Table of Content

12 October 2020, Volume 51 Issue 10

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APPLICATION OF PETROLEUM COKE IN CEMENT INDUSTRY AND PROSPECT ANALYSIS

Ling Yiqun

2020, 51(10):  1-6. 

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The delayed coker is an important processing method for heavy and inferior residuum in refineries. In 2018, the total supply of petroleum coke in the world was 130 Mt, of which the petroleum coke with sulfur content greater than 3% accounted for 67.84% of the total production. Petroleum coke is widely used in cement, electrolytic aluminum, steel, glass, power plant and chemical industry. In 2018, the consumption of petroleum coke in the global cement industry was 39.2551 Mt, accounting for 30.09% of the total supply of petroleum coke. Cement enterprises in Europe, Japan, South Korea, India and other regions used petroleum coke in large quantities. Petroleum coke is widely used in electrolytic aluminum industry in China, reaching 18.3819 Mt in 2018, but only 0.4390 Mt in cement industry. When petroleum coke is used in cement production, most of its sulfur can be fixed in cement clinker in form of sulfate. In foreign countries, high sulfur petroleum coke can be used safely and environmentally as the fuel for cement kiln calcination to meet the local emission requirements. Through long-term cooperative pricing mechanism, cement enterprises can purchase petroleum coke with stable cost performance advantage, which improves the initiative of cement enterprises to utilize petroleum coke. By improving the performance price ratio, expanding the sales channels in cement industry and increasing the export intensity, the application scope of high sulfur petroleum coke can be widened, and the outlet problem of high sulfur petroleum coke in China can be solved under the premise of meeting the environmental protection regulations.

ADVANCES OF INHIBITION AND PLUG REMOVAL TECHNOLOGY FOR ASPHALTENE DEPOSITION

2020, 51(10):  7-15. 

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There are many living examples of asphaltene deposition in crude oil all over the world, which bring great difficulties to crude oil exploitation and post-treatment. It is of great significance to study asphaltene deposition inhibition technology and unblocking technology. The inhibition technologies of asphaltene deposition in oil wells are reviewed, including adjusting production parameters and adding chemical inhibitors, such as natural fatty acid organic compounds, surface active substances containing benzene rings, processed products of vegetable oils or oils, ionic liquids and metal oxide nanoparticles. The plugging removal technology of asphaltene deposition is introduced, including mechanical method, chemical method, thermal method, biological method, external force field, composite plugging removal method. The future development trends of asphaltene deposition inhibition and plug removal technology are analyzed. It is necessary to evaluate, analyze and predict oil wells or pipelines in advance, and study the mechanism of sedimentation inhibition and plug removal in depth, clarify the adaptability of different technologies, and strengthen the research and application of composite plug removal technology.

REVAMPING AND OPERATION OF FIXED BED RESIDUE HYDROTREATING UNIT FOR LONGER OPERATION CYCLE

Shao Zhicai Deng Zhonghuo Liu Tao Dai Lishun

2020, 51(10):  16-22. 

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The residue hydrotreating pilot tests were carried out at 14.5 MPa, 385 ℃ and 390 ℃, LHSV of 0.20，0.30，0.40 h-1, and H2/oil of 700, respectively, using the Middle-East high sulfur AR as feedstock.The results showed that the sulfur content，carbon residue，metal (Ni+V) content and nitrogen content of the hydrogenated oil were all reduced as the LHSV decreased under the other process conditions unchanged. Furthermore, two sets of industrial fixed-bed residue hydrogenation units were revamped. For refinery A，adding an upflow reactor in front of the original fixed bed first reactor made the capacity of the unit increase from 0.84 Mt/a to 1.5 Mt/a. During 9th operation cycle(RUN-9)，the sulfur content in the hydrotreated residue was less than 0.5%, nitrogen was between 0.2% to 0.3%，metal (Ni + V) content below 15 μg/g，and Conradson carbon residue between 3% to 5%. Time on stream（TOS）was prolonged from 240 d to 480 d. For refinery B，a fixed bed reactor was added after the original second reactor of the fixed bed system，the LHSV of the unit decreased from 0.4h-1 to 0.25 h-1. Compared with RUN-9 results before the revamp, HDS rate in RUN-12 was slightly increased，while the HDCCR rate，HDM rate and HDN rate were all significantly increased. TOS of the unit was prolonged from 335 d to 518 d.

