Table of Content

12 May 2012, Volume 43 Issue 5

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ISOMERIZATION OF ETHYLCYCLOHEXANE OVER SHAPE SELECTIVE MOLECULAR SIEVES

2012, 43(5):  1-5. 

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The isomerization of ethylcyclohexane (ECH) was investigated via three types of shape selective molecular sieve, ZSM-5, MOR and EU-1. The structural and acidic properties of these molecular sieves were characterized by XRD，N2 adsorption，NH3-TPD, Py-IR adsorption and TG techniques. The experimental results demonstrate that the structure and acidity of various molecular sieves play an important role on the reaction network of ECH isomerization, especially the pore structure. In ECH isomerization reactions, more strong/medium acid sites and enough space for reaction are required. Since MOR has 12-membered ring structure and EU-1 has 12-membered ring side pockets, they possess better reaction activity. On the whole, among these three molecular sieves, EU-1 exhibits as the optimal catalyst for ethylbenzene isomerization based on its high ECH conversation and good C8 isomerization selectivity.

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STUDY ON INTENSIFYING THE PROCESS OF SHENGLI VACUUM RESIDUE THERMAL CRACKING

2012, 43(5):  6-9. 

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It is investigated to use additive L to intensify the thermal cracking of Sheng Li Vacuum Residue were tested on the lab-scale evaluating equipment. The result demonstrated that much higher liquid yields and much lower coke yields have been achieved by adding L additive. Increased the liquid product is mainly the VGO fraction and its composition is mainly above 3-ring or multi-ring aromatic hydrocarbons. Therefore, that indicates L accelerates the cracking of alkyl chain of polycyclic aromatic and bridge chain between polycyclic aromatic structures. Gas composition data showed that the contents of methane, ethane and ethylene decreased the contents of propane, propylene, butane and butylenes increased with the introducing of L. It indicated that L likely has changed the way of hydrocarbon thermal cracking.

A RESEARCH OF DEACIDIFICATION OF 2nd VACUUM DISTILLATES BY CATALYTIC DECOMPOSITION

2012, 43(5):  10-13. 

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The 2nd vacuum side cuts are the feedstocks of lube oil, but naphthenic acid in the distillates could cause serious corrosion problems during processing. In this paper, Mg-Al hydrotalcite spherical catalyst made by mechanical rolling process was used to catalytic decompose the naphthenic acid in Zhonghai 2nd vacuum distillate and the effect of reaction conditions on the removal rate of naphthenic acid was investigated. Test results show that Mg-Al hydrotalcite is an effective catalyst for decomposing naphthenic acid, and the Mg-Al hydrotalcite catalyst particles made by mechanical rolling possess excellent anti-press strength and good pore structure. Under the conditions of a reaction temperature of 320℃, a reaction time of 60 min, a reaction pressure of 0.1 MPa and catalyst/oil mass ratio of 0.2, the acid number of treated Zhonghai 2nd vacuum distillate was reduced from 4.32 mgKOH/g to 0.46 mgKOH/g, its corrosion hazard is less. Therefore, materials of equipments and pipeline in processing this distillate do not need to be upgraded.

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OLIGOMERIZATION OF ISOBUTENE CATALYZED BY AlCl3 IONIC LIQUIDS

2012, 43(5):  14-18. 

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AlCl3 ionic liquids having various cations and anions were synthesized. Tests for oligomerization of isobutene catalyzed by various AlCl3 ionic liquids were conducted in an autoclave, and the effect of reaction temperature, reaction time and stirring speed was studied. Experimental results indicated that these AlCl3 ionic liquids exhibited good catalytic performance in isobutene oligomerization with conversion of isobutene over 95%. For ionic liquids synthesized by AlCl3 and [C2H5]3NHCl, when the mole ratio of AlCl3 to [C2H5]3NHCl was below 1:1, the AlCl3 ionic liquid was inactive to isobutene oligomerization; when the mole ratio of AlCl3 to [C2H5]3NHCl was 1:1, the ionic liquid exhibited certain catalytic activity and its selectivity to dimers and trimers was good; when the mole ratio of AlCl3 to [C2H5]3NHCl was above 1:1, these ionic liquids could effectively catalyze oligomerization reactions, the conversion of isobutene reached more than 95%, yet the selectivity to dimers and trimers declined and the product distributions were continuous with certain amount of cracking byproducts. The optimal reaction conditions were as follows: a reaction temperature of 80 ℃, a reaction time of 30 min and stirring speed of 1 300 r/min.

