Phosphoric Acid Extraction Research Articles

Three-liquid-phase behavior in the quaternary systems of water + phosphoric acid + diisopropyl ether + tributyl phosphate/methyl isobutyl ketone at 298.2 K

The three-liquid-phase formation in the ternary system of water + phosphoric acid + diisopropyl ether (DIPE) makes the phosphoric acid extraction only effective for acid mass fractions above 0.69. To avoid the undesirable formation of the third phase and enhance acid extraction, particularly at low concentrations, two phase modifiers, methyl isobutyl ketone (MIBK) and tributyl phosphate (TBP), were systematically studied. In order to quantify the synergetic effect of the mixed solvents of DIPE+TBP and DIPE+MIBK, the liquid–liquid equilibria for the quaternary systems of H2O+H3PO4 + DIPE+TBP and H2O+H3PO4 + DIPE+MIBK were fully established for different DIPE/phase modifier (TBP or MIBK) mass ratios (90/10, 70/30, 50/50, and 20/80) at 298.2 K under atmospheric pressure using the cloud point and Othmer graphical method. Othmer-Tobias and Hand correlations were used to fit the tie-line data and assess its consistency. In addition, the behavior of the three-phase zone was also studied as a function of the phase modifiers content. Separation factor (S) and acid distribution (D2) were used to identify the most effective solvent with the potential to enhance phosphoric acid extraction from aqueous solutions.

Flow characteristics and mass transfer performance of phosphoric acid extraction in a T-type central plug-in microreactor

In recent years, the demand for phosphoric acid, a key raw material for lithium iron phosphate batteries, has surged. However, current phosphoric acid extraction equipment faces challenges such as low mass transfer efficiency and difficulty in phase separation, leading to reduced production efficiency, bulky equipment, and scaling issues. To address these problems, this study introduces a T-type central plug-in microreactor (TCPM) designed to enhance mass transfer efficiency and facilitate rapid phase separation. The extraction of phosphoric acid from the water phase to the organic phase (volume ratio of tributyl phosphate to kerosene is 4:1) was chosen as the experimental system. We investigated the effects of various parameters on liquid-liquid flow and mass transfer characteristics in the TCPM. Visualization techniques identified slug and parallel flow as the primary liquid-liquid flow patterns within the TCPM. Notably, the central plug-in promotes the formation of parallel flow, improving phase separation compared to conventional T-type microreactors. The volume mass transfer coefficient of the TCPM ranges from 0.023 to 0.074 s-1, and the optimal phosphoric acid extraction efficiency and volume mass transfer coefficient can reach up to 90.5% and 0.074 s-1, respectively, outperforming conventional T-type microreactors. Predictive model for extraction efficiency was developed, showing deviations within 10%. These findings demonstrate the TCPM's potential as an efficient phosphoric acid extraction device with rapid phase separation, holding significant promise for liquid-liquid extraction applications.

Study of the Production of Wet-processing Phosphoric Acid by Clinker Method on Base of Mineralized Mass

The article presents the results of the study of extractive phosphoric acid extraction processes from the mineralized mass (MM) - mineralized mass (MM) produced during the thermal processing of Central Kyzylkum (CK) phosphorite. Effects of sulfuric acid concentration on the quality parameters of the obtained wet-processing phosphoric acid (WPPA), processes of WPPA extraction through different concentrations of phosphoric acid solution from phosphoric acid-gypsum porridge were studied. The optimal parameters of these processes have been determined. In the composition of WPPA obtained in acceptable parameters 19,30-19,59% Р2О5, 0,08-0,09% F will be. Filtration rates of phosphatic-acid-gypsum porridges during extraction with different concentrations of WPPA are equal to 1096-1192 kg/m2·h. It was also determined that the main composition of the resulting phosphogypsum is as follows: 2,44-2,59% Р2О5total (t.)., 29,93-30,09% CaOtotal (t.), 41,29-41,50% SO3 and 1,16-1,21% F.

Physico-chemical features of acid decomposition and production of extraction phosphoric acid based on moroccan phosphorites

The results of research on the establishment of physicochemical features of acid processing of North African (Moroccan) phosphorites, as well as their influence on the technological process and technical and economic indicators of extraction phosphate acid (EPA) production are presented. Significant differences have been established in the nature of the acid decomposition process, syngony and the size of the formed calcium sulfate crystals for different grades of phosphorites, which is due to a significant influence on the decomposition process not only of the technological mode of the process, but to a large extent differences in the mineralogical composition of phosphate ores. Thus, the increased content of carbonate apatites in phosphorites of the K-9 and K-10 grades led to a higher reactivity in the region of low concentrations. At the same time, the high reactivity of carbonateapatites leads to a number of negative processes, in particular, abundant foaming and passivation of grains of phosphate raw materials with fine-crystalline calcium sulfate precipitate, formed due to the rapid supersaturation of the system, which in turn leads to a sharp decrease in the degree of decomposition. A significant difference in the nature of calcium sulfate crystallization for the conditions for obtaining EPA from the known data was established, which made it possible to conclude that the rate and nature of the process of calcium sulfate recrystallization in the CaO-P2O5- H2O system is determined not only by temperature, sulfate regime and P2O5 content in the liquid phase, but also by the nature and composition of phosphate raw materials. Based on experimental data, conclusions were drawn about a decrease in power during the transition from apatite to phosphorites from 21.89 to 24.23% (depending on the brand of Moroccan phosphorite), a significant increase in the load on filters and a decrease of 1.5–2 times in the amount of fluorine compounds released into the gas phase during decomposition.