PROBLEM OF DOCTOR TEST FOR HYDROCRAKING LIGHT NAPHTHA AND COUNTERMEASURES

2020, 51(10):  23-27. 

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The light naphtha from the hydrocracking unit of PetroChina Dushanzi Petrochemical Company is used as a blending component of vehicle gasoline. At the initial stage of plant start-up, the sulfur mass fraction of the light naphtha was no more than 3.5 μg/g, with the mercaptan sulfur content less than 3 μg/g, but sometimes the doctor test failed. To solve this problem, different active sulfides in light naphtha were analyzed qualitatively and quantitatively. The results showed that the main reason for the failure of the doctor test was the synergy of trace amounts of hydrogen sulfide (no more than 0.5 μg/g) with mercaptan in samples, as long as the hydrogen sulfide was removed, the doctor test could pass. Based on this, some feasible industrial solutions were put forward, such as optimizing the operation of light naphtha fractionation system, stripping by reboiled gas instead of steam stripping in light naphtha fractionator, and using the adsorptive desulfurization or sweetening process.

EFFECT OF REACTION TEMPERATURE ON COAL-OIL CO-PROCESSING UNDER MILD CONDITION IN HYDROGEN

2020, 51(10):  28-31. 

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The effects of reaction temperature on coal-oil co-processing were studied using FCC slurry and three kinds of coals from different resources in autoclave under mild hydrogen pressure. The results showed that the liquefaction rate first increased and then decreased, the yield of gasoline (<200℃) decreased，diesel（200-350℃）increased, >350℃ residue yield first increased and then decreased while the ash content gradually increased with the increase of temperature. The changing trends of volatile matter and fixed carbon in the semicoke were dependent on coal from different sources, but mainly related to the reaction severity, raw material properties, formation rates and transformation rates of different components during the complex parallel-sequential reactions.

INDUSTRIAL PRACTICE OF VGO HYDROGENATION UNIT TO PRODUCE CHINA Ⅴ DIESEL

2020, 51(10):  32-35. 

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In order to solve the problem that diesel cannotbe sold during shutdown and catalyst replacement of diesel liquid phase circulating hydrogenation unit, SINOPEC Shijiazhuang Refining and Chemical Company produced the China Ⅴ diesel through VGO hydrogenation unit. The results showed that the sulfur content of diesel product was 3 μg/g under the conditions of a capacity of 175 t/h , a reactor inlet temperature of 352 ℃,a reaction pressure of 9.4 MPa, a hydrogen oil volume ratio of 500, a space velocity of 0.97 h-1, a fractionator bottom temperature of 222 ℃ and a top pressure of 0.11 MPa. During the operation, it was found that the cold high pressure separator and the heating furnace were overloaded, the outlet temperature of the tail oil from the unit was on the high side, and the diesel water content was also high. These problems were well resolved. The results of industrial practice can provide data support and basis for transformation of the unit for the production of China Ⅴ diesel fuel.

INITIATION PROCESS OF WAX OXIDATION AND INTERFACIAL PROPERTIES OF PRODUCT

2020, 51(10):  36-41. 

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The oxidation modification of wax through free radical chain reaction initiated by lauryl hydrogen peroxide under relative mild conditions was studied using 58# fully-refined paraffin wax as raw material, air as oxidant and lauryl as initiator. The effect of reaction temperature and time, the amount of the initiator and the air flow on the acid number and saponification value of the oxidized wax were investigated. The results showed that at the optimized reaction conditions of a temperature of 130 ℃, a reaction time of 6 h, a initiator amount of 0.5%, and a air flow of 220 mL/min, the acid mumber and saponification value of the oxidized product were 40.5 mgKOH/g and 65.3 mgKOH/g, respectively. The binary system consisted of 0.8% oxidized product and 1.2% sodium hydroxide used for oil-displacing system had an interfacial tension of 2.9×10-3 mN/m with crude oil, and the oil removal rate at the surface of sandstone was 61.0%, indicating the excellent oil-water interface properties of paraffin oxidation product.

