Deep-Cut Vacuum Distillation in the 10 Mt/a CDU/VDU

This article introduces the concepts relating to deep-cut vacuum distillation and its suitability,and analyzes the deep-cut vacuum distillation technique licensed by the KBC Advanced Technologies to the 10 Mt/a CDU/VDU of the Qingdao refinery and makes comparison on the test run data after commissioning of the distillation unit. The test results have confirmed that the operation of the CDU/VDU had reached the expected goal to achieve good social and economic benefits.

Thermodynamics of removing impurities from crude lead by vacuum distillation refining

A novel technique was developed to remove impurities from crude lead by vacuum distillation.The thermodynamics on vacuum distillation refining process of crude lead was studied by means of saturated vapor pressure of main components of crude lead,separation coefficients and vapor-liquid equilibrium composition of Pb-i（i stands for an impurity） system at different temperatures.The behaviors of impurities in the vacuum distillation refining process were investigated.The results show that the vacuum distillation should be taken to obtain lead from crude lead,in which Zn,As and partial Sb are volatilized at lower temperature of 923-1023 K.Lead is distilled from the residue containing Cu,Sn,Ag and Bi at higher temperature of 1323-1423 K,but the impurity Bi is also volatilized along with lead and cannot be separated from lead.

Application of molecular interaction volume model in separation of Pb-Sn-Sb ternary alloy by vacuum distillation

Based on the molecular interaction volume model （MIVM）, the activities of components of Pb Sn Sb ternary alloy were predicted. The vapo^liquid phase equilibrium of Pb-Sn-Sb alloy system was calculated using the activity coefficients of Pb Sn-Sb alloy system in the process of vacuum distillation. The calculated results show that the content of Sn in vapor phase increases with the increasing distillation temperature and content of Sn in liquid phase. However, the content of Sn in vapor phase is only 0.45% （mass fraction） while 97% in liquid phase at 1100 ℃, which shows that the separating effect is very well. Experimental investigations on the separation of Pb-Sn-Sb ternary alloy were carried out in the distillation temperature range of 1100-1300 ℃ under vacuum condition. It is found that the Sn content in vapor phase is 0.54% while 97% in liquid phase at 1100 ℃. Finally, the predicted data were compared with the experimental results showing good agreement with each other.

STUDY ON CONCENTRATING SULFURIC ACID SOLUTION BY VACUUM MEMBRANE DISTILLATION

Concentrating sulfuric acid solution by vacuum membrane distillation with flat PEFE membrane is explored. The effects of sulfuric acid concentration, temperature of the feed, the vacuum degree of the vacuum side on the flux of membrane distillation and the separation efficiency of acid are investigated. The results illustrate that the flux of the membrane distillation increases with the rise of feed temperature and the vacuum degree of the vacuum side, but it decreases with the rise of the sulfuric acid concentration of the feed. The separation efficiency of acid is correlated with the flux of membrane distillation; the separation efficiency of the acid can amount to 100% in the process, when operative conditions are properly controlled. It can also been obtained from the experiment that, compared with other methods of membrane distillation, the vacuum membrane distillation can obtain greater distillation flux.

Study on the Removal of MIBK from Aqueous Solution by Vacuum Membrane Distillation

Methyl isobutyl ketone(MIBK) is widely used as extraction agent in hydrometallurgy. As it has a definite solubility in water, so when using MIBK as extraction agent, there will be MIBK in stripping solutions inevitably, which not only pollutes working conditions, but also affects the quality of ultimate product. In order to remove MIBK from aqueous solutions, the means of flat vacuum membrane distillation(VMD) is studied in the paper. The area of the membrane used in the study is 0.02 m 2, the initial volume of feed is 2 L, each experiment was conducted over a time period of 60 120 min. The influences of the factors such as temperature(34.8 55.0 ℃); pressure in the permeate side(10.67 14.67 kPa) and feed flow rate(27.8 69.4 mL/s) were experimentally studied. Increasing the temperature or reducing the pressure in the permeate side results in a faster removal of MIBK; however there is a decrease in removal factor β , increasing the feed flow rate results in a faster removal of MIBK and an increase of removal factor β , especially in the range of lower flow rate. The study indicates that the aim of MIBK removal and recycle from dilute aqueous solutions can be achieved by VMD.

