Table of Content

12 May 2015, Volume 46 Issue 5

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STUDY ON SIDE CHAINS OF AROMATICS IN TAHE VACUUM GAS OIL

2015, 46(5):  1-6. 

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In order to elucidate the characterization of side chains in aromatics of vacuum gas oil, Tahe VGO was separated into light, medium and heavy aromatic fractions according to the polarity, then the average composition of aromatics and the side chains were investigated by instruments and ruthenium ion catalyzed oxidation reaction. The results show that carbon number and average molecular weight of n-alkyl chain decrease, while the polycyclic aromatics, heteroatom aromatics increase from light to heavy aromatics. By analyzing the water phase and organic phase of ruthenium ion catalyzed oxidation reaction, it is found that about 80% of side chain of the three aromatics fractions is normal alkyl. The short side chain of C1~C7 is increased as fractions become heavier, but the amount of the side chain longer than C7 is on the contrary. In addition, most of isomerized alkyl side chains are the side chain with single methyl.

STUDY ON REFINING OF CAPROLACTAM FROM VAPOR-PHASE BECKMANN REARRANGEMENT REACTION OF CYCLOHEXANONE OXIME

2015, 46(5):  7-11. 

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The crude caprolactam was obtained by the vapor-phase Beckmann rearrangement. The product was successively refined by distillation, benzene dissolving, water extraction, ion exchange, hydrogenation and triple effect evaporation, similar to the liquid-phase Beckmann purification process. The changes of purity, UV number, color, volatile base number and potassium permanganate absorption values (PM) in each refining step were investigated. The results show that the purity of the refined product is up to 99.950%, PM and color meets the premium grade, the UV number and the volatile base value reaches the first class and the qualified class, respectively.

RESEARCH ON CATALYTIC CRACKING OF HIGH-NITROGEN CONTAINING FEEDSTOCKS

2015, 46(5):  12-18. 

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Column-chromatography and Soxhlet extraction methods were used to separate high-nitrogen feedstocks. The molecular structure and functional group of the isolated basic nitrogen compounds, non-basic nitrogen compounds and condensed aromatics were characterized by a Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) and GC-MS. The results show that the basic nitrogen compounds are mainly composed of acridines and cycloalkyl-acridines. Benzocarbazoles are of the most relative abundance in non-basic nitrogen compounds. The main polycyclic aromatics are three ring aromatics with short side chain. Based on coking mechanism of FCC process, two suitable processes were proposed for processing high-nitrogen feedstocks: the pretreatment-FCC combined process (physical improvement method) and the partition conversion process (chemical improvement method). The results of partition conversion process show that the conversion and gasoline yield increase 5.84 percentage points and 6.49 percentage points, respectively with improved product distribution.

PRODUCTION OF HEAVY TRAFFIC ASPHALT BY FURFURAL REFINING OF FCC SLURRY OIL

2015, 46(5):  19-22. 

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The FCC slurry from PetroChina Daqing Petrochemical Complex was extracted by furfural solvent at the ratio of solvent to oil slurry of 4:1, the catalyst powder after extraction was removed by filtration. The FCC slurry extract oil and raffinate oil were obtained by this extraction process. The properties of FCC slurry extract oils where different percentages of light components were distilled off via vacuum distillation and the quality of the mixed products of blending FCC slurry extract oil with different types of National Standard asphalt were investigated. As was shown by the results: after the light components were distilled off by vacuum distillation, the quality of FCC slurry extract oil(asphalt) could meet the requirement of National Standards of 70 #, 90 # asphalt; meanwhile the quality of the mixed products blending FCC slurry extract oil with the standard asphalt in different proportions are greatly improved either.

HYDROGEN SULFIDE REMOVAL BY Fe-BASED DEEP EUTECTIC SOLVENTS

2015, 46(5):  23-27. 

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Wet oxidation method can remove hydrogen sulfide and recover sulfur by-product and the desulfurizer can be recycled. The ferric salt in deep eutectic solvent was used as oxidant for removing hydrogen sulfide. The effect of different reaction conditions on the desulfurization is investigated. The results show that the suitable concentration of Fe(NO3)3?9H2O is the necessary requirement for high efficiency desulfurization, and the ionic liquid system is the main factor influencing the desulphurization rate. Under the conditions of certain eutectic solvent, the desulfurization efficiency is mainly affected by inlet flow rate of hydrogen sulfide gas. The product is of monoclinic sulfur.

KEY TECHNOLOGIES TO PROLONG RUNNING PERIOD OF GAS OIL PRE-HYDROTREATING UNIT AND INDUSTRIAL APPLICATION

2015, 46(5):  28-33. 