CAUSE ANALYSIS AND COUNTERMEASURES OF HIGH PRESSURE DROP OF DECHLORINATING AGENT BED FOR REFORMATE

2020, 51(10):  42-45. 

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During the first application of molecular sieve type liquid phase dechlorination agent in a 2.2 Mt/a continuous reforming unit of a refinery, it was found that the pressure drop of dechlorination agent bed was increasing, which made the operation of downstream depentanizer difficult. The analysis of the waste dechlorination agent indicated that the large molecular aromatics in reformate blocked the micropores of the molecular sieve, leading the pressure drop rising. A small amount of molecular sieve with large diameter and large pores dechlorination agent loaded on the top of the dechlorination bed can effectively solve the problem. At the same time, it is proposed that attention should be paid to the control of the final boiling point and nitrogen content of the reformer feed.

STUDY ON SO2 ADSORPTION PERFORMANCE OF HY MOLECULAR SIEVES

2020, 51(10):  46-52. 

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Three HY molecular sieves HY-1，HY-2，HY-3 with different ratios of Si/Al were used as adsorbents to perform experiments of SO2 adsorption in a fixed bed device. The relationship between saturation adsorption capacity and Si-Al ratios of the sieves was investigated. Physicochemical properties of HY molecular sieves were characterized by BET，XRD，XRF，CO2/O2-TPD techniques and correlated with SO2 saturated adsorption capacity. It was shown by the results that with the increase of Si/Al ratio, the SO2 penetration time of molecular sieves HY-1, HY-2 and HY-3 decreased in turn, and the saturated adsorption capacity decreased in turn, indicating that increasing Si/Al ratio is not conducive to adsorption of SO2 by HY molecular sieves and that the SO2 saturation adsorption capacity of HY molecular sieve was directly proportional to the basic content on its surface. It was found that the adsorption performance of molecular sieve for SO2 is directly related to the species and content of oxygen on its surface. With the increase of Si/Al ratio, the content of chemically adsorbed oxygen on HY molecular sieve surface decreased in turn for the three sieves, and the amount of chemically adsorbed SO2 decreased in turn.

STUDY OF HYDROCARBON STRUCTURE ORIENTATION FOR HEAVY OIL FEEDSTOCK TO PRODUCE MORE CHEMICALS

2020, 51(10):  53-59. 

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The chemical transformation of petroleum refining and the proportion of intermediate crude oil supply have a tendency to increase continuously. However, the content of heteroatoms such as sulfur, nitrogen and heavy metals in intermediate base inferior residual oil is high, and there are many hard-to-crack heavy components such as polycyclic aromatic hydrocarbons, resins and asphaltenes, which bring challenges to the way of producing more chemicals and need to be upgraded by pretreatment processes such as hydrotreating. Based on the research of heavy oil molecular level composition, hydrocarbon molecular structure and catalytic cracking reaction chemistry, it is proposed that the best raw material hydrocarbon composition structure for chemicals production is paraffin, cycloalkanes and alkylbenzenes, which needs a good residue hydroupgrading coupling with catalytic cracking. The direction of hydrogenation upgrading of intermediate residue should be super-deep hydrogenation saturation of condensed aromatic hydrocarbons and moderate cracking. The changes of hydrocarbon composition structure of intermediate base residue before and after hydrotreating characterized by molecular level showed that the polycyclic aromatic hydrocarbons, thiophene-type sulfur-containing aromatic hydrocarbons, resins and asphaltenes were directionally converted into the dominant ideal hydrocarbon structure by deep hydrotreating for producing more chemicals, such as paraffins and cycloalkanes, especially monocyclic-tricyclic cycloalkanes. Furthermore, the coupling with highly selective catalytic cracking technology can achieve the goal of producing more chemicals such as light olefins and BTX from inferior intermediate base residue.

STUDY ON ADSORPTION AND DESORPTION BEHAVIOR OF THIOPHENE ON Ni-Mo-W/γ-Al2O3 CATALYST BY IN-SITU INFRARED SPECTROSCOPY

2020, 51(10):  60-64. 