A NEW TWO-STAGE IN SERIES PROCESS OF SLURRY BED FISCHER-TROPSCH SYNTHESIS

2012, 43(5):  19-23. 

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Simulation tests of a patent two-stage in series process and conventional single-stage process for Fischer-Tropsch synthesis were carried out on a 10 L(oil)/h pilot plant slurry bed reactor system continuously, using a commercial precipitation iron catalyst. The test results show that as compared with single-stage process under the same processing capacity or oil yield, the required catalyst of this new process is more than 20% less, the processing capacity of per unit volume reactor is much higher and a reduction of about 60% total circulating gas is observed, thus the energy consumption and operation cost are lower. This unit is more integrated and its initial investment is also lower since a few equipments, such as a recycle gas compressor can be omitted.

RESEARCH AND COMMERCIAL APPLICATION OF DEEP CRACKING DELAYED COKING TECHNOLOGY

2012, 43(5):  24-28. 

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Based on studying the reaction characteristics of delayed coking and coking mechanism in furnace tubes, a technical revamping of the coking furnace of a 1.6 Mt/a delayed coking unit was carried out in order to control the cracking severity of feedstock leaving furnace, a software simulating process happened inside and outside of the furnace tube was adopted. Several novel technical measures and patents were involved in the revamping, as well as operating parameters optimization to enhance the heat provided for coking reactions by furnace and improve product distributions. The simulation results post to furnace revamping showed that the cracking severity of feedstock leaving furnace was deepened and the heat provided for coking reactions was enhanced significantly. Commercial running results showed that by adopting deep cracking technology in coking furnace, the processing capacity of the furnace increased and reached 1.85—1.90 Mt/a; the external surface temperature of furnace tube was about 80 ℃ lower than that of prior to revamping, and the operation period after coke burning was prolonged from 9-month to more than 15-month. After revamping, although the carbon residue in feed was higher, the coke yield/coke yield coefficient decreased and the liquid yield increased with good economic benefit, which indicated that this delayed coking unit could meet the requirements of processing inferior feedstock with high processing capacity and improved product distributions.

PILOT PLANT TEST OF REMOVING NAPHTHENIC ACID FROM 4th VACUUM CUT OF KARAMAY HEAVY CRUDE VIA MICROREACTOR

2012, 43(5):  29-31. 

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Pilot plant tests of removing naphthenic acid from the 4th vacuum side cut of Karamay heavy crud were carried out on a 200 kg/h microchannel reactor. Test results showed that the acid removal rate of this single stage microreactor process was more than 85%, which was better than that of the industrial two-stage extraction process with the same feedstock. Besides, this new process simplified the acid removal process, its solvent to oil ratio and energy consumption were much lower. It offers a new choice to remove large naphthenic acid molecules from heavy crude fractions effectively.

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PROCESS ANALYSIS AND OPTIMIZATION OF AMMONIA BURNING IN A SULFUR RECOVERY UNIT

2012, 43(5):  32-35. 

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After a period of operation and analysis, the process conditions of ammonia burning at the sulfur recovery unit of SINOPEC Luoyang Branch Company were optimized. Results showed that by increasing the air/feed gas volume ratio and the inlet temperature of sour gas to furnace, adjusting the volume fraction of ammonia in sour gas and optimizing instrumentation and control, the temperature difference of reactor inlet and bed layer increased to ensure fully reactions; the system pressure was maintained at 0.038 MPa and the NH3-N content in quench water was around 300 mg/L. Good economic, environmental and social benefits were obtained.

STUDY ON THE DEMULSIFICATION/DEHYDRATION TECHNOLOGY OF LIAOHE AGING OIL

2012, 43(5):  36-39. 

