Table of Content

12 July 2022, Volume 53 Issue 7

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FLEXIBILITY OF DCC TECHNOLOGY AND ITS COMMERCIAL APPLICATION IN CHEMICAL-TYPE REFINERY

2022, 53(7):  1-5. 

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The characteristics of deep catalytic cracking (DCC) and enhanced deep catalytic cracking (DCC-plus) technology and their relationships were reviewed. DCC-plus technology has higher propylene yield than DCC technology, and the yield of dry gas and coke is significantly reduced. For a set of 2.2 Mt/a DCC-plus unit for processing 50% atmospheric residue mixed with 50% hydrocracking tail oil as feedstock, the yields of ethylene and propylene yields were 5.6% and 21.5%, respectively. A set of 1.2 Mt/a DCC-plus unit has switched between two operation modes of fuel oil program and olefins program. Compared with the fuel oil mode, the propylene yield was increased by 125.8%, and the DCC naphtha and light cycle oil (LCO) yields were reduced by 37.4% and 20.0%,respectively,under the olefins production mode. DCC technology is mature and reliable, and the large-scale and long-term operation of DCC unit has been verified in industry. For chemical refineries with the DCC units as the core, the oil product ratio (the total output of gasoline, diesel and aviation fuels as a proportion of crude oil processing) can be as low as 16.0%, and the rate of chemicals (the total production of propylene, aromatics and ethylene as a proportion of crude oil processing) is as high as 67.3%, which is a competitive technical choice for building a new generation of full chemical-type refinery.

DEVELOPMENT AND COMMERCIAL APPLICATION OF HYDROUPGRADING TECHNOLOGY FOR FULL RANGE MID-LOW TEMPERATURE COAL TAR

2022, 53(7):  6-11. 

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In view of the high contents of metal, particulate matter and aromatic hydrocarbon in full range mid-low temperature coal tar, the combined technology of low-pressure pretreatment-fixed bed hydrogenation was developed. The results of pilot plant indicated that the clean diesel fraction with sulfur content less than 20 μg/g could be produced by the combined process using mid-low temperature coal tar as raw material, at the same time, the by-product naphtha with the sulfur less than 0.5 μg/g, the nitrogen less than 0.5 μg/g, and the aromatic potential content(w) more than 70% could be used as excellent reformer feed. The hygro-upgrading technology of full fraction of mid-low temperature coal tar had the characteristics of low investment, simple process, and high liquid yield and good product quality.It provides the technical support for the clean and efficient utilization of coal in China.

SYNTHESIS OF EPICHLOROHYDRIN BY CATALYTIC EPOXIDATION OF ALLYL CHLORIDE IN ACETONE SOLVENT

2022, 53(7):  12-17. 

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In the presence of the catalyst TS-1, allyl chloride can directly react with hydrogen peroxide to produce epichlorohydrin. Acetone is compatible with the mixed system of allyl chloride and hydrogen peroxide. The conversion of hydrogen peroxide was greater than 97% and the selectivity of epichlorohydrin was more than 95% when the stirring rate was more than 300 r/min, the reaction time was 60 min, the reaction temperature was 55-70 ℃ and the molar ratio of allyl chloride to hydrogen peroxide was 1.5. Compared with methanol as solvent, the solubility of acetone per unit mass was lower than that of methanol, and the consumption of acetone was 20% more than that of methanol, but the evaporation heat of acetone was only 82.4% of that of methanol. The energy consumption of acetone recovery and recycling is equivalent to that of methanol. The main side-reactions with acetone as solvent were the hydrolysis reactions of epichlorohydrin, and with methanol as solvent, besides hydrolytic ring-opening reaction of epichlorohydrin, there was also alcoholytic ring-opening reaction.

INDUSTRIAL TEST OF MFP TECHNOLOGY IN FCC UNIT

2022, 53(7):  18-22. 

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The catalytic cracking and hydrodesulfurization technology for producing more The catalytic cracking and hydrodesulfurization technology for producing more propylene and low sulfur fuel oil components in FCC unit was introduced, including revamping, industrial test and industrial application, so as to flexibly adjust the production plan to meet market demand. The MIP-CGP process was used as blank calibration, and the changes of Marine Fuel and Propylene (MFP) process operating conditions and product distribution were compared when the special catalyst accounted for 50% and 80% of the system storage. The results show that hydrogen distribution is improved, the propylene and isobutene content in LPG is greatly increased, the yield and selection of low-carbon olefins are improved, and dry gas and coke production are kept stable. FCC technology has been changed from high conversion rate to high selectivity, which can realize the efficient utilization of hydrocarbon resources, and can adjust production plan flexibly according to the change of market demand to realize the maximization of economic benefit.