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In order to improve hydrodesulfurization catalysts and production processes, the in-situ diffuse reflectance infrared spectroscopy was used to study the sulfidation performance of Ni-Mo-W/γ-Al2O3 catalyst and adsorption behavior of thiophene. The results showed that Ni-Mo-W/γ-Al2O3 catalyst surface was sulfided at 320 ℃, and the thiophene adsorption test at 400 ℃ sulfidation for 1 h found that during in-situ temperature programmed desorption process of sulfided catalyst, the characteristic peak at 1 558 cm-1 (C=C stretching vibration) disappeared at 150 ℃; characteristic peak at 1 575 cm-1 (C=C stretching vibration), and 1 413 cm-1, 1 396 cm-1 (C-H bending vibration) disappeared at 250 ℃; the thiophene adsorption characteristic peaks at 1 537 cm-1, 1 513 cm-1 (C=C stretching vibration) and 1 340 cm-1 (C-H bending vibration) strengthen; characteristic peaks at 1 700, 1 679 cm-1 (C=C stretching vibration) disappeared at 350 ℃, indicating different adsorption way of thiophene. The experimental data provides basis for design and development of higher active HDS catalysts with different sulfur removal pathway.

STUDY ON PORE STRUCTURE OF SEMI-SYNTHETIC AND IN-SITU CRYSTALLIZATION FCC CATALYSTS

2020, 51(10):  65-69. 

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Two catalytic cracking catalysts (numbered LDO-75, LB-5) prepared by semi-synthesis process and in-situ crystallization process were respectively subjected to high temperature hydrothermal treatment (numbered LDO-75-T, LB-5-T). The pore structures and hydrothermal stabilities of the two catalysts before and after high temperature hydrothermal treatment were investigated. The results showed that the pore volume and specific surface area of LB-5 were 0.35 cm3/g and 307.3 m2/g, respectively, higher than those of LDO-75 with 0.27 cm3/g and 214.1m2/g. The most probable pore size of LDO-75 and LB-5 were 3.8 nm and 6.3 nm, respectively. Although the crystallinity of Y zeolite in LB-5 catalyst was similar to LDO-75 catalyst, the microporous specific surface area of LB-5 was 216.0 m2/g, which was significantly higher than LDO-75. The microporous surface area retention rates of LDO-75 and LB-5 were 44.4% and 25.1%, respectively, after hydrothermal treatment, which indicated that LB-5 had unstable microporous structure. After hydrothermal treatment, the pore volume around 3.8 nm pore diameter of LDO-75-T increased, the pore volume around 6.3 nm of LB-5-T decreased, while that in range of 10-50 nm diameters increased.

EFFECT OF RESIN ON ASPHALTENE STABILITY

2020, 51(10):  70-76. 

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It is generally acknowledged that the particle size of the deposit reflects the influence of resin on the stability of asphaltene. To further study the effect of the interaction between resin and asphaltene on the stability of asphaltene, based on the analysis of the average structural units of asphaltene and resin and the calculation of solubility parameters, resin NBR and resin VRR were added into a asphaltene model oil (its deposit known as AS deposit), resulting in the AS + NBR and AS + VRR deposits, respectively. The results showed that asphaltene had the strongest aromaticity and the largest solubility parameter (20.61 MPa1/2), and the aromaticity and solubility parameter (17.80 MPa1/2) of resin VRR was higher than that of resin NBR. In asphaltene model oil, with the increase of the mass concentration of VRR, the sediment particle size decreased. The addition of NBR did not make the deposit particle size smaller, but when the mass concentration reaches 1 000 mg/L, the sediment particle size increased instead. The results of TGA, XRD and GPC of three deposits showed that there was association between resin and asphaltene, which decreased the thickness and diameter of aromatic lamellae, increased the interlayer space, and decreased the number of aromatic lamellae. The order of the relative molecular weight of the three deposits was AS > AS + NBR > AS + VRR. It is concluded that the resin VRR, which has strong aromaticity and solubility parameter close to asphaltene, can disperse and stabilize asphaltene better, make the particle size and molecular weight of deposit smaller, and the degree of graphitization smaller, so it is not easy to deposit and coking.

