Table of Content

12 December 2022, Volume 53 Issue 12

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HYDROTREATING TECHNICAL SCHEME OF CATALYTIC CRACKING LCO FOR COMPREHENSIVE UTILIZATION

2022, 53(12):  1-7. 

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Based on the analysis of hydrocarbon composition and heteroatom distribution in light cycle oil(LCO) from catalytic cracking unit, the different processing technology routes were proposed for different fractions of LCO. The analysis results show that aniline and indole nitrides in LCO are mainly distributed in the light and middle (<290 ℃)distillation section, while carbazole is mainly concentrated in heavy distillation section (>320 ℃). There is almost no thiophene sulfide in LCO, and the benzothiophene sulfide appears in the LCO fraction with initial boiling point over 290 ℃. Moreover almost all the sulfides in the heavy fraction belong to dibenzothiophene sulfide. The hydrotreating process results show that the full fraction of LCO requires severe conditions to achieve the increase of cetane number by hydrogenation reaction. The aromatics hydrogenation saturation in the middle fraction of LCO (240-320 ℃) under mild conditions could result in the 13.9 increase in cetane number of the product which could serve as the diesel blending components for China VI standard. The light fraction of LCO(<240 ℃) is suitable for catalytic cracking process to produce high-octane gasoline blending components.

INFLUENCE OF HIGH PROPORTION BLENDING CATALYTIC CRACKING SLURRY ON DELAYED COKER

2022, 53(12):  8-12. 

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In order to further solve the usage problem of catalytic cracking(FCC) slurry, the test of high-proportion blending of FCC slurry was carried out in the delayed coking unit of PetroChina Yunnan Petrochemical Company. The results showed that when the blending ratio of FCC slurry increased from 25% to 29%, the yield of petroleum coke decreased significantly, the yield of gas oil increased, and the yield of light oil and total liquid increased. The volatile matter and ash content of petroleum coke increased by 1.9 percentage points and 0.04 percentage point, respectively, and the sulfur content of petroleum coke decreased by 0.1 percentage point. The petroleum coke before and after high proportion blending could meet the 4A grade of enterprise standard. At the same time, it was found that the high proportion blending only accelerated the corrosion of the feed pump pipeline of the furnace, and had little effect on the process operation conditions of the coker. The economic benefit of processing per ton of raw materials was increased by 67.0 Yuan, indicating that it was feasible to blend FCC slurry with high proportion under the optimized scheme.

TECHNICAL ANALYSIS OF REPROCESSING MIXED WASTE OIL INTO DELAYED COKER

2022, 53(12):  13-18. 

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In view of the mixed waste oil with light, heavy and active chemical properties in the tank farm of a refining and chemical enterprise, the mixed waste oil was reprocessed in the furnace system of the delayed coker. The difficult problem of treating mixed waste oil was solved by the optimizing the technological process and analyzing the effect after putting into use. The results showed that after refining the mixed waste oil the yield of diesel increased by 2.59 percentage points, and the monthly average efficiency increased by 2.2807 million Yuan. The implementation of the mixed waste oil refining project of delayed coker is an exploratory innovation in the light oil treatment process of heavy oil unit, which has certain reference significance for the processing of ethylene tar in coker.

OPTIMIZING OPERATION OF CRUDE DISTILLATION UNIT TO REDUCE THE YIELD OF STRAIGHT-RUN DIESEL

2022, 53(12):  19-22. 

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At present, PetroChina Dushanzi Petrochemical Company mainly processes Kazakhstan crude oil, Karamay Mahu crude oil and South Xinjiang Yaha crude oil, and the designed yield of mixed diesel is 31%. In recent years, the demand for dieselin the market has been decreasing. In order to alleviate the high pressure on the refinery's diesel inventory and the shortage of naphtha directly supplying ethylene unit due to the less volume of the crude oil than before. Some outstanding contributions were made to improving the refinery overall operating efficiency by implementing the adjustment side line pumparound of atmospheric and vacuum distillation units, optimizing the operation of atmospheric distillation tower, which could lead to reducing the yield of straight-run diesel to 26.06% and optimizing the refinery's product distribution and improving the refinery's overall operating efficiency.

EFFECT OF OCTANE NUMBER PROMOTER MODIFIED WITH GALLIUM AND PHOSPHORUS ON AROMATIZATION PERFORMANCE

2022, 53(12):  23-30. 

