For industrial use, iron-ore concentrates shall correspond to definite requirements regarding both basic substance content – iron as well as phosphorus content. Decreased phosphorus content in iron-ore concentrate can be received by the method of hydrometallurgy (desalinization of phosphorus by mineral acid). On theexperimental base of OJSC VNIIMT, a laboratory research was carried out regarding iron ore dephosphorization; as a result maximum possible content of phosphorus was obtained in a final product. The optimal technological parameters of sulphuric acid desalinization were defined that have an effect on quality of phosphorus removal of iron ore magnetite concentrate: size degradation of roasted concentrate; phosphorus removal duration; pulp heating temperature effect; sulphuric acid-specific consumption.
Keywords: desalinization, iron ore, concentrate, pulp, sulphuric acid, phosphorus content, optimal parameter

Epishin, A

Kai, C

Karelin, V

Malikbaev, B

Zajnullin, L

English

KnE Publishing Platform

 TIM’2018VII All- Russian Scientific and Practical Conference of Students,Graduate Students and Young Scientists on“Heat Engineering and Computer Science in Education, Science and Production”Volume 2018Conference PaperIron Ore Dephosphorization of Gara DjebiletDeposit By Hydrometallurgical MethodLik Zajnullin1,3, Vladimir Karelin1, Artem Epishin1, Chen Kai2, andBakhodur Malikbaev31OJSC ”Scientific Research Institute of Metallurgical Heat Engineering” (OJSC «VNIIMT»),Ekaterinburg, Russia2Chine Metallurgical Engineering and Project Corp., Chine3Ural Federal University (UrFU), Ekaterinburg, RussiaAbstractFor industrial use, iron-ore concentrates shall correspond to definite requirementsregarding both basic substance content – iron as well as phosphorus content.Decreased phosphorus content in iron-ore concentrate can be received by themethod of hydrometallurgy (desalinization of phosphorus by mineral acid). On theexperimental base of OJSC VNIIMT, a laboratory research was carried out regardingiron ore dephosphorization; as a result maximum possible content of phosphoruswas obtained in a final product. The optimal technological parameters of sulphuricacid desalinization were defined that have an effect on quality of phosphorusremoval of iron ore magnetite concentrate: size degradation of roasted concentrate;phosphorus removal duration; pulp heating temperature effect; sulphuric acid-specificconsumption.Keywords: desalinization, iron ore, concentrate, pulp, sulphuric acid, phosphoruscontent, optimal parameters1. IntroductionIn the Algerian People’s Democratic Republic there is iron ore deposit Gara Djebilet,one of the largest deposits in the world. Development of this deposit is suppresseddue to high (up to 0.75–1.0%) content of phosphorus in the ore.Research works on iron ore beneficiation of Gara Djebilet deposit were carried outbeforemany times starting from the 1960s. In the researchmainlymechanicalmethodsof beneficiation were used (degradation and subsequent operations of separation ofore constituents from mining waste – magnetic separation, floatation etc.). In this caseHow to cite this article: Lik Zajnullin, Vladimir Karelin, Artem Epishin, Chen Kai, and Bakhodur Malikbaev, (2018), “Iron Ore Dephosphorizationof Gara Djebilet Deposit By Hydrometallurgical Method” in VII All- Russian Scientific and Practical Conference of Students, Graduate Studentsand Young Scientists on “Heat Engineering and Computer Science in Education, Science and Production”, KnE Engineering, pages 168–176.DOI 10.18502/keg.v3i5.2666Page 168Corresponding Author:Lik Zajnullinaup@vniimt.ruReceived: 6 June 2018Accepted: 15 June 2018Published: 17 July 2018Publishing services provided byKnowledge ELik Zajnullin et al. This articleis distributed under the terms ofthe Creative CommonsAttribution License, whichpermits unrestricted use andredistribution provided that theoriginal author and source arecredited.Selection and Peer-reviewunder the responsibility of