Application of vacuum distillation in refining crude indium

Vacuum distillation is a technique suitable for low boiling and melting point materials,to remove the heavy and low vapor pressure impurities at low level.As indium has low melting point and high boiling point,it is suitable for refining by vacuum distillation.First,saturation vapor pressure for major elements in crude indium was calculated by the Clausius–Clay Prang equation,which could approximately predict the temperature and pressure during vacuum distillation process.Second,the activity coefficients for In–Cd,In–Zn,In–Pb,In–Tl at 1373 K,and In–Sn at 1573 K were acquired by means of molecular interaction on volume model.Vapor–liquid equilibrium composition diagrams of those above systems in crude indium were drawn based on activity coefficients.These diagrams could estimate the compositions of products in each process during the refinement of crude indium.Finally,1.2–1.6 ton crude indium was used per day when vacuum distillation experiments were carried out,and experimental results are in good agreement with the predicted values of the vapor–liquid equilibrium composition diagrams.

Hydrochloric acid recovery from rare earth chloride solutions by vacuum membrane distillation

The possibility of the recovery of hydrochloric acid from rare earth （RE） chloride solutions was first experimentally studied by batch vacuum membrane distillation （VMD）. The recovery by continuous VMD was also studied to devise methods that enabled the operation of VMD setup in a stable condition as well as to increase the membrane-operating life The results indicated that HCl separation with RE by VMD was possible, and the recovery ratio of 80% could be achieved by batch VMD. In continuous VMD, when the temperature of circular solutions, circular rate, and downstream pressure was 62-63℃, 5.4 cm/s, and 9.33 kPa, respectively, the HCl concentration in circular solutions and the processing capacity per membrane area were obtained. The mathematical results were in accordance with the experimental ones.

Pretreatment of lead anode slime with low silver by vacuum distillation for concentrating silver

The feasibility of separation of lead anode slime with low silver by vacuum distillation was analyzed theoretically. The volatilization rates and mass fractions of elements, influenced by distillation temperature, heat preservation time and material thickness, were investigated under laboratory conditions. The experimental results indicate that almost all of lead and bismuth can be separated from silver-contained multicomponent alloy at 1 223 K for 45 min when the chamber pressure maintains at 10-25 Pa. Silver can be easily enriched in the residue and its mass fraction increases from 3.6% to 27.8% when the distillation temperature is between 1 133 K and 1 373 K. Due to the forming ofintermetallic compounds Cu2Sb, Cul0Sb3 and Ag3Sb, the antimony could not be evaporated completely during the vacuum distillation. EDS analysis indicates that the condensate has a columnar crystal structure.

Hydrochloric Acid Recovery from Rare Earth Chloride Solutions by Vacuum Membrane Distillation (1) Study on the Possibility

The equilibrium between the gas-liquid phases of the system of HCl-RECl_3-H_2O was analyzed,and the possibility of hydrochloric acid recovery from rare earth chloride solutions by vacuum membrane distillation (VMD) was experimentally studied in the laboratory scale. The results indicate that increasing initial concentrations of both hydrochloric acid and rare earth increase recovery ratio of hydrochloric acid,and recovery ratio of 80% can be achieved. Concentrated multiple of rare earth shows great influence on recovery ratio,leakage ratio of rare earth is less than 2% generally,and pure acid can be acquired in the permeate side. The two factors,namely flux and leakage ratio,which may determine the future use of VMD were also discussed.

Emission-Reductive and Multi-Objective Coordinative Optimization of Binary Feed for Atmospheric and Vacuum Distillation Unit

A genetic algorithm based multi-objective coordinative optimization strategy is developed to optimize the operation of a binary feed atmospheric and vacuum distillation system, in which the objective functions cover the economic benefit, the furnace energy consumption and the CO_2 emissions, and meanwhile the simultaneous effect of binary feed composition is also investigated. A cross-call integration of software is developed to implement the optimization algorithm,and once the maximum economic benefit, the minimum furnace energy consumption and the minimum CO_2 emissions are obtained, the Pareto-optimal solution set is worked out, with the practical problems of the refinery being solved. The optimization result shows that under the same furnace energy consumption and the CO_2 emissions as the existing working condition, the economic benefit still allows for a considerable potential of increment by adjusting the heavy oil proportion of the binary feed crude oil.

Impurity distribution in distillate of terbium metal during vacuum distillation purification

The distribution rules of impurities in distilled terbium metal were investigated by vacuum distillation purificationexperiment and theoretical analysis.It is found that Ti impurity in distilled terbium is220mg/kg in the initial stage of the distillationpurification,increases slowly in the middle stage,and increases rapidly in the last stage,reaching2260mg/kg,and the modifiedseparation coefficient of Ti is1/19.02.The diffusion of the impurity Ti in liquid metal can reach a quasi-equilibrium state in theinitial stage of distillation purification and the calculated results agree well with experimental results;the distribution profile ofimpurity Cu is opposite to Ti,being380mg/kg in the initial stage,decreasing linearly to290mg/kg in the last stage,and themodified separation coefficient is17.99,and the theoretical calculated results are inconsistent with the experimental result.