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Octane number promoters were modified by the addition of gallium and phosphorus through impregnation. The catalyst was characterized by a series of analysis methods, and the performance of the catalyst was evaluated by a fixed fluidized bed reactor. The effects of gallium and phosphorus on the physical and chemical properties of the catalysts and on the selectivity of gasoline aromatics were investigated. The results showed that the aromatization ability of the catalyst modified with gallium could be improved and the octane number of gasoline could be increased. After the gallium modified catalyst was reintroduced with phosphorus, phosphorus interacts with gallium, which weakens the aromatization ability of the catalyst,but the increase of B acid center is beneficial to the increase of the selectivity of low-carbon olefins.

STUDY ON AROMATICS HYDROGENATION SATURATION PERFORMANCE OF Pt-Pd/SiO₂-Al₂O₃ CATALYST

2022, 53(12):  31-38. 

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The SiO₂-Al₂O₃ carriers with different SiO₂ contents were prepared by using the amorphous aluminosilicate with mass fraction of 40% SiO₂ and aluminum hydroxide gel as raw materials, and Pt-Pd/SiO₂-Al₂O₃ catalysts were prepared by equal volume impregnation method with chloroplatinic acid and palladium chloride as precursors of Pt and Pd. The prepared catalyst was characterized by N₂ adsorption-desorption, XRD, TPD, metallographic microscope, TEM and other methods. On a 10 mL fixed bed hydrogenation unit, the hydrogenation activity of the catalyst was evaluated with the model compound containing 2% tetralin + 10% decalin + 88% isooctane as the raw material. The results showed that the specific surface of the catalysts increased with the increase of SiO₂ content in the range of 20%-40%, the crystal phase composition remained unchanged, the amount of B acid and medium acid increased but L acid declined.The dispersion of Pt-Pd on SiO₂-Al₂O₃ carriers was gradually changed from eggshell type to homogeneous type,the degree of dispersion increased, and the hydrogenation activity of tetralin increased. With the increase of the concentration of hydrochloric acid in the impregnation solution, the dispersion of the catalyst first increased and then decreased. The Pt-Pd/SiO₂-Al₂O₃ active component had the best dispersion at the concentration of 0.1 mol/L hydrochloric acid, and the tetralin hydrogenation activity of the catalyst was the highest.

PREPARATION OF MOF-74 SUPPORTED PHOSPHOTUNGSTIC ACID CATALYST AND ITS CATALYTIC PERFORMANCE FOR OXIDATION OF CYCLOHEXENE TO ADIPIC ACID

2022, 53(12):  39-45. 

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With Cu²⁺ as the metal center, 2,5-dihydroxyterephthalic acid as the organic ligand and phosphotungstic acid (H₃PW₁₂O₄₀, PTA for short) as the active component, a series of PTA/Cu-MOF-74 catalysts (x%PTA@Cu-MOF-74, x=0, 10, 20, 30, 40）with x% PTA loading (w) were synthesized by one-step hot solvent method. The catalysts were characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy, nitrogen adsorption-desorption, and the catalytic activity of cyclohexene oxidation to adipic acid was tested. The results showed that the active component of PTA was successfully loaded into the Cu-MOF-74 skeleton, and the skeleton structure of MOF-74 remained intact. Under the reaction temperature of 80 ℃, reaction time of 6 h, the volume of cyclohexene of 1 mL, the volume of 30% H₂O₂ of 4.5 mL, and the dosage of 10%PTA@Cu-MOF-74 catalyst of 0.2 g, the yield of adipic acid was the best (61.96%), and the yield of adipic acid was 59.89% after the catalyst was reused for 4 times under the same test conditions, which was only 3.3% lower than that of using fresh catalyst.

RULES OF CATALYTIC CRACKING OF ALKYLBENZENE TO BENZENE

2022, 53(12):  46-52. 