LONG-TERM COMMERCIAL APPLICATION OF HYDROCRACKING TECHNOLOGY FOR INCREASING JET FUEL AND HIGH QUALITY TAIL OIL IN LARGE PROPORTION

2022, 53(7):  23-29. 

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The hydrocracking technology of increasing jet fuel and high quality tail oil in large proportion and the long-term industrial application of supported catalyst in a 2.0 Mt/a high pressure hydrocracking unit were introduced. The production situation of blending different secondary processing oil and using flexible hydrocracking catalyst in the previous cycle were compared. The results of initial and mid-term industrial calibration showed that the yield of kerosene fraction was more than 40% with the smoke point more than 25 mm, and BMCI of tail oil fraction was less than 9. After continuous operation for 57 months, the products had excellent properties, and the goals of increasing kerosene fraction in large proportion was successfully achieved, improving the quality of tail oil and flexible production of diesel fuel. The catalyst bed temperature, bed pressure drop and radial temperature difference increased slowly, which showed that the catalyst had good activity stability, low temperature raising rate and strong impact resistance, which could meet the needs of long-term operation. The successful application of the new technology in the unit has guaranteed the supply of jet fuel supply in the capital area, provided technical support for transformation and development of the refinery, integration of refining and chemical industry, maximization of benefits, and provided high-quality raw materials for ethylene unit.

INDUSTRIAL TEST OF PROCESSING FLUID CATALYTIC CRACKING DIESEL IN COKING GASOLINE AND DIESEL HYDROTREATING UNIT

2022, 53(7):  30-35. 

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A large account of fluid catalytic cracking diesel（FCC diesel） with high aromatic content, low cetane number was produced in a petrochemical company. In order to solve the problems of high hydrogen consumption and high operating cost of FCC diesel processing in the hydrocracking unit, the FCC diesel is converted to the coking gasoline and diesel hydrogenation unit as an industrial test. The data of raw material properties, main operating parameters, product properties, material balance under different blending ratio were compared. The results show that the density and the content of polycyclic aromatic hydrocarbons are increased significantly, the cetane number is greatly reduced, and the average temperature of the reaction increases greatly. Under the present production conditions, it is suitable to control the feed ratio of FCC diesel no more than 20%.

EXPLORATION AND INDUSTRIAL PRACTICE OF USING EXISTING DIESEL HYDROTREATING UNIT TO PRODUCE REFORMER FEEDSTOCK

2022, 53(7):  36-39. 

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The scheme of using the existing diesel hydrotreating unit to produce reformer feedstock was studied. The effects of different types of hydrotreating catalysts, hydrocracking catalysts and conversion rate on hydrocracking reaction of diesel oil were investigated, and the suitable hydrotreating and hydrocracking catalyst system was selected. It was found that under the same reaction conditions, Ni-Mo hydrotreating catalyst had better hydrodesulfurization, denitrification and aromatics saturation performance, and was more suitable as a refining catalyst for hydrocracking of diesel oil to produce reformer feedstock. In light oil hydrocracking catalyst system, the aromatics and aromatic potential content of naphtha fraction were the highest, and in major middle oil hydrocracking catalyst system, the cetane number of diesel oil is higher. The yield of naphtha was increased from 6.47% to 10.47%, and the  aromatic potential content of naphtha was increased from 44.5% to 47.9% in a 2.6 Mt/a hydrotreating unit of diesel oil, to achieve the goal of structural adjustment of raw materials for producing more reformer feedstock with high aromatic potential content.

INDUSTRIAL PRACTICE OF MIXING FCC SLURRY ON DELAYED COKING UNIT WITH HIGH SEVERITY

2022, 53(7):  40-44. 

