst has more coke and less metal deposition than HDM catalyst. The content of soft coke on HDM catalyst is 56.68% of the total coke deposition, while most coke deposited on HDS catalyst is refractory coke, about 97.04% of the total coke deposition and no soft coke exists. Structure of coke has a significant difference between HDS catalyst and HDM catalyst. The coke on HDS catalyst has higher aromatic ring condensation degrees than HDM catalyst, so the coke on HDS catalyst is more difficult to converse.

STUDY OF HYDROCRACKING OF LIGHT CYCLE OIL OVER Ni-Mo-P/SSY-Beta-Al2O3 CATALYST

2016, 47(10): 6-10.

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Ni-Mo-P/SSY-Beta-Al2O3 hydrocracking catalyst was prepared by impregnation method using SSY and Beta zeolite as acid components and evaluated in a 100 mL fixed bed reactor using LCO from SINOPEC Qingdao Refining & Chemical Co. At the conditions of 8 MPa, H2/oil radio of 700:1, and Sv of 1.25 h-1 and 360 ℃ in hydrorefining zone, while space velocity of 1.5 h-1 and 400 ℃ in cracking zone, the diesel yield is 58.67 %, cetane number increases by 10 units, and the gasoline yield is about 34.74 % with RON of 91.37.

IN-SITU HYDROTHERMAL SYNTHESIS OF ZSM-5/CORDIERITE MONONLITH CATALYSTS AND THEIR CATALYTIC PERFORMANCE OF TOLUENE ALKYLATION WITH METHANOL

2016, 47(10): 11-16.

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ZSM-5/cordierite monolith catalysts were synthesized by in-situ hydrothermal method and characterized by X-ray diffraction (XRD), scanning electron microscope (SEM). The effects of the template dosage of tetra-propyl ammonium hydroxide (TPAOH), n(SiO2)/n(Al2O3) ratio and crystallization time on the growth of ZSM-5 on cordierite supporter were investigated and the performance of catalysts for alkylation of toluene and methanol was tested. The results reveals that different growth on the support are found for ZSM-5 zeolites with different Si/Al ratios, the above factors can effectively control the growth of ZSM-5 zeolites on cordierite surface. The load and crystal size of ZSM-5 on supporter surface can be adjusted effectively by the amount of TPAOH. Compared with the ZSM-5 powder samples, the toluene conversion on monolithic samples is lower but higher in selectivity of para-xylene. With the increase of n(SiO2)/n(Al2O3) ratio in monolithic catalysts, the conversion of toluene reduces and xylene selectivity increases.

ALCOHOLYSIS REACTION OF VEGETABLE OIL CATALYZED BY Li-Ca-Zn-Al-O

2016, 47(10): 17-22.

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Using nitrates of lithium, calcium, zinc and aluminum as raw materials, urea as precipitating agent, the Li-Ca-Zn-Al-O composite oxide catalysts were prepared by precipitation-calcination method. Effect of preparation conditions on the catalytic activity for alcoholysis is investigated by single factor experiment. The optimal conditions for preparing the optimal catalyst are: the element ratio of n(Li):n(Ca):n(Zn):n(Al) =1:4:2:2, reaction temperature of 120 ℃, calcination temperature of 800 ℃, calcination time of 7.0 h. With Li-Ca-Zn-Al-O catalyst prepared under optimal conditions, the alcoholysis reaction of castor oil and methanol was tested at the conditions of n(methanol):n(castor)=9:1, m(catalyst):m(castor oil)=0.04:1, stirring speed of 550 r/min, reaction temperature of 65 ℃, reaction time of 3 h. The castor oil conversion is 91.9%. The optimal catalyst and its precursor were characterized by Hammett indicator method, TG, BET and XRD. The results show that the base strength of Li-Ca-Zn-Al-O composite oxide is in the range of 7.2-11.2, the weight of Li-Ca-Zn-Al with hydrotalcite-like structure is invariable when the calcination temperature is above 800 ℃, proven by TG analysis. The specific surface area of the optimal catalyst is 25.70 m2/g, the pore volume is 0.047 74 cm3/g, and is mainly composed of CaO and ZnO crystals.