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Based on the analysis of RVHT technology industrial experience, key technologies were proposed to prolong running period of gas oil pre-hydrotreating unit. Analysis results showed that the key technologies to extend the period included management of feedstock, optimum of process parameters, good catalyst properties as well as proper catalyst combination. The industrial application data indicated that the RVHT technology with its matching catalysts had a good adaptability to inferior gas oils, such as HVGO, CGO and DAO. Meanwhile the technology showed good performance in product quality and operation stability. Low deactivation rate of the catalysts also contributed to the long-term operation.

STUDY ON HYDROTREATING OF VGO BLENDING WITH VACUUM RESIDUE

2015, 46(5):  34-38. 

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To widen the sources of FCC feedstocks and upgrade residue, the two step hydrotreating process (DVHT) of VGO blending with vacuum residue (VR) was studied in pilot plant. The VGO blended with VR directly as feed (one step process) was taken as the reference. The effect of VGO/VR mass ratio on the impurity removal activity and catalyst stability for both processes were investigated. The results show that the product of DVHT process are characterized by lower sulfur, lower nitrogen, but higher content of hydrogen, metal, and carbon residue. It is better to adopt DVHT scheme for high-sulfur VGO feedstock. With increase of VR blending ratio, the removal rates of sulfur, nitrogen, carbon residue and metal decrease rapidly. The VR blending ratio gives the largest influence on removal of HDN and HDCCR, and the influence on HDM takes the second place, while the influence on HDS is the smallest. The 4000 h stability test indicates that the VR blending ratio has a great influence on the activity stability of the catalysts and that the VR blending ratio lower than 15% is appropriate for high-asphaltene residue.

C5, C6 ISOMERIZATION UNIT UPGRADE TECHNOLOGY

2015, 46(5):  39-44. 

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Zhanjiang Dongxing Petroleum Refinery Ltd. SINOPEC adopted a “de-isopentane tower+ isomerization reaction” process to produce C5, C6 isomerization gasoline with RON 82 using moderate temperature zeolite-based C5,C6isomerization catalyst developed by RIPP. In order to upgrade gasoline, the unit upgrading was conducted to use RIPP`s solid superacid isomerization catalyst to improve the ON of isomerate. Two kinds of C5, C6 isomerization processes were simulated to compare the effect of catalyst dosage, RON of isomerate, equipment, and energy consumption on transformation results. The results show that using the original process with little changes and low cost, the unit can produce RON 84.2 isomerate with much less solid superacid isomerization catalyst dosage.

ENGINEERING DESIGN AND START UP OF 300Kt/a CATALYTIC REFORMING UNIT PROCESSING BLENDING FCC GASOLINE

2015, 46(5):  45-48. 

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Introduced are the engineering design and startup of 300 kt/a catalytic reforming unit in Golumd refinery. Considering the project involving the relocation or reuse of the existing devices and the characteristic of the blending FCC gasoline in the pre-processing part of the unit, three technical measurements (catalyst graded loading, raw material filtration and dehydration, and feed mixture ratio control) were adopted. The scheme of reforming process technology and equipment reuse was also determined. Golmud refinery 300 kt/a catalytic reforming unit has been running smoothly since feeding nearly 1 year, the technical and economic indicators meet or exceed the design requirements. The blending of catalytic cracking gasoline relieves the shortage of reforming feedstock. The sulfur content of the catalytic cracking middle distillate is also reduced. The total construction investment reduces by around 40%, and the energy consumption of the unit is effectively lowered.

APPLICATION OF CATALYTIC DISTILLATION TECHNOLOGY IN FCC HEAVY GASOLINE HYDRODESULFURIZATION UNIT

2015, 46(5):  49-53. 

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Catalytic distillation technology is successfully applied in FCC heavy gasoline hydrodesulfurization unit of Sinochem Quanzhou Petrochemical Co.，Ltd. The calibration results show that for high sulfur feed，the sulfur content of FCC heavy gasoline is lowered from 599.0-981.0 μg/g to 3.8-7.0 μg/g and RON loss is only 2.1-2.9；and for the low sulfur feed，the sulfur content is reduced from 176.0 μg/g to1.3 μg/g and RON loss is about 0.5. At the initial stage of running，larger level fluctuation in the CDHDS column and the serious liquid entrainment of interstage knockout drum of circulating hydrogen compressor were observed. Measures，such as improving the level control scheme for CDHDS column，increasing the inlet pressure of the recycle hydrogen compressor，and adding the level regulating valve at bottom of the knockout-drum were adopted, resulting in improvement of the unit operation.