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Using toluene, ethylbenzene, n-propylbenzene, n-butylbenzene, n-pentylbenzene and n-hexylbenzene as model compounds, the catalytic cracking reaction was carried out in a small fixed fluidized bed reactor to study the rule of benzene formation from alkylbenzenes with different side chain lengths under different reaction temperatures and using different zeolite (USY and REY) catalysts. The results showed that the yield of benzene from alkylbenzene was closely related to the carbon number of alkyl side chain under FCC conditions. The short side alkyl benzene mainly generates benzene through alkyl transfer reaction, and the long side alkyl benzene mainly generates benzene through dealkylation reaction. When the side chain carbon number is greater than or equal to 3, the selectivity of cracking products increases while benzene selectivity decreases. Low temperature is beneficial to inhibit the cracking of alkylbenzene to benzene,high acid density zeolite catalyst is conducive to reducing the dealkylation selectivity of long side chain alkylbenzene, and low acid density catalyst is conducive to reducing the conversion of alkylbenzene cracking to benzene.

SYNTHESIS AND ANALYSIS OF VISCOSITY REDUCTION MECHANISM OF AN OIL-SOLUBLE ANTICOSTIC AGENT

2022, 53(12):  53-58. 

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A new oil-soluble viscosity reducer SMN was synthesized in two steps from styrene, maleic anhydride, and nonylphenol polyoxyethylene ether, in order to reduce the viscosity and enhance oil recovery. The viscosity reduction effect of SMN on Shengli high viscosity crude oil was investigated. It was found that the maximum viscosity reduction rate could reach 68.5%. It was inferred that the polar groups such as benzene ring, carboxyl group and ester group in SMN could enter the asphaltene layer through hydrogen bond and π-π stacking, and the polyoxyethylene group with larger steric hindrance in the molecule could prevent asphaltenes from accumulating, thus dispersing heavy components in crude oil and reducing the viscosity of crude oil.

ADSORPTION AND CHEMICAL REDUCTION PERFORMANCE OF CARBON-SUPPORTED NANO-ZERO VALENT IRON PREPARED BY AEROSOL METHOD

2022, 53(12):  59-64. 

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Nano zero-valent iron (nZVI), as a new type of environmentally friendly material, is limited in the field of environmental pollution control due to its inherent instability and easy agglomeration. In this study, nano-zero-valent iron/carbon(Fe⁰/C) composites were prepared by using aerosol carbon as a carrier, and their effects on organic matter adsorption and nitrate reduction were studied. SEM results show that Fe⁰ is uniformly embedded in the inner and outer surfaces of spherical carbon in the form of nanoparticles, with a diameter ranging from 80 to 120 nm. Combined with BET and other characterization results, it is shown that Fe⁰/C composite has a high specific surface area. The results of adsorption and chemical reduction experiments showed that the maximum adsorption capacity of Rhodamine B was 853.7 mg/g, the removal rate of nitrate for 2 h was 50.6%, and 54.7% of the product was nitrogen, which proved the good reduction performance and practical application value of the composite material.

TECHNICAL DEVELOPMENT AND PERFORMANCE EVALUATION OF MOLYBDENUM DISULFIDE GREASE FOR LOW AND HIGH TEMPERATURE CONDITIONS

2022, 53(12):  65-69. 

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The development status of US standard MIL-G-21164D（grease，molybdenum disulfide，for high and low temperature）and foreign-related grease products and technology,domestic standards and product were introduced. The comprehensive physical and chemical performance of lubricating grease B developed by SINOPEC Research Institute of Petroleum Processing Co., Ltd. can meet the requirements of MIL-G-21164D specification.With high structural strength and viscosity,grease B has more suitable thixotropic behavior unde high temperature conditions. Pressure differential scanning calorimetry(PDSC) shows that its oxidation induction period is longer,and the high temperature oxdation thermal stability is better.

EFFECT OF LUBE BASE OIL ON ENGINE OIL TEOST 33C DEPOSITS

2022, 53(12):  70-76. 

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The main sources and chemical composition of TEOST 33C deposits, and the base oil properties influence on the TEOST 33C deposits were studied. The results show that TEOST 33C deposits formed mainly from the additives, mainly composed of oxygenated hydrocarbon compounds, also contain a small part of nitrides, calcium sulfate, phosphate, MoS₂, MoO₂ and molybdate.Base oil has a great influence on the amount and composition of TEOST 33C deposits.The TEOST 33C deposits weight from the oil containing HVIⅠ150 base oil is less than the oil containing HVI Ⅱ 4, HVI Ⅱ⁺ 4, or HVI Ⅲ 4 base oils. TEOST 33C deposit weight decreases as the base oil viscosity increases. HVI II 10 base oil greatly reduce the weight of TEOST 33C deposits. Increasing the polarity of base oil conduce to reduce the weight of TEOST 33C deposits.