PERFORMANCE COMPARISON OF LRC-99 AND LDO-75 CATALYST IN FCC UNIT OF NIGER REFINERY

2016, 47(10): 23-26.

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The performance of LRC-99 catalyst for increasing diesel and the LDO-75 catalyst for increasing gasoline in Niger refinery FCC unit was introduced. The results show that the LRC-99 catalyst increases the total yield of light oil by 0.68 percentage points (diesel yield increases 1.52 percentage points, gasoline reduces 0.84 percentage points), indicating the ability of increasing diesel production of the LRC-99 catalyst. It is found that LRC-99 also has stronger anti-wear and anti-pollution by heavy metal than LDO-75 catalyst. At Ni content of 22.55 μg/g in feed and 15000μg/g on equilibrium catalyst, FCC unit using LRC-99 catalyst still provides a better product distribution.

EFFECT OF PREPARATION FACTORS OF Pt/ZSM-22 CATALYST ON ITS HYDROISOMERIZATION

2016, 47(10): 27-31.

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The effect of Pt loading method, the pH of precursor solution and the Pt loading amount on hydroisomerization of Pt/ZSM-22-γ-Al2O3 was investigated for hydrocracking tail oil. The results show that the catalyst prepared by ion-exchange after support forming has the highest dispersion of Pt. The hydroisomerization selectivity and activity order is: ion-exchange after forming > molecular sieve ion-exchange > impregnation. When the pH of precursor solution of ion-exchange after forming is 9 and the Pt loading is 0.30%, the dispersion degree of Pt is 87.2%, the yield of 150N base oil with a pour point of -15℃ is 75.8%, and the hydroisomerization selectivity achieves the best.

CATALYTIC ACTIVITY OF Bi-Cu/C CATALYST FOR ACETYLENE HYDROCHLORINATION

2016, 47(10): 32-37.

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To develop a catalyst to substitute mercuric chloride for hydrochlorination of acetylene, a series of Bi-Cu/C catalysts was prepared by equivalent-volume impregnation and characterized by XRD, SEM and BET. Under the reaction conditions of 170 ℃, C2H2 gas hourly space velocity of 30 h-1, feed volume ratio V(HCl)/V(C2H2)=1.05, the catalytic performance of Bi-Cu/C catalysts was investigated in a fixed bed reactor at atmospheric pressure. The results show that the active components of Bi-Cu /C catalyst is highly dispersed on the surface of the carrier; after 20 h reaction, the activity of the best BiCl3-CuCl2/C catalyst is above 70%, the selectivity is higher than 99%. After PO43- modification, the activity and stability is significantly improved, the acetylene conversion rate is close to 98%, which achieves the activity of mercuric chloride for hydrochlorination of acetylene. Although the stability is not as good as mercuric chloride catalyst, it provides an experimental basis for further research and development of non-mercury catalyst for acetylene hydrochlorination.

STUDY ON CATALYTIC CRACKING OF HYDROTREATED LCO

2016, 47(10): 38-44.

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The catalytic cracking experiments of hydrotreated LCO (HLCO) were conducted in an ACE unit for Y zeolite, active meso-pore material and zeolites withβor MFI structure. The conversions of the components in the feed and the influence of conditions on the cracking reaction were investigated. The results show that the higher gasoline and C6-C9 aromatics yields are obtained by catalysts containing Y type zeolite with higher gasoline octane, but aromatics with double ring and multi-ring are generated simultaneously during the reaction process, which offset part of the benefit of hydrotreating process. The reaction temperature and catalyst to oil ratio has less influence on the HLCO conversion; the increase of reaction temperature has negative impact on gasoline yield, while catalyst to oil ratio has weak influence on it. The high reaction temperature promotes the generation of heavy product, but high catalyst to oil ratio is just opposite. The increase of both reaction temperature and catalyst to oil ratio raise the aromatics content of gasoline.

EFFECT OF CARBON DEPOSITION ON REGENERATED FCC CATALYST ON LIGHT HYDROCARBON CRACKING REACTION

2016, 47(10): 45-50.