INDUSTRIAL APPLICATION OF REFORMING CATALYST SR-1000

2020, 51(10):  77-80. 

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Semi-regeneration catalytic reforming catalyst SR-1000 developed by SINOPEC Research Institute of Petroleum P rocessing was applied in a 450 kt/a reforming unit of Refinery and Chemical Industry Corporation of Yumen Oilfield Company of PetroChina. The operation results of nearly 400 days showed that the octane number RON of C5+ stabilized gasoline is 94.0 and the yield was 89.2% at a WABT of 468℃, which indicates that SR-1000 catalyst has better activity and selectivity. Under the condition that the raw material properties and reaction severity were basically the same, the performance of SR-1000 catalyst was better than that of PRT-C/PRT-D reforming catalyst and can meet the needs of long-term stable operation of semi-regeneration catalytic reforming unit. The start-up method of SR-1000 catalyst is simple, safe and environmentally friendly.

STRUCTURE AND PROPERTY ANALYSIS OF POLYISOBUTYLENE AND ITS DERIVATIVES

2020, 51(10):  81-88. 

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As an intermediate in the preparation of ashless dispersant, the structure and properties of polyisobutylene succinic anhydride (PIBSA) were the critical factor of subsequent amination reactions. The structures of polyisobutylenes with different activities prepared by two catalytic processes (BF3和AlCl3) and of PIBSA prepared by different alkylation processes (chlorination and thermal addition) were characterized by IR and 1H NMR to study the systhetic reaction mechanism. The ashless dispersants were prepared by further amination of two PIBSAs. The dispersity of low temperature sludge, high temperature cleanness and soot dispersability of the ashless dispersants were compared and analyzed. The results indicated that the structures of PIBSAs prepared by two alkylation processes were great different due to the difference of polyisobutylene structures and reaction principles. The end of PIBSA prepared by thermal addition method was mainly composed of grafted monopentacyclic anhydride structure, while at the end of PIBSA prepared by chlorination method, phthalic anhydride structure was predominant. Two different structures had a great influence on the performance of ashless dispersants. The ashless dispersant DL prepared by chlorination of PIBSA and the ashless dispersant DR prepared by thermal addition of PIBSA had a similar low-temperature oil sludge dispersibility. The high temperature detergency of DL was better than that of DR, while the soot dispersibility was slightly worse than that of DR.

CHANGES OF TRIBOLOGICAL PROPERTIES OF MANUAL TRANSMISSION FLUID BEFORE AND AFTER SYNCHRONOUS DURABILITY TEST

2020, 51(10):  89-93. 

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The changes of physical and chemical tribological properties of two kinds of manual transmission oils before and after SSP180 synchronous durability test were evaluated by MRS-1J four-ball tester, SRV testing machine and EHD2 oil film thickness tester. The results indicated that the physcochemical properties of the sampes were basically unchanged before and after the test. The four-ball friction coefficient of the oils that can pass SSP180 synchronous durability bench test (100000 cycles)was kept at about 0.10, the SRV friction coefficient was kept at about 0.14, the maximum non seizing load, the four-ball mill spot diameter, the SRV horizontal, vertical, and average wear spot diameter had no obvious changes. The oil film thickness after durability test kept well with the increase of test speed. The four-ball friction coefficient and SRV friction coefficient of the oils that could not pass the SSP180 synchronous durability bench test decreased after the synchronous durability test and before the test. With the extension of the test time, the SRV friction coefficient of the two samples before and after the test decreased from 0.16 to 0.09 and 0.15 to 0.07, respectively. The stability of oil film, the size and stability of friction coefficient were the important factors that affect whether the oil could pass the ssp180 transmission synchronous durability test.

CLUSTER ANALYSIS OF S ZORB UNIT FEEDSTOCKS

2020, 51(10):  94-99. 