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Adopting thermo-gravity settling method to demulsify and dehydrate Liaohe aging oil, the demulsifiers were screened and the effect of demulsification temperature, stirring rate, stirring time, depositing temperature and depositing time on the dehydration of aging oil was investigated. Test results showed that polyether demulsifier could be used for the demulsification/dehydration of Liaohe aging oil with an optimum amount of 400 μg/g. The optimum dehydration process conditions were obtained as follows: demulsification temperature of 80 ℃, stirring rate of 120 r/min, stirring time of 60 min, depositing temperature of 70 ℃ and depositing time of 72 h. When using polyether as main demulsifier and compounded with additive (alcohol/HEDP), treating Liaohe aging oil under the above conditions, the water content of the treated aging oil was 10.8 %, which could be further disposed by electrostatic desalting and dewatering device to reach a water content of less than 0.5%.

EFFECT OF PEPTIZATION CONDITIONS ON THE DISPERSITY AND PELLETIZATION OF PSEUDO-BOEHMITE

2012, 43(5):  40-44. 

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Aluminum hydroxide sol was prepared by method of dispersing pseudo-boehmite powder in acidic water. The effect of peptizing conditions on the acid dispersion index of pseudo-boehmite was studied, and it was found that the reaction temperature and acid amount had great effect while the influence of reaction time was not significant. Using aluminum hydroxide sol samples obtained under various reaction temperatures, spherical alumina supports were prepared by oil-ammonia column shaping method and followed by drying and calcination. The results of characterization by BET and XRD showed that with the increase of sol prepared temperature, for the prepared alumina support, its pore volume decreased, the distribution of pore diameter was more concentrated, bulk density and crush-strength increased, and the specific surface area changed little. Results of hydrothermal stability test at 650 oC for 50 h showed that the specific surface area of treated self-made alumina spheres was close to that of treated industrial one, which indicated that they possessed the similar hydrothermal stability.

DEVELOPMENT AND APPLICATION OF DESULPHURIZATION CATALYST SERIES FOR LO-CAT SULFUR RECOVERY UNIT

2012, 43(5):  45-48. 

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Considering the characteristics of acid gas produced by desulphurization treatment of natural gas and the operation conditions of LO-CAT sulfur recovery unit, a series of desulphurization catalysts for sulfur recovery unit was developed. The application of this catalyst series in the LO-CAT sulfur recovery unit of an enterprise indicated that the sulfur removal rate of this series catalysts was more than 99.99%, the volume fraction of hydrogen sulfide in off-gas was less than 30 μL/L, and the average output of sulfur was 0.8 t/d, which met the demand of the production device, significant economic, social and environmental benefit was achieved.

INDUSTRIAL APPLICATION OF FHUDS-6 CATALYST IN A 4.1 Mt/a DIESEL HYDROFINING UNIT

2012, 43(5):  49-53. 

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The deep hydrofining catalyst FHUDS-6 was applied in a 4.1 Mt/a diesel hydrofining unit firstly, and the operation data of performance test in full capacity was analyzed. Results show that using a feedstock with 11% FCC diesel fraction, under the process conditions of an average catalyst bed temperature of 352 ℃, a space velocity of 2.53 h-1, a hydrogen partial pressure of 6.15 MPa and hydrogen to oil volume ratio of 254.3, FHUDS-6 catalyst exhibits high hydro-desulfurization activity and hydro-upgrading activity, the sulfur removal rate researches 98.02% and the cetane number of treated diesel fuel increases by 5.7 units. The quality of the obtained diesel product can meet the requirements of National Emission Standard III for diesel fuel.

COMMERCIAL APPLICATION OF CATALYST ABC FOR ANTI-BASIC NITROGEN DEACTIVATION IN FCC UNIT

2012, 43(5):  54-58. 

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Catalyst ABC for anti-basic nitrogen deactivation was successfully applied in the FCCU of SINOPEC Jiujiang Petrochemical Corporation. The results of industrial application showed that in comparison with the conventional catalyst used in base case under similar processing capacity, feedstock for catalyst ABC case had significant increase of total nitrogen and basic nitrogen content, the total liquid yield, gasoline yield and conversion in this case increased by 1.25, 1.77 and 2.15 percentage points, respectively; when the properties of feedstocks were similar, but processing capacity increased significantly in catalyst ABC case, the total liquid yield, gasoline yield and conversion of this case increased by 1.02, 0.99 and 0.11 percentage points, respectively. Besides, the properties of the liquid products were basically unchanged in these two cases. Thus, catalyst ABC is suitable to be used for processing feedstocks with high nitrogen and basic nitrogen content; it exhibits good performance of heavy oil conversion, high gasoline yield, good product distribution and selectivity to high value products.