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To reduce the yield of hydrogen, methane and coke in the secondary reaction of light hydrocarbon in FCC process for more low carbon olefins，the effect of reaction temperature and catalyst bed density on the catalytic cracking of light hydrocarbon and 2-methyl-2-butene on coked regenerated FCC catalyst was investigated in a small fixed-fluidized bed reactor. A series of coked catalysts with different carbon deposition was made by reaction of regenerated catalyst with heavy cycle oil (HCO) or atmospheric residue and used for catalytic cracking of light hydrocarbon test. The experiment results show that the yield of propylene rises with increasing reaction temperature and catalyst bed density, but the yield of hydrogen and methane increases rapidly at high temperature. The increase of catalyst bed density causes rapid growth of coke yield. Compared with the results on the regenerated catalyst, the total yields of hydrogen, methane and coke on the coked catalyst significantly decrease and yield of propylene is almost unchanged. Even if the coked catalyst is recycled many times, the cracking activity for light hydrocarbon still remains stable. The performance of the coked catalyst obtained with HCO is better than the coked catalyst obtained with residue oil.

NUMERICAL SIMULATION OF TEMPERATURE DISTRIBUTION IN FOUR-LEAF SHAPE CATALYST BY MESHLESS METHOD

2016, 47(10): 51-55.

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Based on three-dimensional bulk of real four-leaf type hydrocracking catalyst, the meshfree calculation to solve the fourier partial differential equation for heat transmission was used to simulate the influence of external temperature fluctuation on the internal temperature distribution in the catalyst using industrial operating temperature and catalysts size as the boundary conditions. The analysis results show that the reactions in the catalyst do not occur under real isothermal surroundings. The maximum and average temperature increases in the cylindrical and four-leaf type catalyst as the increase of reaction heat release, space velocity, feed density, catalyst radius and length of the catalyst. Among them, the heat release and catalyst radius have much more influence. Even under ideal apparent isothermal reaction conditions, the non-isothermal area still exists in the two catalysts. When the operation conditions and catalyst size are the same, the four-leaf type catalyst has the highest internal temperature, while its average temperature and distribution are lower and better than cylindrical one.

EFFECT OF SILICA GEL PORE STUCTURE ON DIESEL DESULFURIZATION WITH STRONG OXIDATIVE ACIDS

2016, 47(10): 56-60.

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Using concentrated nitric acid, peroxyacetic acid, hypochlorous acid as oxidant and silica-gel with different pore structures as adsorbent, the silica gel loaded with acid oxidant was prepared by mixing and characterized by IR and N2 adsorption-desorption. The effects of silica gel pore structure on desulfurization of model diesel with 1 000 μg/g of 4,6-dimethyldibenzothiophene（4,6-DMDBT）by strong oxidative acids were investigated. The results show that the pore structure of silica gel hardly relates to the desulfurization efficiency for peroxyacetic acid. However, the pore size of the silica gel has great influence on the S removal for hypochlorous acid with relative larger molecular size. Both pore diameter and inner specific surface area affect the desulfurization efficiency significantly for concentrated nitric acid. No relations of oxidative products and silica gel pore structure are observed.

STUDY OF ANTICOKING AND INCREASING LIQUID YIELD BOOSTER IN DELAYED COKING

2016, 47(10): 61-65.

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The delayed coking reactions of Liaohe heavy oil was simulated in an autoclave reactor at 395 ℃，405 ℃, 415 ℃，460 ℃ and 500 ℃, respectively, with addition of different anticoking and increasing liquid yield boosters. With the best booster selected from above tests, the coking products gas, distillates and SARA of residue were analyzed. It is found that the addition of 0.5% booster I can reduce coke and methane in gas 0.78 percentage points and 14.96 percentage points, respectively. The yield of gasoline + diesel increases 3.0-4.5 percentage points，the amount of saturate+aromatics increases 1.86-2.38 percentage points, indicating the good functions of booster for anticoking and increasing liquid yield.

PROPERTIES OF ADSORPTION, DIFFUSION AND ACIDITY OF ALKALI TREATED ZSM-5 WITH HIERARCHICAL PORE STRUCTURE

2016, 47(10): 66-72.