APPLICATION OF WGS WET FLUE GAS DESULFURIZATION TECHNOLOGY IN FCC UNIT

2015, 46(5):  54-56. 

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In order to get clean regenerated flue gas with little SO2 and PM, CNPC Jinxi Petrochemical Company built a wet flue gas desulfurization facility for 1 Mt/a FCC Unit. The facility used WGS technology, whose process is simple and equipment investment is low. It doesn’t need to modify heat recovery boiler but can fit long term operation of FCC unit. The WGS operation results show that SO2 and PM removal rates are very high; the cleaned gas contains no alkali liquor. The SO2 and PM emissions achieve the national integrated emission standard of air pollutants（GB16297-1996 ）. The facility has no bad effect on FCC unit and flue gas turbine; the flue gas pressure drop <0; the facility produce a little waste water that reaches the integrated wastewater discharge standard (DB21.1627—2008) of Liaoning province.

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APPLICATION OF MODIFIED ZSM-11 IN BENZENE ALKYLATION WITH METHANOL

2015, 46(5):  57-61. 

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A series of ZSM-11 was modified by NaOH, HCl acid and Mg loading. The samples were characterized by XRD、FE-SEM、NH3-TPD and BET techniques, respectively. The results show that the modified samples generate a number of mesopores, while aximum crystallinity and micropores are retained. The strong acid centers of the zeolite that facilitate carbon deposition reaction are covered by Mg. Alkylation of benzene with methanol (n（benzene）：n（methanol）=1) was performed over the modified ZSM-11 catalysts under the conditions of 460 ℃, 0.2 MPa and the weight hourly space velocity of 3 h-1. The benzene conversion is 52.60%. The total selectivity of toluene and xylene is 89.91%. The xylene selectivity is 34.08%. The reactivity of modified ZSM-11 is stable in 200 hours alkylation reaction.

BEHAVIORS OF ORGANIC Mo CATALYSTS IN HEAVY OIL HYDROTREATING AND ITS REASON ANALYSIS

2015, 46(5):  62-66. 

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Three kinds of organic molybdenum catalysts: molybdenum catalyst without sulfur (CAT-MoI), powder molybdenum catalyst with sulfur (CAT-MoII), and oily molybdenum catalyst with sulfur (CAT-MoIII) were synthesized. The performance of these catalysts in residue hydrocracking was investigated in an autoclave at the initial H2 pressure of 7MPa,430 ℃. The results show that the inhibition of coke formation enhances in the order of CAT-MoI＜CAT-MoII＜CAT-MoIII. To explore the cause for the difference, CAT-MoI, CAT-MoII, CAT-MoIII were dispersed in VGO and sulfurized at the conditions of initial H2 pressure of 7 MPa, 375 ℃for 60 min, respectively. XRD、TEM、SEM and Melvin Dynamic Light Scattering（DLS）were used to characterize the metal sulfides separated from VGO. The characterization results show that the metal sulfides from CAT-MoIII display the highest dispersity, lowest crystallinity and smallest particle size. The CAT-MoI has the highest crystallinity and the largest particle size.

PRODUCTION OF HIGH VISCOCITY AND HIGH VI PARAFFIN-BASE BASE OIL BY HYDRO-TECHNOLOGY

2015, 46(5):  67-70. 

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A combined catalyst system with iso-dewaxing catalyst as a core and relative hydro-technologies were used for production of high viscosity and high viscosity index base oil. The paraffin-based fraction of the 4th side cut of vacuum tower of Karamay Petrochemical Company, PetroChina was used as a feedstock. The industrial results show that the base oil with viscosity >8 mm2/s(100 ℃) and VI > 110 can be obtained by the above combined technology.

PREPARATION AND CHARACTERIZATION OF SILICON-CONTAINING PSEUDO-BOEHMITE

2015, 46(5):  71-76. 

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Silicon-containing pseudo-boehmites were prepared with kaolin as silicon source and then used to prepare the related catalysts. Orthogonal design experiments were applied to investigate the effect of the concentration of sodium meta-aluminate and aluminum sulfate, reaction temperature, pH on the characteristics of the silicon-containing pseudo-boehmite and catalysts. The samples were characterized by XRD, BET, FT-IR, and SEM. The evaluation tests of residual hydrogenation activity were conducted. The results show that the silicon-containing pseudo-boehmites are easily prepared with lower cost. The pore volume of silicon-containing alumina is 0.866 cm3/ g, and the proportion of large pore (pore diameter more than 20 nm) can reach 52.63 %. The particle diameter can reach maximum 54.14 μm. Compared with the silicon-containing alumina prepared by carbonation method and aluminum sulfate method, the B/L acid value of the support by new method is higher 6.3% and 3.5%, respectively. The catalyst prepared by the new method has a good hydrogenation performance. At the similar removal rate of impurities, the conversion of residue above 500 ℃ is 14.5% and 11.6%, respectively higher than that of the carbonation method and aluminum sulfate method.