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S Zorb process is one of the main technologies to remove sulfur in fluid catalytic cracking gasoline. Based on the feedstock property data from a S Zorb gasoline adsorption desulfurization unit for 4 years, the characteristics and reaction mechanism of S Zorb process，the saturated hydrocarbon content, olefin content, aromatic content, sulfur content, density, and bromine number of the feedstocks were selected as the feedstock clustering variables. K-means and fuzzy C-means clustering algorithms were used to cluster the feedstocks by MATLAB programming platform. The results showed that both the K-means and fuzzy C-means clustering algorithms have a good classification effect on the feedstocks of the S Zorb unit and they both classify the raw oil into three categories. On this basis, the octane number prediction models can be established for different kinds of raw oils, which can provide guidance for finding the operating conditions to reduce the octane number loss of gasoline of S Zorb plant.

APPLICATION OF PSO-SVR-RSM METHOD IN STRUCTURE OPTIMIZATION OF GAS-LIQUID DISTRIBUTOR OF HYDROGENATION REACTOR

2020, 51(10):  100-105. 

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CFD in designing and optimizing the structure of the trickle bed gas-liquid distributor have the disadvantages of the slow speed and high calculation time cost. In this paper, we selected the support vector regression machine (SVR) model as the proxy model for prediction. In order to obtain a fast and accurate SVR model, the particle swarm optimization (PSO) algorithm was used to optimize the parameters of support vector regression (SVR), including the penalty coefficient C, the parameter g of the kernel function, and the insensitive loss coefficient ε. Then, using the PSO-SVR hybrid model as the data source coupled with the response surface method (RSM), the structural parameters corresponding to the minimum liquid uneven distribution were calculated. The CFD results showed good agreement with the values predicted by the response surface method, and the liquid distribution unevenness was 0.159 and 0.162, respectively. The research shows that the hybrid PSO-SVR-RSM method provides an effective tool for guiding the optimal design of gas-liquid distributors in trickle beds.

CAUSE ANALYSIS AND COUNTERMEASURE OF EMULSIFICATION OF PRODUCED FLUID IN BINARY COMPLEX FLOODING

2020, 51(10):  106-111. 

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The produced fluid of binary complex flooding in Shengli Oilfield of SINOPEC was analyzed, and the state of polymer, petroleum sulfonate and surfactant at oil-water interface was investigated by molecular simulation method. The cationic polymer water purification agent was developed in laboratory and tested in Dongyi union station in Gudong oil production plant in Shengli Oilfield. The result showed that the oil content in the 1st settling tank decreased from 1900 mg/L to 1050-1250 mg/L, the oil content of external sewage was qualified, and the expected effect was achieved.

INDUSTRIAL APPLICATION OF ANOXIC/OXIC FLUIDIZED BED BIOFILM REACTOR FOR COAL TO EG WASTEWATER TREATMENT

2020, 51(10):  112-117. 

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The wastewater from coal to ethylene glycol is a typical coal chemical wastewater, which is difficult to be treated stably by conventional biochemical treatment and has high operation cost. The A/O fluidized bed biofilm reactor has the characteristics of high microbial concentration, high volume load and sludge load, fast mass transfer, strong impact load resistance and good treatment effect. The A/O fluidized bed biofilm reactor developed by SINOPEC(named A/O SFBBR) was used to treat glycol wastewater. The treating effects of operating conditions, such as C/N, HRT and nitrate liquid reflux ratio, were investigated. The economic technique analysis for SFBBR and traditional A/O reactor were compared. The results showed that: (1) the performance of SFBBR was best when the C/N was in the range of 3.5 to 5.0, the hydraulic retention time (HRT) of aerobic reactor was in the range of 10 to 21h and the nitrate reflux ratio was in the range of 1.5 to 4.5; and the average COD, NH4--N and TN concentration of the effluent were 18.3 mg/L, 4.7 mg/L and 19.3 mg/L, respectively; (2) compared with the traditional A/O reactor, the SFBBR exhaust gas emission reduced by about 80%, waste produced sludge reduced by about 43%, the project investment decreased by about 16%, and the operating cost reduced by 30% approximately.

TECHNICAL AND ECONOMIC ANALYSIS OF S Zorb UNIT

2020, 51(10):  118-122. 

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The technical and economic characteristics of gasoline adsorption desulfurization unit (S Zorb) were analyzed in terms of investment, cost, financial benefit, industry and social benefit; the ways to reduce the operating cost of the unit were discussed, and the sources and compositions of good economic benefit and great industry and social benefit of the unit were revealed.