PERFORMANCE COMPARISON AND STRUCTURE-ACTIVITY RELATIONSHIP OF DIFFERENT SULFURIZDE OLEFINS

2022, 53(12):  77-85. 

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Two sulfurized olefin lubricating additives (T321 and LZ5340) with different structures were selected to investigate their extreme pressure and anti-wear properties by using four-ball friction and wear testing machines, and their copper strip corrosion resistance were compared. The results showed that two sulfurized olefins could effectively reduce the friction coefficient and wear rate of the base oil, and significantly improve the extreme pressure performance of the oil. Among them, T321 is superior to LZ5340 in anti-friction, wear resistance and copper strip corrosion resistance, but its extreme pressure performance was slightly worse than that of LZ5340. The composition and structure of the additives were analyzed by infrared spectroscopy (IR), gas chromatography-mass spectrometry (GC-MS), element analyzer and nuclear magnetic resonance spectroscopy (NMR).It was found that the difference of components and active sulfur content had direct influence on the properties of sulfurized olefin. The structure-activity relationship of two sulfurized olefins with different structures was systematically investigated, which could provide guidance for the application of sulfurized olefin lubricating additives.

OPTIMIZATION ANALYSIS OF ENERGY CONSUMPTION OF DOMESTIC AROMATICS COMBINED PLANT

2022, 53(12):  86-90. 

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The aromatic production technology developed by SINOPEC has been successfully applied in large-scale chemical units of 600 kt/a and 1000 kt/a, breaking the long-term technical monopoly of foreign countries, in energy conservation and environmental protection to achieve substantial promotion and improvement. By comparing the energy consumption, raw materials, heat combination, low-temperature heat utilization, and the use of catalysts and adsorbents of the xylene unit in two domestic aromatic combined units, the methods and measures to reduce the energy consumption of the xylene unit were analyzed. The results showed that the heat utilization efficiency could be increased through direct heat transfer between materials by enhancing the combined heat utilization level of the xylene unit; the recovered low-temperature waste heat could generate steam or hot water, which was preferentially used in the compressor power drive medium, the rest was used for self-generation of electricity to minimize or avoid the use of external steam; comprehensive energy consumption of the xylene unit could be effectively reduced, and the benefit of the plant could be increased by using new generation of high performance catalysts and adsorbents.

TREATMENT OF GASIFICATION WASTEWATER FROM SE COAL WATER SLURRY BY SODIUM CARBONATE SOFTENING-STRIPPING AMMONIA REMOVAL PROCESS

2022, 53(12):  91-96. 

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The industrial operation effect of pretreatment of gasification wastewater from SE coal slurry by sodium carbonate softening-stripping ammonia removal process in a refinery was analyzed. The results showed that when the wastewater flow rate was 160 m³/h, pH of the wastewater was 10.5-11，the chemicals addition order of sedimentation tank was NaOH, Na₂CO₃, polymeric aluminium chloride (PAC), polyacrylamide (PAM), the steam flow rate of the stripper was 7.5-8.5 t/h, the pressure was 0.14-0.16 MPa, and the temperature at the column kettle was not more than 125 ℃, the discharge concentration of hardness and ammonia-nitrogen of wastewater could be reduced to 174 mg/L and 17 mg/L respectively, and the pollutant indexes were better than the design values.

SOLIDIFICATION OF HEAVY METAL IN WASTE CATALYTIC CRACKING CATALYST BY HIGH TEMPERATURE MELTING TECHNOLOGY

2022, 53(12):  97-101. 

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The high temperature melting technology was used to solidify the waste FCC catalyst. Three different fluxes, CaO, SiO₂ and CaF₂, were selected to investigate the effects of the fluxing agent type, addition ratio, reaction temperature and reaction time on the solidification of the waste catalyst. The results showed that three kinds of fluxing agents could cure the heavy metals Ni and V on the waste FCC catalysts, and the acid fluxing agent SiO₂ had the best effect. The surface microstructure showed that the catalyst with SiO₂ was smoother, more compact, and had no surface porosity, which was similar to the structure of vitreous body. The leached concentration of the heavy metals Ni and V in the cooling slag were 1.0 mg/L and 0.5 mg/L respectively when the addition of SiO₂ was 20%, the reaction temperature was 1 000 ℃ and the reaction time was 2 h. Increasing the reaction temperature and prolonging the reaction time could strengthen the immobilization of heavy metals Ni and V.