HYDROCRACKING PERFORMANCE OF NiW/USY ZEOLITES FOR COAL TAR

2015, 46(5):  77-82. 

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A series of NiW hydrocracking catalysts with different contents of USY with high silica to alumina ratio (Si/Al=42) were prepared by co-impregnation method. The catalysts were characterized by NH3-TPD, BET, XRD, XPS and HRTEM techniques. The hydrocracking performance of the catalysts was evaluated in a fixed-bed reactor using diesel fraction from the hydrotreated middle/low-temperature coal tar. The results show that the NiW catalysts containing USY zeolite have a high hydrocracking activity and the cracking activity is mainly derived from the acidity of USY zeolite. Under the preconditions of ≥95% of the product yield, and the catalyst having appropriate USY zeolite content (30%), the density of the product decreases to 0.8485 g/ml from original 0.8990 g/ml, or less from original 17.4%, the C/H mole ratio decrease to 6.89 from original 7.32, the 50% distillation temperature decrease to 270℃ from original 304℃ and the cetane index increases to 43.5 from original 40.0, and the polycyclic aromatic hydrocarbons are cracked almost completely.

REASONS OF FILTER MEMBRANE BLOCKING OF AUTOMOBILE DIESEL

2015, 46(5):  83-87. 

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To understand the reason of filter screen blocking of automobile diesel, the amount of residue by pre-filtering the diesel fuel for the oxidation stability test, the total contamination, the filter-blocking tendency, and the soluble macromolecules with oxidation activity (SMORS) was determined. The results indicate that the colloidal particle formed by conglomeration of organic acid additives and amines in diesel fuels is the main reason for the blocking. The current domestic automotive diesel standards of cleanliness (GB 19147-2013) cannot reflect the reality of the diesel engine cleanliness, and the filter-blocking tendency or total pollution items should be considered.

TRIBOLOGICAL PROPERTIES OF MOLYBDENUM DIALKYDITHIOCARBAMATE IN LITHIUM BASE GREASE

2015, 46(5):  88-92. 

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he organic molybdenum compound, molybdenum dialkydithiocarbamate (MoDTC), was prepared. The functional group and element content of the compound was determined. The thermal stability was tested by TG-DSC. Its tribological properties in lithium base grease were evaluated by four-ball friction tester and compared with MoS2. The results show that MoDTC possesses a good thermal stability, the physicochemical property of the lithium base adding MoDTC grease is unchanged. Compared with the blank lithium base grease, at 392 N loading, the best anti-friction effect is achieved at 3.0% of MoDTC in grease, the average friction coefficient could reduce by 40.2%, and the mass fraction of MoDTC in grease is 2.0%, when the wear scar diameter is reduced by 29.8%.

PREPARATION OF MODIFIED NANOPARTICLE SiO2 AND EVALUATION OF ANTI-WEAR AND FRICTION-REDUCING PERFORMANCE

2015, 46(5):  93-97. 

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A series of SiO2 nano-particles were modified by different solvents and modifiers and characterized by SEM technique. The dispersing properties and tribology performance of the modified particles were investigated to screen out the best solution and modifier. The tribology performance of the lubricant adding the best modified SiO2 was tested to determine the optimal amount of modified SiO2 nano- particles. It is found that ethanol is the suitable solvent for SiO2 naoparticle surface modification, and the best modifier is KH-550. The best way to use KH-550 is to prepare KH-550 alcohol solution first and then add into the lubricant system. The lubricant with 2% (w) modified SiO2 nano-particles has the best anti-wear and anti-friction performance.

APPLICATION OF TOTAL SITE INTEGRATION TECHNOLOGY IN OIL REFINING ENTERPRISE

2015, 46(5):  98-100. 

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This paper introduces the characteristics of total site integration technology. With a real case of oil refining enterprise and SuperTarget software, the method was introduced in detail and optimized. The theoretical optimal utility configuration, total site pinch position, the direction of the utility level optimization, potential heat and power co-generation, and the potential of the processes and utilities combination optimization were investigated. Guided by the above analysis, energy system optimization of the sample refinery was implemented. The energy saving of 31.4 MW is obtained. The application shows that the technology to guide energy system optimization of oil refining enterprises has an obvious effect.