Purification of indium by vacuum distillation and its analysis

High purity （99.999% or 5N, mass fraction） indium （In） was obtained through vacuum distillation using a 2N （99%） In as input material under a dynamic vacuum of 5 Pa. The glow discharge mass spectrometry （GDMS） was applied for the analysis of input material and the distilled indium. The results indicate that high-volatile impurities namely Cd, Zn, T1 and Pb can be removed from the indium matrix at the low fraction stage of 1 223 K for 120 min; Low-volatile impurities such as Fe, Ni, Cu, Sn can be reduced at the high fraction stage of 1 323 K for 120 min. The separation coefficient ,8i and activity coefficient Yi of impurities are calculated according to the experiments to fill the inadequate data of the thermodynamics.

Removal of aqueous phenol compound by vacuum membrane distillation

The effects of feed temperature and pH value on the removal of aqueous phenol wastewater by vacuum membrane distillation process are studied by experiments employing micro porous membranes of poly vinylidene fluoride (PVDF) and ploy tetrafluoro ethylene (PTFE) with nominal average pore sizes 0.22 mm and 0.20 mm, respectively. It is found that the optimal feed temperature for PVDF membrane is 50 ℃; and for PTFE membrane, 60 ℃. The pH value of the feed has little influence on the membrane fluxes and ion rejection ratios, while it influenced considerably on the selectivity. Increase of pH value of the feed is conducive to the increase of selectivity. In the same experimental conditions, PTFE membrane shows better separation performance than PVDF membrane does.

Removal of 2,4-dichlorophenol from wasterwater by vacuum membrane distillation using hydrophobic PPESK hollow hiber membrane

2,4-Dichlorophenol was removed from wasterwater using a new hydrophobic poly（phthalazinone ether sulfone ketone） （PPESK） hollow fiber membrane by vacuum membrane distillation （VMD）.

Superhydrophobic modification of ceramic membranes for vacuum membrane distillation

The hydrophobically modi fied ceramic membranes have great potential for energy-ef ficient membrane distillation.In this work,flat-sheet ceramic membranes with a superhydrophobic surface were fabricated by grafting 1H,1H,2H,2H-per fluorooctyltrichlorosilane or 1H,1H,2H,2H-per fluorodecyltriethoxysilane and followed by ultraviolet irradiation.The surface water contact angle was improved from 46° of original ceramic membrane to 159°,which exhibited a stable and excellent superhydrophobic effect.The modi fied membranes showed a high flux of 27.28 kg·m^(-2)·h^(-1) and simultaneously maintained an excellent retention rate of 99.99%,when used in vacuum membrane distillation process for treatment of a 1 wt% NaCl(75 °C) aqueous solution.These results suggested that superhydrophobic modi fication of ceramic surface is a facile and cost-effective way to achieve higher membrane distillation performance.The superhydrophobically-modi fied ceramic membrane with an excellent desalination capacity would show considerable potential in practical membrane distillation utilizations.

THE SEPARATION OF Pb-Sb ALLOYS BY VACUUM DISTILLATION

This paper summarizes the research results of vacuum distillation of Pb-Sb alloy and crude antimony.In our study,we have found the basic law which states that in Pb-Sb phase diagrams,the part which is rich in lead can be used to guide the purification of lead by distillation,while the part rich in antimony can be used to guide the purification of Sb.where the compositional point C is the azeotropic mixture.The technical experi-mental results at temperatures between 7OO-85OC are coincident with those of theorical study.The expanding experiment at the 100kg scale produced satisfactory results.

Novel design of lubricant-type vacuum distillation process for lube base oils production from hydrocracking tail oil