theTIM’2018 ConferenceCommittee. TIM’2018iron ore concentrate could not be obtained with acceptable for subsequent metallur-gical process phosphorus content that basically transferred to the concentrate duringthe beneficiation as presumably it was mainly tied chemically to iron.For the subsequent use of the iron ore concentrate, for example, in the blast-furnaceprocess phosphorus content is required 0.2% or less, and phosphorus removal in thesteelmaking process is an economically expensive procedure. In this regard it is rele-vant to carry out laboratory research to determine, test and select effective process ofthe Algerian iron ore processing of Gara Djebilet deposit with obtaining of maximumpossible beneficiation of ore on iron content by high-temperaturemagnetizing roastingand maximum possible reduction of phosphorus content in a final product after thestage of sulphuric acid desalinization.2. Research ObjectivesTo achieve objectives of this research work the following tasks shall be completed:1. To develop technique and equipment for a laboratory experiment on dephospho-rization of iron ore concentrate after high-temperature magnetizing roasting byhydrometallurgical processing method.2. To determine optimal parameters of sulphuric acid desalinization of phosphorus:process duration, sulphuric acid concentration in aqueous solution, ratio of solidsubstance to liquid phase in the pulp, pulp’s temperature.3. Laboratory Research and Results AnalysisThe work on desalinization of preliminary roasted concentrate was carried out ina chemical laboratory of OJSC VNIIMPT [1–4] with using of laboratory stirring shaftDAIHAN-HS-120A (Figure 1) for the pulp’s mixing.Technological stages totally influenced on dephosphorizing of the concentrate are:preliminary high-temperature magnetizing roasting of the material, degradation upto defined by testing optimal size, magnetic separation and subsequent phosphorusdesalinization by light aqueous solution of sulphuric acid. Quality of each stage has aneffect on dephosphorizing extent of the material in whole.In the first series of testing influence of size on residual content of phosphorusafter dephosphorizing process was studied. Desalinization of the roasted concentrateat temperature of 950∘C was made under the following parameters of sulphuric acidDOI 10.18502/keg.v3i5.2666 Page 169 TIM’2018 Analog control drive Clamp (CL200) Stainless steel rotary mixer Chromed holder Tripod Figure 1: General view of laboratory stirring shaft.processing: solid-to-liquid ratio – 1:2, sulphuric acid concentration in aqueous solution20 gr per 100 gr of the concentrate, desalination time 120 minutes, pulp’s temperature65∘C. Technological parameters of dephosphorization (temperature, concentration andtime) in research works were selected in experimental way of the hydrometallurgicalprocessing of Lisakovsk ores [5, 6] and are overrated on purpose in order to estimateonly influence of the material degradation extent before desalinization on residualcontent of phosphorus in a final product.By 2–0 mm size of iron ore magnetite concentrate the residual content of phospho-rus in the leached concentrate was obtained as 0.45% (experiment 3), in this casephosphorus content in the base ore makes up 0.75%. The material’s leaching in 2–0mm size reduces phosphorus insignificantly. For the leached concentrate of 0.071 mmsize the best result with residual content of phosphorus 0.17% is observed.With decreasing of fraction size of the roasted iron ore magnetite concentrate upto minus 0.044 mm under the same technological parameters the residual content ofphosphorus made up 0.19% (experiment 1). Based on data of the Table 1 it is seen thatthe residual content of phosphorus in the concentrate after sulphuric acid treatmentminus 0.044mm in size and minus 0.071 mm in size does not differ much (makes up onan average 0.18%, error limit of chemical analysis 0.024%). Based upon the obtainedresults given in Table 1 as optimal degradation size of