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In order to solve the problem of mixing FCC slurry in delayed coking unit, the thermal reaction characteristics of FCC slurry were studied by using a heavy oil micro-thermal reactor. The results showed that the coke yield and gas yield of slurry were higher than that of the vacuum residue under the same reaction conditions, the product distribution of vacuum residue changed little with the reaction time increasing from 2 h to 4 h, and the coke yield of FCC slurry was decreased by 3.07 percentage points, which indicated that the more heat and higher reaction severity were needed in thermal reaction of FCC slurry. Through revamping the coking furnace of the industrial unit, the industrial practice of mixing FCC slurry with high severity was carried out. Under the condition of mixing FCC slurry, the conversion rate at the exit of coking furnace was increased from 8% to 12%, the yield of petroleum coke in the unit was reduced by 1.1 percentage points, and the volatile content of petroleum coke was reduced by about 2.1 percentage points, which indicated that the thermal conversion degree of feedstock was improved and the high severity condition was favorable for the deep conversion of slurry oil.

ACQUISITION AND ANALYSIS OF PROCESS PARAMETERS OF C₈ AROMATICS ISOMERS ADSORPTION SEPARATION SYSTEM

2022, 53(7):  45-50. 

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The adsorption properties of toluene and C₈ aromatics isomers on KBaX and NaY adsorbents were studied. The adsorption equilibrium parameters C₈ aromatics isomers on the adsorbents were determined by static equilibrium test. The changes of saturated adsorption capacity and relative selectivity coefficient with temperature and component composition were analyzed, including the saturable adsorption capacity and relative selectivity coefficient. At the same time, a dynamic penetration test was used for measuring and calculating the mass transfer coefficients, and the mass transfer coefficients were calculated by fitting the penetration test data with Aspen software. The results show that the adsorption performance parameters measured by the test are in good agreement with the simulation results, and the reliability of the adsorption performance parameters measured by the test is good.

STUDY ON THE MECHANISM OF SULFATE REDUCING BACTERIA ON SILVER STRIP CORROSION OF JET FUEL

2022, 53(7):  51-57. 

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The effects of sulfate reducing bacteria (SRB) in jet fuel storage system on the corrosion performance of silver strips were investigated by using two kinds of SRB, namely Desulfotomaculumruminis and Desulfovibriofructosivorans. The corrosion mechanism of SRB on silver strip was analyzed by means of SEM/EDS and XPS, and the morphology and functional groups of the corroded silver strip were analyzed. The results show that both SRB can cause silver strip corrosion in jet fuel. The more SRB there are, the more serious the corrosion of silver strips is. The SRB concentrate on the water phase and adhere to the surface of the silver strips to corrode. During the process, H2S produced by SRB diffused from the water phase to the oil phase to cause corrosion of the oil phase silver strips. The main corrosion products of silver strips in the oil phase were Ag2S, and those in the water phase were FeS2 and FeS.

COMMERCIAL APPLICATION OF PST-100 CATALYST IN PROPANE DEHYDROGENATION UNIT

2022, 53(7):  58-63. 

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The application of PST-100 catalyst in 450 kt/a propane dehydrogenation unit is introduced. The industrial application results showed that the catalyst had excellent activity, high selectivity, high strength and low dust content with low carbon deposition rate and the carbon deposition amount of spent catalyst about 1.5% . The catalyst strength remained above 38 N after 3.5 a of operation, and the particles size smaller than 0.8 mm in the dust were less than 1.5 kg/d, which could greatly reduce the adverse impact of dust on the stable operation and prolong the operation cycles of the unit. The catalyst has strong chlorine holding capacity which can decrease the chlorine loss of catalyst. The chlorine injection amount in regeneration progress was about 0.1% of the catalyst circulation rate, which could greatly weaken the corrosion of chlorine to the equipment and improve the operation stability of the unit. After 3.5 a of industrial application, the catalyst activity remained stable, the consumption of propane for the production of 1 t propylene was 1.16 t, and the service life of the catalyst was expected to exceed 4 a.

PERFORMANCE DIFFERENCE OF CATALYTIC CRACKING CATALYSTS MADE OF KAOLIN FROM DIFFERENT REGIONS

2022, 53(7):  64-69. 

