PETROLEUM PROCESSING AND PETROCHEMICALS

ORTHOGONAL EXPERIMENT OF ALUMINUM HYDROXIDE PREPARATION BY HYDROLYSIS OF ALKOXIDES

2016, 47(11): 1-7.

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Aluminum alkoxide hydrolysis is one of the main methods for preparing high purity aluminum hydroxide. Aluminum hydroxide was prepared from n-pentanol aluminum alkoxide by hydrolysis and the effect of the process parameters (hydrolysis temperature, hydrolysis time, molar ratio of water to aluminum alkoxide, aging temperature and time) on the crystalline size, surface area and pore volume of aluminum hydroxide was investigated by orthogonal experiment. The mechanism of the process was discussed. The results show that aging temperature is the most important factor affecting aluminum hydroxide crystalline size and specific surface area; hydrolysis temperature is the most important factor affecting the pore volume and also has a significant effect on the specific surface area and crystalline size. It is considered that the aging process can promote the growth of crystallite, and the hydrolysis temperatures determine the crystalline phase of aluminum hydroxide.

CONTRLLABLE PREPARATION OF Fe3O4 MICROSPHERES AND THEIR APPLICATION IN LOWER OLEFINS SYNTHESIS FROM SYNGAS

2016, 47(11): 8-13.

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A series of Fe3O4 microspheres with controllable structures was prepared from ferric chloride by solvothermal reaction method with different preparation parameters (solvothermal reaction times, types of alcohols and carboxylate) and characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) and H2-TPR, separately to investigate the size of primary grains and secondary particles, their surface areas as well as reducibilities. The results indicate that by adjusting the preparation parameters, the size of primary grain can be controlled in the range of 5.6-25.1 nm, while the particle size of microspheres is in the range of 149-503 nm. With the decrease of grain size, the surface area of Fe3O4 microspheres increases and the reducibility is improved. It is found based on the test results of syngas to olefins that the decrease of the grain size increases the selectivity of lower olefins and decreases the CO2 selectivity. While the decrease of the microscopes particle sizes is favorable to improve CO conversion.

OLIGOMERIZATION OF 1-DECENE WITH DIFFERENT STRUCTURE METALLOCENE CATALYSTS

2016, 47(11): 14-19.

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The oligomerization of 1-decene was catalyzed by metallocene catalysts with different structures and the effect of conditions on 1-decene oligomerization reaction and properties of oligomers were invesgated as well. It is found that the structure of metallocene catalysts affects the catalytic behavior and the distribution of oligomer components significantly. The unbridged metallocene catalysts, sterically hindered metallocene catalysts, constrained geometry configuration metallocene catalysts, and silicon-bridged binuclear metallocene catalysts mainly produce low viscosity oligomers (kinematic viscosity at 100 ℃: 2-5 mm2/s) with dimer content more than 50%); it is interested to find that Cs symmetrical metallocene catalysts show a higher activity and primarily produce medium-high viscosity oligomers (kinematic viscosity at 100 ℃ >30 mm2/s). The GC-MS results demonstrate that the oligomer mixture is composed of dimer to pentamer.

EFFECT OF DIFFERENT VANADIUM SOURCE ON Y ZEOLITE STRUCTURE

2016, 47(11): 20-24.

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The contaminations of Y zeolite by vanadium from different sources were conducted using ammonium metavanadate, vanadyl-naphthenate and vanadium pentoxide, respectively. The contaminented Y zeolites were than hydrothermally treated and investigated to see the destruction extent of treated Y zeolites. Results show that vanadium from different source has a different impact on Y zeolite structure. At the same vanadium content and hydrothermal treatment, the destroyed extent of Y zeolites is: vanadyl-naphthenate > ammonium metavanadate > vanadium pentoxide. This illustrates that for vanadium contamination experiment, the V source and contaminating way must be exactly the same. The results also indicate that the hydrothermal treatment is the most important factor affecting Y zeolite crystlinity. After hydrothermal treatment at 800 ℃, the mullite crystal phase was observed, without the formation of AlVO4, and REVO4 is generated in the case of REY. The V2O5 destroys the Y zeolite structure in a non-stoichiometric manner.

SYNTHESIS OF ZSM-5 WITH LAMELLAR MORPHOLOGY BY SOLID-LIKE PHASE METHOD

2016, 47(11): 25-30.