the roasted ore 0.071 mm isaccepted.DOI 10.18502/keg.v3i5.2666 Page 170 TIM’2018In the second series of tests research works on influence of dephosphorizing dura-tion on phosphorus content in a final product were carried out. Desalinization time wasselected in the range of from 20 to 120 min. The results are given in Table 2.T 1: Influence of degradation size of roasted ore on phosphorus content in dephosphorizedconcentrate.No. Roasting Desalinization Size Fr.,mmFe Growth%1 T𝑟𝑜𝑎𝑠 = 950∘C,Τ𝑟𝑜𝑎𝑠 = 80′′S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 60′′ t𝑠𝑜𝑙 = 65∘C–0.044 63.0 0.192 T𝑟𝑜𝑎𝑠 = 950∘C,Τ𝑟𝑜𝑎𝑠 = 80′′S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 60′′ t𝑠𝑜𝑙 = 65∘C–0.071 63.8 0.173 T𝑟𝑜𝑎𝑠 = 950∘C,Τ𝑟𝑜𝑎𝑠 = 80′′S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 60′′ t𝑠𝑜𝑙 = 65∘C2–0 57.6 0.45Legend: t𝑟𝑜𝑎𝑠 – ore roasting temperature; τ𝑟𝑜𝑎𝑠 – ore exposure time; t𝑠𝑜𝑙 – pulp temperature(solution + ore); τ𝑑𝑒𝑝ℎ – dephosphorization time; S – solid phase (ore); L – aqueous solution ofsulphuric acid; C H2SO4 – concentration of sulphuric acid in aqueous solution.T 2: Influence of dephosphorizing duration on phosphorus content in dephosphorized concentrate.No. Roasting Magnetite Concentrate Dephosphorization Dephosphorized ConcentrateContent, % Content, %P Fe SizeFr.,mmFe P1 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.52 63.3 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 20′′, t𝑠𝑜𝑙 = 65∘C–0.071 65.5 0.202 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.52 63.3 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 80′′, t𝑠𝑜𝑙 = 25∘C–0.071 65.3 0.183 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.55 63.3 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.044 65.3 0.16Legend: t𝑟𝑜𝑎𝑠 – ore roasting temperature; τ𝑟𝑜𝑎𝑠 – ore exposure time; t𝑠𝑜𝑙 – pulp temperature (solution +ore); τ𝑑𝑒𝑝ℎ – dephosphorization time; S – solid phase (ore); L – aqueous solution of sulphuric acid; C H2SO4– concentration of sulphuric acid in aqueous solution.With increasing of dephosphorization process duration of from 20 to 120 minutesinsignificant reduction of the residual content of phosphorus in the dephosphorizedDOI 10.18502/keg.v3i5.2666 Page 171 TIM’2018concentrate from 0.20 to 0.16% is observed. Based upon the obtained results asoptimal and sufficient duration of dephosphorizing the time equal to 20 minutes isaccepted.In the third series of tests pulp heating temperature influence on the quality ofthe dephosphorized magnetite concentrate was determined. In each experiment theaqueous solution of sulphuric acid was heated up to 25, 45 and 65∘C. The magnetiteconcentrate with the optimal size of 0.071 mm was treated by the leaching procedurewith light aqueous solution of sulphuric acid of mass concentration of 20 gr per 100 grof the concentrate and ratio of solid material to liquid phase S:L = 1:2. The results ofthe tests are given in Table 3.T 3: Influence of temperature of pulp heating on residual content of phosphorus in dephosphorizedconcentrate.No. Roasting Magnetite Concentrate Dephosphorization Dephosphorized ConcentrateContent, % Content, %P Fe Size Fr.,mmFe P1 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.55 63.6 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.071 65.3 0.162 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.45 63.6 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 45∘C–0.071 66.0 0.153 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.45 63.6 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 25∘C–0.071 65.9 0.15Legend: t𝑟𝑜𝑎𝑠 – ore roasting temperature; τ𝑟𝑜𝑎𝑠 – ore exposure time; t𝑠𝑜𝑙 – pulp temperature (solution +ore); τ𝑑𝑒𝑝ℎ – dephosphorization time; S – solid phase (ore); L – aqueous solution of sulphuric acid; C H2SO4– concentration of sulphuric acid in aqueous solution.As it is seen in Table 3 in the range of temperatures of pulp heating from 20 to 65∘Cthe residual content of phosphorus in the dephosphorized concentrate was receivedalmost the same (0.15–0.16%). In