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The physicak and chemical properties of five kinds of kaolin (American kaolin, Hengyang kaolin, Guizhou halloysite, Zhangzhou kaolin, Hepu kaolin) were analyzed, and the difference of catalytic cracking catalysts prepared with these five kinds of kaolin was investigated. The results show that the main components of the five kinds of kaolin are SiO₂ and Al₂O₃.The contents of Fe₂O₃ and CaO, the specific surface area and the particle diameter of halloysite are the largest.The wear index of FCC catalyst made of halloysite is the highest, and its catalytic cracking performance is the worst. The catalyst prepared from Zhangzhou kaolin showed the lowest heavy oil yield (6.81%) and the highest liquid yield (88.43%). The catalysts prepared from American kaolin, Hengyang kaolin and Hepu kaolin showed similar yields of LPG, gasoline, dry gas and coke.

EFFECT OF HETEROATOMS SULFUR AND NITROGEN ON OXIDATION STABILITY OF LUBRICATING BASE OIL

2022, 53(7):  70-74. 

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The oxidation processes, oxidation products and colors of nitrogen-containing compounds and sulfur-containing compounds were studied using a density functional theory based on quantum mechanical method, and the effects of nitrogen-containing compounds and sulfur-containing compounds on the oxidation stability of base oil were investigated by model compound test. The results show that the oxidation of nitrogen-containing compounds to carbonyl compounds can promote the oxidation of other organic hydrocarbon molecules, and carbonyl was the chromogenic group of the oxidizing products.The sulfur-containing compounds were oxidized to sulfoxide compounds containing sulfinyl or sulfone compounds containing sulfuryl, which did not produce new hydroperoxide radicals and could stop the oxidation reaction of free radicals. The sulfur-containing compounds did not show color.

PRODUCTION TECHNOLOGY OF ANTI-YELLOWING RUBBER PLASTICIZER

2022, 53(7):  75-79. 

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With the decrease of resources of high-quality paraffinic base crude oil, the quality of lube base oil produced by the traditional solvent refining process has become worse, the viscosity index is lower, and some of them can not meet the standard requirements of API Ⅰ. Because the paraffin market is relatively stable, the low viscosity index base oil maintains a considerable output to maintains the production of paraffin products. In order to effectively utilize this part of low viscosity index base oil, the technology of producing high-grade SBS rubber plasticizer by hydrotreating base oil with low viscosity index was developed by SINOPEC Research Institute of Petroleum Processing, and the added-value of the product was increased. The results show that the color of the rubber plasticizer produced by the process of hydrogenation prerefining-distillation separation-hydrofinishing is basically unchanged after UV irradiation, and it has good yellowing resistance. The expected goal was achieved.

EFFECT OF OVERBASED CALCIUM SULFONATE DETERGENT ON ANTI-FRICTION AND ANTI-WEAR PERFORMANCE OF LUBRICATING OIL

2022, 53(7):  80-85. 

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The effects of three overbased calcium sulfonate detergents on the friction performance of manual transmission oil were studied. The friction coefficient, wear spot and scar were analyzed and evaluated by HFRR high frequency reciprocating rig, SRV wear machine, MPR micropitting rig and Automax synchronous bench machine. The results showed that the three kinds of high base calcium sulfonate all had anti-friction and anti-wear effects. When the dosage (w) was 1%, the detergent C with the highest calcium content and alkali value had the best anti-friction and anti-wear effects, the friction coefficient, the diameter of wear scar and the change rate of MPR roller width of oil were the smallest, and the axial wear of Automax synchronous ring was the lowest.

DETERMINATION OF TRACE SULFUR AND SODIUM IN PSEUDO-BOEHMITE BY ICP-AES BASED ON MICROWAVE DIGESTION

2022, 53(7):  86-91. 

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A novel method was developed to determine trace sulfur and sodium in pseudo-boehmite commercial products by ICP-AES based on microwave digestion. Then the conditions of microwave digestion and interelement interference were investigated to optimize the microwave digestion procedure and accuracy of analysis. Finally, the standard curve for analyzing the content of sodium and sulfur was established. In the method, 0.1 g pseudo-boehmite was completely digested with 10 mL hydrochloric at the temperature of 185 ℃ in 50 min. The linear range of the standard curve for analyzing the content of sodium in solution by ICP-AES was 0.07-15.00 μg/g with a linear correlation coefficient of 1.000 00; relative standard deviation was 1.1%, and the recovery of the method was between 100.0% and 101.0%. The linear range of the standard curve for analyzing the content of sulfur in solution by ICP-AES was 0.10-35.00 μg/g with a linear correlation coefficient of 0.999 99; relative standard deviation was 1.1%, and the recovery of the method was between 95.0% and 100.0%. The method is suitable for the analysis of contents of sulfur and sodium in pseudo-boehmite commercial products with sodium of 35-7 500 μg/g and sulfur of 50-17 500 μg/g.