Dividing-wall columns(DWCs)are widely used in the separation of ternary mixtures,but rarely seen in the separation of petroleum fractions.This work develops two novel and energy-efficient designs of lubricant-type vacuum distillation process(LVDP)for the separation of hydroisomerization fractions(HIF)of a hydrocracking tail oil(HTO).First,the HTO hydroisomerization reaction is investigated in an experimental fixed-bed reactor to achieve the optimum liquid HIF by analyzing the impact of the operating conditions.A LVDP used for HIF separation is proposed and optimized.Subsequently,two thermal coupling intensified technologies,including side-stream(SC)and dividing-wall column(DWC),are combined with the LVDP to develop side-stream vacuum distillation process(SC-LVDP)and dividing-wall column vacuum distillation process(DWC-LVDP).The performance of LVDP,SC-LVDP,and DWC-LVDP are evaluated in terms of energy consumption,capital cost,total annual cost,product yields,and stripping steam consumption.The results demonstrates that the intensified processes,SC-LVDP and DWC-LVDP significantly decreases the energy consumption and capital cost compared with LVDP.DWC-LVDP further decreases in capital cost due to the removal of the side stripper and narrows the overlap between the third lube oils and fourth lube oils.This study attempts to combine DWC structure into the separation of petroleum fractions,and the proposed approach and the results presented provide an incentive for the industrial implementation of high-quality utilization of HTO through intensified LVDP.

Innovative hydrophobic/hydrophilic perfluoropolyether(PFPE)/polyvinylidene fluoride(PVDF)composite membrane for vacuum membrane distillation

Though membrane distillation(MD)has gained more and more attention in the field of desalination,the wetting phenomenon was still a non-negligible problem.In this work,a method combined dip-coating and UV in situ polymerization for preparing hydrophobic/hydrophilic perfluoropolyether(PFPE)/polyvinylidene fluoride composite membranes.This composite membrane consisted of a top thin hydrophobic coating layer and hydrophilic substrate membrane.In terms of anti-wetting properties,contact angle and liquid entry pressure of all composite membranes(except for those based on 0.45μm)exceeded 160°and 0.3 MPa,respectively.In particular,the desalination performance was tested in vacuum membrane distillation tests by feeding 3.5%(mass)saline solution(NaCl)at 60℃.The composite membranes with larger support pore size and lower PFPE content had higher membrane distillation flux.And for stability tests(testing the 0.22μm membrane coated by 5%(mass)PFPE),the highest MD flux29.08 kg·m^(-2)·h^(-1) and stable salt rejection(over 99.99%)during the period.Except that,the effects of coating material concentration and pore sizes of substrate membrane were also investigated for surface morphology and topography,porosity,mechanical strength and pore size characteristics.This work provided a simple and effective alternative to prepare excellent hydrophobic composite membranes for MD applications.

Use of various MgO resources for high-purity Mg metal production through molten salt electrolysis and vacuum distillation

A green and effective electrolytic process was developed to produce high-purity Mg metal using primary and secondary resources containing Mg O as a feedstock. The electrolysis of various Mg O resources was conducted using a Cu cathode in MgF2– LiF – KCl molten salt at 1043 K by applying an average current of 1.44 A for 12.5 h. The electrolysis of calcined North Korean magnesite and seawater Mg O clinker yielded Mg alloys of MgCu2and(Cu) phases with current efficiencies of 89.6–92.4%. The electrolysis of oxidized Mg O-C refractory brick, aged ferronickel slag, and ferronickel slag yielded Mg alloys of MgCu2and(Cu) phases with current efficiencies of 59.3–92.3%. The vacuum distillation of Mg alloys obtained was conducted at 1300 K for 10 h to produce high-purity Mg metal. After vacuum distillation, Mg metal with a purity of above 99.994% was obtained. Therefore, this study demonstrates the feasibility of the production of high-purity Mg metal from various Mg O resources using a novel electrolytic process with a Cu cathode, followed by vacuum distillation.

Application of molecular interaction volume model in separation of Sn-Zn alloy by vacuum distillation

The activity of components of Sn-Zn binary alloy system was predicted based on the molecular interaction volume model （MIVM）. The calculated values are in good agreement with available experimental data of activities, which indicates that this model is of stability and reliability because the MIVM has a good physical basis. The vapor-liquid phase equilibrium of Sn-Zn alloy system in vacuum distillation was calculated as a function of the activity coefficient. The results show that the content of Sn in vapor phase is 4.2x 10-7 （mass fraction） while in liquid phase it is 90% （mass fraction） at 1 073 K, and the content of Sn in vapor phase increases with increasing the melt temperature and content of Sn in liquid phase. Vacuum distillation experiments were carried out on Sn-Zn alloy for the proper interpretation of the results of the MIVM in the temperature range of 973-1 273 K under pressures of 15-200 Pa. The experimental results show that the content of Sn in vapor phase is 5x 10 6 （mass fraction） while in liquid phase it is 90% （mass fraction） under the operational condition of 1 073 K, 100 rain and 15 Pa. The experimental results are in good agreement with the predicted values of the MIVM for Zn-Sn binary alloy system.