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ZSM-5 zeolite with lamellar morphology was synthesized by solid-like phase method at H2O/SiO2 molar ratio of 0.5-1.0. The uniform mixing for solid and solution was realized using high pressure spray-adsorption method and the influence of the synthetic conditions on the properties of prepared ZSM-5 were investigated as well. This synthetic method solved the problem in low water content system where the solid and liquid were hard to mix uniformly. The results show that the ZSM-5 grain is in the form of irregular, rough and lamellar morphology. The synthesized ZSM-5 with a hierarchical pore structure has a surface area 405 m2/g and a pore volume of 0.37 cm3/g. The ZSM-5 can be synthesized in the 0.03-0.13 Na2O/SiO2 ratio range. The crystallinity reaches to 112% at the P/SiO2 ratio of 0.036 and the crystallization time of 20 h. It is found that water is in the form of vapor and has a function of heat transfer during the synthesis process. The synthesized ZSM-5 has an outstanding hydroisomerization performance for diesel isodewaxing. The diesel yield reaches to 95.50 % with a condensation point of -35 ℃.

EFFECT OF ACTIVE RECOVERY PROCESSING ON HYDROTREATING PERFORMANCE OF Mo-Ni/γ-Al2O3 REGENERATED CATALYST

2016, 47(11): 31-34.

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In order to investigate the effect of active recovery processing on industrial Mo-Ni/γ-Al2O3 regenerated catalysts, the Mo-Ni/γ-Al2O3 regenerated catalysts before and after active recovery treatment was characterized by BET, XRD, SEM, TPR, and TG techniques and the hydrotreating performance for diesel was evaluated in pilot plant. The results show that after active recovery treatment, the specific surface area and pore structure of the regenerated catalyst are increased. The metal dispersion is improved and the interaction strength is weakened, resulting in the reduction temperature 100 ℃ lower than the catalyst before treatment. The activity evaluation shows that after activation treatment, the activity of Mo-Ni/γ-Al2O3 regenerated catalyst is better than Mo-Ni/γ-Al2O3 without treatment at 10 ℃ lower reaction temperature, indicating the better performance of the active recovery treated catalyst.

STUDY OF FISCHER-TROPSCH SYSNTHESIS PERFORMANCE OF RFT-2 CATALYST IN FIXED-BED REACTOR

2016, 47(11): 35-40.

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The effect of reaction temperature, pressure, ratio of H2/CO in feedstock, gas hourly space velocity, pressure of steam drum and superficial gas velocity on the Fischer-Tropsch synthesis performance over the industrial production RFT-2 catalyst were investigated in a fixed-bed reactor. The results show that increasing temperature leads to an increase of activity. The high temperature region and the temperature peak in catalyst bed are enlarged. The sensitive degree in different temperature ranges is different. Increasing the pressure increases the activity and improves the selectivity. However the temperature gradient in catalyst bed becomes larger. The ratio of H2 to CO in feedstock affects mainly the catalyst activity and product distribution, while has a less impact on the temperature distribution of catalyst bed. The increase of gas hourly space velocity leads to a decrease of CO and H2 conversion rate, while the selectivity and temperature distribution of catalyst bed did not change significantly. It is found that adjusting the pressure of steam drum is a very effective and sensitive to control the temperature of catalyst bed and it influences the catalyst performance and temperature distribution significantly. The increase of superficial gas velocity can improve the radial heat transfer of catalyst bed and make the temperature distribution more uniform.

RESEARCH AND PRACTICE OF DIESEL QUALITY UPGRADING IN HAINAN REFINERY

2016, 47(11): 41-47.

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SINOPEC Hainan Petrochemical Company was designed to produce the national Ⅲ clean diesel. Due to the high proportion of FCC light cycle oil with very low cetane number in diesel pool, the existing diesel hydrotreating unit with a capacity of 2.0 Mt/a could not satisfy with the production of the national IV or national V diesel. By comparison, a flexible hydro-upgrading MHUG-Ⅱ process with separately feeding system developed by RIPP was selected and adopted for revamping the unit. The results show that the diesel in compliance with the specification of national Ⅳ(S is less than 50 μg/g，cetane number higher than 49) or the national V(S is less than 10 μg/g，cetane number higher than 51) is successfully produced after revamping from mixed feed of straight run gas oil and FCC light cycle oil under mild operating conditions.