IMPROVING ESTIMATION EFFICIENCY OF LUMPED MODEL PARAMETERS FOR CONTINUOUS CATALYTIC REFORMING

2022, 53(7):  92-98. 

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The process simulations of continuous catalytic reforming needs high-efficient and accurate model. At present, the initial model is established by lumping according to the kinetic characteristics of the reactants, and the model is then estimated using laboratory or actual production data. However, because of the large difference in reaction rate between the lump components, the model has strong rigidity, which makes it difficult to estimate the parameters of the model and has the problems of time-consuming and poor convergence. In order to solve these problems, a quasi-steady-state assumption was proposed to simplify the calculation of the rigid components in the lumped model. The results show that this method can effectively simplify the lumped model for the 30 lumped model with continuous reforming band, and improve the estimation efficiency of model parameters.

STUDY ON TREATMENT TECHNOLOGY OF EXHAUST GAS OF OIL-PRODUCT DURING VEHICLE LOADING

2022, 53(7):  99-104. 

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On the basis of analyzing the characteristics of the exhaust gas of the oil-product during loading, through the comparative analysis of the exhaust gas treatment technology of the fuel trucks, the technology of low-temperature diesel absorption-total hydrocarbon concentration homogenization-catalytic oxidation was determined to treat the trucks loading exhaust gas in an enterprise in Shandong province. The results indicated that under the operating conditions of the absorption liquid gas ratio of 60-120 L/m³, the absorption temperature of 8-14 ℃, the absorption pressure of 0.2 MPa, the catalytic oxidation temperature of 350-410 ℃, and gas space velocity of catalytic oxidation of 5 000-20 000 h^-1, the mass concentrations of non methane total hydrocarbons, benzene, and toluene plus xylene in purified gas were less than 20 mg/m³, 0.001 mg/m³ and 0.003 mg/m³, respectively. The emission concentration of the purified gas pollutants can meet the requirements of environmental protection emission standards and the emission targets of grade an enterprises. The exhaust gas treatment device can recover 2 836.1 t/a VOCs and had certain economic benefits and obvious environmental protection benefits.

H₂S REMOVAL PERFORMANCE OF Fe/Cu WET OXIDATION DESULFURIZATION SYSTEM

2022, 53(7):  105-111. 

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In order to improve the efficiency of removing H₂S by wet oxidation, FeCl₃ and CuCl₂ were added into acidic N-methylpyrrolidone solvent to prepare bimetallic organic desulfurization system, and its viscosity, density, chemical structure and thermal stability were measured. The effects of metal salt concentration, temperature and regeneration time on desulfurization and regeneration efficiency were investigated, and the mechanism of desulfurization was analyzed. The results show that the organic wet oxidative desulfurization system containing Fe/Cu bimetallic salt has high efficiency, and the sulfur capacity of static desulfurization can reach 1.65 g/L at atmospheric pressure. The desulfurized product is high purity sulfur without by-products such as thiosulfate and sulfate, and there is no the problem of sewage discharge. Compared with traditional aqueous wet oxidation desulfurization agent, the Fe/Cu bimetallic salt organic desulfurization system has better economic benefits and environmental friendliness.

RESEARCH PROGRESS IN DEEP CATALYTIC CRACKING OF DECALIN TO LOW-CARBON OLEFINS

2022, 53(7):  112-121. 

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The reaction mechanism of decalin under the action of different types of catalysts is reviewed. Decalin is converted to free radicals by carboanion and then cracked by free radical mechanism under the action of lattice oxygen and adsorbed oxygen species on metal oxide catalysts. Decalin forms carbocation on the B acid center of solid acid catalyst, and then it reacts with a carbocation mechanism. Advantages and disadvantages of different pyrolysis catalysts were analyzed. The metal oxide catalysts were resistant to hydrothermal and high temperature, and could inhibit coking, but had no promoting effect on greatly decreasing reaction temperature and increasing propylene yield. Solid acid catalyst has acid center and unique pore structure, which can greatly reduce the reaction activation energy and flexibly adjust the proportion of low carbon olefins. Finally,the effects of different process conditions on decalin cracking reaction were listed.