COMMERCIAL APPLICATION OF CASCADE RECOVERY TECHNOLOGY FOR HYDROGEN-RICH GAS

2022, 53(12):  102-105. 

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In view of the problem that a large amount of hydrogen-rich gas in the fully hydrogenation refinery enters the fuel gas pipeline network as low value fuel, a cascade recovery and utilization scheme of hydrogen-rich gas with different concentrations was proposed: the hydrogen-containing gas with low concentration was initially separated through the membrane recovery unit (phase II).The product hydrogen(phase II), dry gas from light hydrocarbon recovery unit and isomerization unit, and flare recovery gas were used as the raw materials of the membrane recovery unit(phase I) for secondary separation.The product hydrogen(phase I), the continuous reformer hydrogen, low pressure separation gas from residue hydrotreater, gas oil hydrocracker and diesel hydrogenation unit were thirdly separated by PSA to produce high purity hydrogen with 99.54% of hydrogen. The commercial application results showed that for a refinery with a processing capacity of 10.0 Mt/a, the hydrogen recovery was 13.1 kt/a, the natural gas consumption was reduced by 21.2 kt/a, the carbon emission was reduced by 150 kt/a, and the processing cost was reduced by 4.62 Yuan/t.

RAMAN SPECTRUM IDENTIFICATION METHOD FOR CLASSIFICATION OF LIGHT FUEL BASED ON SPARSE PRINCIPAL COMPONENT ANALYSIS

2022, 53(12):  106-113. 

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In order to achieve rapid on-site detection of common light fuel classification, five types of Raman spectra of 92# gasoline, 95# gasoline, 98# gasoline, 0# diesel and 3# jet fuel from different origins were collected. Normalization operator, Savitzky-Golay smooth convolution operator (SG) and adaptive iterative penalized least squares operator (airPLS) were successively used to preprocess the original spectrum. Then the sparse principal component analysis (SPCA) is applied to reduce the dimension of the preprocessed spectrum. Finally, the classification model is constructed by different methods to classify light fuel samples. The analysis results indicate that: the preprocessing of Raman spectrum can effectively eliminate the background noise interference and improve the accuracy of the classification model; the classification model constructed by sparse principal component analysis-support vector machine (SPCA-SVM) method has the best classification and identification effect on light fuel; the SPCA-SVM method is used to construct the classification model for distinguishing 95# gasoline from 92#gasoline + 95# gasoline blended gasoline, when the volume fraction of 92# gasoline in blended gasoline is more than 15 %, good recognition and classification results are achieved.

IMPROVEMENT OF SAMPLING METHOD IN STANDARD FOR DETERMINING SALT CONTENT IN CRUDE OIL

2022, 53(12):  114-118. 

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The sampling method of the industry standard “Determination of salt content in crude petroleum—Coulometrictitration method”(SY/T 0536—2008) is prone to entrap oil droplets or oil stains in the water alcohol extraction solution under the oil layer, which makes the accuracy and precision of the determination result worse. Theoil contaminationcan be effectively avoided in the water alcohol extraction solutionthrough the sampling methods using a polyethersulfone or polytetrafluoroethylene membrane needle filter, or using a centrifuge tube with an integrated tube cover for layering and using a 12 cm special long needle to insert and puncture the membrane seal at the bottom of the thin tube subsequently.At the same time, the sampling amount is increased by about 5 times, the representativeness of oil sample is improved, and the amount of extraction solution is increased accordingly to facilitate the selection of different detection methods for salt content.

PREPARATION OF ITACONIC ACID HOMOPOLYMER AND ITS ANTI-SCALE AND CORROSION-INHIBITION PERFORMANCE

2022, 53(12):  119-124. 

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A series of itaconic acid homopolymers (PIA) were synthesized by free radical polymerization in aqueous solution, using itaconic acid as monomer and initiator at different reaction temperature. The prepared PIAs were characterized by IR, gel permeation chromatography (GPC) and iodometry, and their anti-scale and corrosion-inhibition performance were evaluated. The results showed that the PIA with average molecular weight of 1 800-2 700 had excellent performance ,the anti-scale rate for CaCO₃ was more than 65%, and the corrosion-inhibition rate for carbon steel was more than 90% .