DESIGN AND CONTROL OF REACTIVE ADSORPTION PROCESS FOR METHYL LAURATE PRODUCTION

2016, 47(11): 48-55.

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Heat integrated reactive separation process, which achieves thermal coupling between the reaction and separation processes, possesses the advantages of lower energy consumption and investment cost. In this study, a novel reactive absorption process was proposed for the methyl laurate synthesis by esterification of lauric acid. The steady-state models for reactive distillation and reactive absorption were established, respectively by the Aspen Plus simulator. The results show that significant energy saving of the reactive absorption process can be achieved, compared with the reactive distillation process. The investment cost of the reactive absorption process can also be reduced due to the use of only one column. Moreover, the dynamic performance of the reactive absorption process was investigated and a control structure was proposed. It is proved that the proposed control structure can handle the feed flow rate disturbance well, showing a good controllability of the reactive absorption process. Therefore, the reactive absorption process for synthesis of fatty acid ester with long chains is an attractive technology with development potential.

INVESTIGATION OF CARBON DIOXIDE AND METHANE REFORMING REACTION IN FLUE GAS SYSTEM

2016, 47(11): 56-61.

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The reforming of CO2, CH4, O2 and He mixture system to syngas was investigated in a continuous flowing fixed-bed reactor. The modified nickel catalysts supported on α-Al2O3 and γ-Al2O3, respectively were used in the reaction. It is found that the volume fraction of syngas obtained increased with the rise of temperature at 500 ℃ to 700 ℃, atmospheric pressure, and the 15% volume fraction of CO2 in feed gas. Compared with γ-Al2O3 supported catalyst, α-Al2O3 supported catalyst possesses a higher activity and selectivity. When α-Al2O3 supported catalyst was used, the presence of oxygen in feed gas promotes the production of syngas and the volume fractions of syngas increase as the volume fraction of O2 increases. Moreover, a lower volume ratio of CO2 to CH4 is conductive to the production of syngas and the conversion of CO2. α-Al2O3 supported catalyst possesses good regenerability. When the volume ratio of CO2 to CH4 is 3:：4 and the volume fraction of O2 is 2.5% in the feed gas, the volume fraction of syngas in product gas reaches 83.82% and the conversion of CO2 is up to 95.05% at atmospheric pressure and 700 ℃.

INFLUENCE OF TRACE IMPURITIES ON DEEP HYDRODESULFURIZATION OF DIESEL

2016, 47(11): 62-65.

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The influence of carbon monoxide (CO) in the gas phase and silicon (Si) in the liquid phase on diesel deep hydrodesulfurization was studied. The results show that CO inhibits the HDS performance of catalyst and with the increase of CO concentration; the inhibition increases and then gradually becomes mild. However, the inhibition of CO is reversible. The Si in liquid phase poisons the catalyst and shortens the catalyst lifetime. It is found that when the SiO2 deposition reaches 3.31%, the activity loss of catalyst is more than 10 ℃.

SYNTHESIS OF HIERARCHICALLY POROUS ZEOLITE FAU/ALUMINA COMPOSITES BY SECONDARY GROWTH ON SEEDED ALUMINA SUBSTRATES

2016, 47(11): 66-73.

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The trimodal porous structured hierarchical FAU/alumina composite (macro-pores/meso-pores/micro-pores) were hydrothermally synthesized using macro-mesoporous alumina monoliths as substrates by seeding and secondary growth method. The influences of supports with different physicochemical features and the seed gel assistant on the properties of the resultant composites were studied. The zeolite seed and composites were characterized by XRD, SEM, nitrogen adsorption-desorption isotherms and DTA/TG. The results show that the coverage of zeolite on monoliths was determined by both of the physicochemical features of the substrates and the chemical compositions of the seed suspension or secondary crystallization solution. After being seeded, the substrate of γ-Al2O3 was partially transformed into zeolite structure with the retainment of the original substrate morphology. The zeolite coverage on α-Al2O3 support is improved significantly by the assistant of seed gel.

DEVELOPMENT AND APPLICATION OF HEAVY AND HIGH ACIDIC CRUDE OIL COMPOSITE DEMULSIFIER

2016, 47(11): 74-78.

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