this range of temperature of dephosphorizing the ironcontent in the dephosphorized concentrate made up 65.3–66.0%. In accordance withresults of tests of sulphuric acid desalinization of phosphorus the pulp temperature of25∘C was defined as optimal value.In the next series of tests the cold roasted concentrate after magnetic separationwas treated by the leaching procedure by light aqueous solution of sulphuric acid ofmass concentration of from 5 to 30 gr per 100 gr of the concentrate under ratio ofDOI 10.18502/keg.v3i5.2666 Page 172 TIM’2018solid material to liquid phase S:L = 1:2. The pulp was actively mixed within 120 minutesat temperature of 65 ∘С. Upon the completion of the experiment a sample of leachedconcentrate was taken for analysis of phosphorus and content of iron and phosphorusin a final product was determined (Table 4).Based on data of Table 4 it is seen that for the roasted concentrate at temperatureof 900 𝑜C and size of minus 0.071 mm with the increase of specific consumption ofsulphuric acid of from 10 to 30 gr per 100 gr of the concentrate the iron content makesup 64.5% on an average; the residual content of phosphorus is reduced in the rangeof from 0.38% to 0.16%. By roasting at 950𝑜 C and degradation size of minus 0.044mm with the increase of specific consumption of sulphuric acid of from 5 to 20 gr per100 gr of the concentrate the iron content makes up 62.5% on an average, and theresidual content of phosphorus is reduced in the range of from 0.47 to 0.19%. As it isseen from the series of experiments the concentration of 5–15 gr of sulphuric acid per100 gr of the concentrate is not enough as the residual content of phosphorus remainsrather high and makes up 0.4% on an average.Also an experiment on dephosphorization of the roasted concentrate was carriedout using as chemical reagent of nitric acid HNO3 under the following technologicalparameters: ratio S:L = 1:2 and specific consumption of HNO3 20 gr per 100 gr of themagnetite concentrate, desalinization time 20 minutes, pulp temperature 25∘C. Due tothis experiment the iron content in the dephosphorized concentrate 66.7% and theresidual content of phosphorus 0.17% were obtained. As alternative chemical reagentfor dephosphorization of iron ore magnetite concentrate the nitric acid can be used butup to date the sulphuric acid is more available and less expensive product.4. SummaryOn the base of OJSC VNIIMT experimental tests on the roasted concentrate dephospho-rization of Gara Djebilet deposit by hydrometallurgical method were conducted. As aresult of research works main technological parameters of sulphuric acid treatment ofmagnetite concentratewere defined underwhich the content of iron in the concentratewas increased from initial 52.1% to 64.0–65.3%, and the residual content of phosphorusin the concentrate was reduced from initial 0.75% to 0.15–0.20%. It was determinedthat for more complete dephosphorization of magnetite concentrate (P𝑟𝑒𝑠≤ 0.2%) bysulphuric acidmethod it is required to carry out preliminary high-temperaturemagneticroasting of ore at temperature not lower than 900𝑜 C and with duration not less than40 minutes. Then the roasted ore degradation follows, wet magnetic separation withDOI 10.18502/keg.v3i5.2666 Page 173 TIM’2018T 4: Influence of specific consumption of sulphuric acid on phosphorus content in dephosphorizedconcentrate.No. Roasting Magnetite Concentrate Dephosphorization Dephosphorized ConcentrateContent, % Content, %P Fe Size Fr.,mmFe P1 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.55 63.6 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.071 65.3 0.162 T𝑟𝑜𝑎𝑠 = 900∘C,Τ𝑟𝑜𝑎𝑠 = 120′′0.45 63.6 S:L = 1:2,C H2SO4= 30 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.071 64 0.193 T𝑟𝑜𝑎𝑠 = 950∘C,Τ𝑟𝑜𝑎𝑠 = 80′′0.6 61.4 S:L = 1:2,C H2SO4= 5 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.044 61.5 0.354 T𝑟𝑜𝑎𝑠 = 950∘C,τ𝑟𝑜𝑎𝑠 = 80′′0.6 61.4 S:L = 1:2,C H2SO4= 10 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.044 62.6 0.475 T𝑟𝑜𝑎𝑠 = 950∘C,Τ𝑟𝑜𝑎𝑠 = 80′′0.6 61.4 S:L = 1:2,C H2SO4= 15 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.044 62.6 0.396 T𝑟𝑜𝑎𝑠 = 950∘C,Τ𝑟𝑜𝑎𝑠 = 80′′0.6 61.4 S:L = 1:2,C H2SO4= 20 gr/100 gr T,Τ𝑑𝑒𝑝ℎ = 120′′, t𝑠𝑜𝑙 = 65∘C–0.044 63 0.19Legend: t𝑟𝑜𝑎𝑠 – ore roasting temperature; τ𝑟𝑜𝑎𝑠 – ore exposure time; t𝑠𝑜𝑙 – pulp temperature (solution +ore); τ𝑑𝑒𝑝ℎ – dephosphorization time; S – solid phase (ore); L – aqueous solution of sulphuric acid; C H2SO4– concentration of sulphuric acid in aqueous solution.obtaining of magnetite product and tails, concentrate drying and its sulphuric acidtreatment by aqueous solution of sulphuric acid.The main technological parameters of sulphuric acid treatment of iron ore concen-trate.1. In a series of experiments with various degradation of the roasted concentratebefore magnetic separation it was shown that the optimal size is 0.071 mm. Insuch fraction the dephosphorized concentrate was obtained with iron content of63.8% and the residual content of phosphorus of 0.17%.2. In a series of tests with different specific consumption of sulphuric acid (5–30 grper 100 gr of the concentrate) it was shown that the optimal mass concentrationDOI 10.18502/keg.v3i5.2666 Page 174 TIM’2018of sulphuric acid in aqueous solution is 20 gr per 100 gr of the concentrate, in thiscase in the dephosphorized concentrate the content of iron made up 65.3%, andthe residual content of phosphorus made up 0.16%.3. In a series of tests with different temperature of pulp heating (25–65∘C) it wasshown that the optimal pulp temperature is 25∘C. In this case in the dephospho-rized concentrate the content of iron made up 65.9%, and the residual content ofphosphorus made up 0.15%.4. In a series of experiments with different duration of the concentrate leaching itwas shown that the optimal duration of dephosphorization process is 20 minutes.In such duration of dephosphorizing the concentrate was obtained containing iron65.0% and the residual content of phosphorus 0.17%.5. As a leaching reagent the nitric acid was tested (HNO3). In this case the content ofiron in the dephosphorized concentrate made up 66.7%, and the residual contentof phosphorus made up 0.17%, but significant minus of nitric acid use is that it isdifficult to get and its rather high price.References[1] Belikov, V. V., Ogorodov, V. B., Yadryshnikov, A. O., et al. (27 June 2002). Methodof purification of iron ore concentrate from phosphorus impurities. Patent of theRussian Federation No. 2184158.[2] Karelin, V. G., Zainullin, L. A., and Epishin, A. Y. (2017). Kinetics of high-temperaturedehydration of Lisakovsk iron ore concentrate. Izvestiya Vysshikh UchebnykhZavedenij. Chernaya Metallurgiya, vol. 60, no. 8, pp. 656–661.[3] Epishin, A. Yu., Zainullin, L. A., and Karelin, V. G. (2011). On dephosphorizing ofLisakovsky brown ironstone with leaching methods with pre-roasting. Digest of theVIII Congress of Dressers of CIS Countries, vol. I, pp. 83–86.[4] Karelin, V. G., Zainulin, L. A., Epishin, A. Y., et al. (2013). The Modern Techniques ofInvolvement of Phosphorous. Containing Sedimentary Production. The 12th China–Russia Symposium on Advanced Materials and Technologies, pp. 388–391. Kuming.[5] Karelin, V. G., Zainulin, L. A., Epishin A. Y., et al. (2015). Combined pyro-hydrometallurgical technology of dephosphorizing brown ironstone of Lisakovskydeposit. Ferrous metallurgy, Bulletin of Scientific and Technical and EconomicInformation, no. 2, pp. 10–15.DOI 10.18502/keg.v3i5.2666 Page 175 TIM’2018[6] Karelin, V. G., Zainulin, L. A., Epishin, A. Y., et al. (2015). Features of pyro-hydrometallurgical technology of dephosphorizing brown ironstone of Lisakovskydeposit. Steel, no. 3, pp. 8–11.DOI 10.18502/keg.v3i5.2666 Page 176

Iron Ore Dephosphorization of Gara Djebilet Deposit By Hydrometallurgical Method

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Iron Ore Dephosphorization of Gara Djebilet Deposit By Hydrometallurgical Method

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