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EFFECT OF NANO-TiO2 ADDITIVE ON THE TRIBOLOGICAL PROPERTIES OF EMULSION FOR COLD ROLLING COPPER PLATE

2012, 43(5):  59-62. 

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The tribological performance of cold rolling emulsions with and without nano-TiO2 additive was compared by four-ball test and cold rolling copper plate test. Four-ball test results show that compared with conventional rolling emulsion, the friction reducing property and extreme pressure anti-wear performance of rolling emulsion with nano-TiO2 additive improved significantly. In cold rolling copper plate tests, using rolling emulsion with nano-TiO2 additive can effectively reduce rolling pressure and increase extreme depress rate, besides, it can repair the surface defects of cold rolled copper plate simultaneously, resulting in a better plate surface.

STUDY ON THE FRICTION REDUCING PERFORMANCE OF DITHIOPHOSPHATES AND GLYCERYL MONO-OLEATE

2012, 43(5):  63-66. 

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Molybdenum dithiophosphate，tungsten dithiophosphate and glyceryl mono-oleate were synthesized and used as lube additives. Their friction reducing performance in lube oil was evaluated by HFRR testing device. Test results showed that these three friction reducing additives could reduce the friction coefficient significantly. Glyceryl mono-oleate had better friction reducing property at low testing temperature, molybdenum dithiophosphate and tungsten dithiophosphate had good friction reducing performance at high temperature. The complex of dithiophosphates and glyceryl mono-oleate exhibited positive synergistic effect on reducing friction.

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EFFECT OF CRUDE OIL DRAG REDUCTION AGENT ON THE SEWAGE TREATING SYSTEM OF SHENGLI REFINERY

2012, 43(5):  67-70. 

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In Sinopec Qilu Company victory refinery processing of aqueous soluble drag reducing agent for crude oil sewage treatment system by A COD standard, can not discharge standards, Sinopec Qilu Company Institute by liquid chromatography, water solubility test, biochemical analysis, identified by the reason of excessive sewage, while the pipeline drag reduction agent for electric desalting simulation evaluation, screening for oil soluble drag reducing agent B and its application in industrial production, both to ensure that the crude oil transportation capacity, but also eliminate the effect of the sewage treatment system.

STUDY ON THE ISOLATION OF BACTERIA FOR QUINOLINE DEGRADATION AND ENHANCED TREATMENT OF REFINING WASTEWATER

2012, 43(5):  71-75. 

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A bacterial strain capable of utilizing quinoline as sole source of carbon, nitrogen and energy was isolated from the petroleum contaminated soil of a petrochemical refinery. The isolate was identified as Enterobacter sp. having strong quinoline degradability. Biodegradation experiments showed that this strain could degrade 486 mg/L of quinoline in pure culture completely within 30 h. Said bacteria not only could degrade quinoline with high concentration in refinery wastewater efficiently, but also could co-treat other organic pollutants together with other organisms to further reduce the CODCr of effluent. The activity of nitrobacterium was inhibited by the high concentration of quinoline temporarily, yet it could be recovered in about one week. The biodegradation of quinoline released as ammonia into the growth medium, which increased the load of ammonia, however, the decrease of ammonia removal rate was also temporary. The degradation of quinoline followed zero-order kinetics equation when the concentration of quinoline in the range of 200 to 686 mg/L.

MODELING AND OPTIMIZATION FOR CATALYTIC CRACKING PRODUCTS OF HEAVY OIL BASED ON SUPPORT VECTOR REGRESSION

2012, 43(5):  76-81. 