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A series of hierarchical micro-meso-pore structure ZSM-5 zeolites were synthesized by NaOH treatment. The structural and acidity properties of as-synthesized zeolites were characterized by XRD, N2 adsorption, SEM, NH3-TPD, and Py-FTIR. The adsorption and diffusion performances of benzene on the treated ZSM-5 zeolites were investigated by an Intelligent Gravimetric Analyzer (IGA). The structure-activity relationship of hierarchical ZSM-5 zeolites was related with the mass transfer, adsorption sites, and acid amount. It is found that the structure of ZSM-5 zeolites is not changed by suitable alkali treatment except crystallinity. After alkali treatment, the meso and micro-porous structures are formed in the hierarchical ZSM-5 zeolites. The acidity of hierarchical ZSM-5 zeolites is improved, which produces more adsorption sites and thus increases the adsorption of benzene on the hierarchical ZSM-5. The adsorption performance of benzene on hierarchical ZSM-5 not only is correlated with the acidity, but also with pore structure of ZSM-5. As a result, the connectivity in the meso-porous ZSM-5 is improved with the increasing of meso-porous in hierarchical ZSM-5, which contributes to the adsorption of active sites and catalytic performance of the treated ZSM-5.

DESULFURIZATION PERFORMANCE OF GRADED MULTICOMPONENT ABSORBENTS FOR FCC Naphtha

2016, 47(10): 73-78.

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The adsorptive desulfurization properties for FCC gasoline of different metal modified molecular sieve adsorbents in grading form by static and dynamic technique were conducted using FCC gasoline as raw material to investigate the effect of adsorbents combination sequence and their ratio. The results indicate that the desulfurization rate of Al-Ti-SBA-15 adsorbent is at least 28% higher than that of the modified Y zeolites. While the CeY/NiY combination exhibits a good desulfurization performance. Its breakthrough curve appears a platform, which indicates a dynamic balance between adsorption and removal of various sulfides and a lower breakthrough rate. And the Cu (I) Y/NiY desulfurization performance ranks the second. The combination of CeY: NiY: Al-Ti-SBA-15 with 1:1:4 (mass ratio) is the best which has the slowest breakthrough rate.

INDUSTRIAL APPLICATION OF IHCC TECHNOLOGY FOR PROCESSING PARAFFINIC RESIDUE OIL

2016, 47(10): 79-83.

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The industrial application of IHCC technology for processing paraffinic residue in Huaian Qingjiang Petrochemical Co. Ltd. was introduced. The results show that comparing with FCC technology，the liquid yield is increased by 6.18 percentage points in the maximum light liquid product scheme; while the liquid yield is increased by 7.27 percentage points according to the maximum gasoline scheme. Upon using the IHCC technology, the olefins content and the octane number of gasoline are increased slightly, the STC of gasoline is decreased, the properties of LCO is improved significantly, and the zero slurry is realized

REVAMPING OF 0. 6 Mt/a JET FUEL HYDROGENATION UNIT AND RUNNING ANALYSIS

2016, 47(10): 84-90.

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Revamping of 0.6 Mt/a jet fuel hydrotreating unit was conducted to enlarge the capacity by adding a new reactor, using a high effective RSS-2 catalyst, and enhancing heater loading. After revamping and using the catalyst developed by SINOPEC Research Institute of Petroleum Processing for RHSS technology, the unit can produces 3# jet fuel at lower reaction temperature.

OPTIMIZATION AND TRANSFORMATION OF GAS FRACTIONATION UNIT BY APPLICATION OF HIGH EFFICIENT NEW TRAYS AND NEW TECHNOLOGIES

2016, 47(10): 91-93.

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This paper introduces the capacity expansion and optimization of the FCC gas fractionation unit of Daqing Refinery. The new high efficient trays, downcomer and other measures are adopted in the revamping. The transformation increases the capacity from 128.17 kt/a to 172.32 kt/a, and ensure the product quality. By using the top cycle oil from FCC unit as the hot source of the de-propane tower to heat the hot water instead of 1.0MPa steam, the comprehensive energy consumption of the unit is greatly reduced from 4303.7 MJ/t to 1634.4 MJ/t.

BLENDING OF NAPHTHA AND OPTIMIZATION

2016, 47(10): 94-98.

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