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The product distributions of catalytic cracking have a complex functional correlation with feedstock compositions and reaction conditions. The experimental results of three heavy oil samples having various compositions and testing under different reaction conditions were normalized as training data, by using support vector regression (SVR) method, a yield model for gasoline and diesel products of heavy oil catalytic cracking was established. For catalytic cracking of recycle stock, gasoline and diesel yields under different operation conditions were calculated by the generalization ability of SVR model. The optimal operation conditions for maximizing light oil (gasoline and diesel) yield were found by particle swarm optimization (PSO) algorithm. Calculated results show that this model has good fitting effect with experimental data under various reaction conditions. The simulated three-dimensional graphs can effectively illustrate the relationships between product yields and reaction conditions. The optimal reaction conditions obtained by PSO algorithm are as follows: reaction temperature of 530℃, catalyst to oil mass ratio of 7.5 and space velocity of 8 h-1. Under such conditions, the simulated and experimental light oil yields are 42.3% and 41.8%, respectively, the relative error is 1.20%.

OPTIMIZATION STRATEGY FOR THE HEAT EXCHANGER NETWORK OF CRUDE DISTILLATION UNIT BASED ON PLUS/MINUS PRINCIPLE

2012, 43(5):  82-87. 

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Based on the characteristics of cold and hot streams in crude distillation unit (CDU), using pinch technology, the streams of the heat exchanger network (HEN) in CDU are divided into four categories: hot streams above the pinch, cold streams above the pinch, hot streams below the pinch and cold streams below the pinch. The bottlenecks of the HEN are analyzed, such as the number of cold stream is much less than that of hot stream and the heat source above the pinch is deficit while the heat source below the pinch is surplus. Therefore, an optimization strategy of HEN based on the plus/minus principle is presented in this paper. A case study of this proposed strategy is carried out in the HEN of an industrial CDU with a capacity of 5 Mt/a. Results show that the final temperature of heat-exchanged crude oil is increased by 33 oC, the comprehensive energy consumption of the whole CDU is decreased by 26 MJ/t, which indicates that the energy saving effect of this proposal is significant.

DETERMINATION OF EXTRACTABLE PETROLEUM HYDROCARBONS IN WASTEWATER

2012, 43(5):  88-92. 

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A method for the determination of extractable petroleum hydrocarbons (EPH) in wastewater, comprising liquid-liquid extraction, purification by florisil and gas chromatography determination, was developed. Sample preparation and analytical conditions were investigated and optimized, including sample extraction, purification and concentration of extracts, and operating parameters of gas chromatography. The results showed that the recovery rates of EPH reached 99.7%—100% during purification by activated florisil; the removal rates of polar non-hydrocarbon model compounds (methyl palmitate or methyl oleate) were in the range of 90.7%—100%; EPH recovery rates reached 90.3%—92.5% by 3-times acidic extraction followed by 3-time alkali extraction. The detection limit of this method was 15.2 μg/L, blank spike and matrix spike recoveries were 92.0% and 81.5%, respectively. A case study of testing a refinery effluent showed that the relative standard deviation (RSD) of determination was 4.1% (n=6).

PROBLEMS EXISTING IN THE UNIT OF RECOVERING CONCENTRATED ETHYLENE FROM FCC DRY GAS AND THEIR COUNTERMEASURES

2012, 43(5):  93-97. 

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The basic principle, technology and equipment improvements of recovering concentrated ethylene from FCC dry gas were introduced based on a case study. In the process improvements, the adjustment of product refining process, adding an arsenic removal step, adding separation and washing after MDEA treatment, altering regeneration gas in drying process, improving compression unit and setting a pre-distillation unit for ethylene pretreatment were reviewed. Equipment improvements including roots vacuum pump, electric heater, refrigeration dryer and semi-product gas compressor were discussed. Finally, factors affecting the long-term operation of unit, such as the properties of raw materials and liquid entrained, troubles in compressor system and vacuum system were analyzed and countermeasures were proposed.

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RESEARCH ADVANCE IN DESULFURIZATION OF TRANSPORTATION FUELS BY EXTRACTION PROCESS

2012, 43(5):  98-102. 

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The mechanism of removing sulfur containing compounds from transportation fuels by solvent extraction is summarized, and research progresses of extraction desulfurization technologies worldwide are reviewed. Compared with other desulfurization technologies, extraction method has the advantages of low investment, simple operation and less octane number loss of gasoline. However, there is still room to be improved in conventional acid/alkali washing and organic solvent extraction. Extraction with ionic liquids exhibits promising future, so dose membrane separation technologies for sulfur removal. The coupling of extraction method with oxidation, biodegradation and others to remove sulfur compounds also has bright developing prospect.