PROCESSING OF A WASHED DRY CONCENTRATE CONTAINING 26% P2O5 INTO AMMOPHOSPHATE, SULPHO- AND NITROAMMOPHOSPHATE FERTILIZERS

The process of obtaining ammophosphate by means of phosphoric acid decomposition of washed dried concentrate (WDC) with 26 % Р2О5 and 10 % СО) - raw material for the production of thermally fired concentrate, has been studied. The extraction phosphoric acid contains (mass. %): 16.46 P2O5, 0.06 CaO, 1.11 MgO, 0.27 Fe2O3, 0.41 Al2O3, 2.98 SO3 and 0.99 F. The mass ratio of WPPA: WDC ranged from 100: 10 to 100: 30. Then acidic phosphate pulps (at 65°C) after 45 minutes were ammoniated to pH = 3.8, granulated and dried at 85 - 90°C. It has been shown that the nitrogen content in the finished product ranges from 4.92 - 7.11 %, total phosphorus (P2O 5t.) 41.48 - 46.44 %, phosphorus assimilated by plants (P2O5acceptable) 34.79 - 45.11 %, water-soluble phosphorus (P2O 5w.s.) 23.49 - 37.73 %. The addition of 5 - 7.5 % H2SO4 or HNO3 in the form of a monohydrate makes it possible to intensify the process of phosphoric acid decomposition of phosphate raw materials and to obtain sulfo- and nitroammophosphate with significantly highcontents of P2O5 acceptable and P2O5 w.s.. So, with a weight fraction of WDC equals to 30 and weight fractions of H2SO4 - 5 and 7.5, there have been 37.6 and 34.47 % P2O5 total in sulfoammophosphate; 24.11 and 22.06 % CaO t. , 88.75 and 96.4 % P2O5 acceptable: P2O5t., 77.39 and 79.54 % P2O5 w.s. : P2O5t., 6.03 and 7.08 % nitrogen, respectively. In the case of using HNO3, nitroammophosphate contains the largest amount of nitrogen due to additionally introduced nitric acid, but the phosphate raw material has a relatively low decomposition coefficient. The strength of granules of all brands of fertilizers averages 3.50 MPa and are quite suitable for bulk storage and transportation. Material balances for the production of ammophosphate, sulfoammophosphate and nitroammophosphate have been calculated.

Application of wastewater recycling in treatment processes

The object of the study is the method of wastewater recycling. The problem of reducing the negative impact on the environment, by increasing the efficiency of treatment facilities is the most urgent at the moment. The methodology of wastewater recycling is one of the most famous and popular, nowadays. Wastewater recycling allows both to reduce the negative impact on the environment and to increase the efficiency of existing technological schemes for wastewater treatment. Examples of the implementation of this method in the meat processing industry, as well as in enterprises producing extraction phosphoric acid and mineral fertilizers, as well as the impact on the operation of biological filters are considered. In the course of the study the current situation in the world on the implementation of this methodology and its effectiveness was considered. Further, both practical and theoretical materials on this issue were considered. The variant of implementation of the recirculation method on the existing technological scheme of wastewater treatment of tannery production was considered. At the end of the study it was concluded that it is important to further investigate this technique for its successful integration into existing wastewater treatment process schemes..

Investigation of the process of extraction of copper from dust of electric filters of oxygen-flare smelting furnace with sulfuric, thermal, and extractive phosphoric acid

The results of studies on the extraction of copper from the dust of electrostatic precipitators of oxygen-torch melting with solutions of sulfuric, thermal, extraction phosphoric depending on S:L, concentration and duration of the leaching process are presented. It has been established that the maximum degree of copper extraction is observed when using extractive phosphoric acid, which reaches more than 86%. The optimal parameters for the extraction of copper in extraction phosphoric acid are S:L = 1:10, temperature 90°C and mixing time 25-30 minutes.

Extraction of Zinc from Zinc Sublimber with Sulfuric, Thermal and Extraction Phosphoric Acid

The study was conducted to extract zinc and the results on the extraction of Zn from zinc sublime with the solution of sulfuric, thermal and extraction phosphoric acids are presented depending on Solid: Liquid (S:L), concentration and duration of the leaching process. Sulfuric acid was used with a content of 8% which is a waste product of non-ferrous metallurgy, thermal phosphoric extraction phosphoric acid from phosphorites of the Central Kyzylkum. It has been established that the maximum degree of zinc extraction is noted when using extraction phosphoric acid, which is 96-98%, S:L=1:(10-15), with the temperature of 90°C and washing sulfuric acid, which is 99.8% at S:L=1:10 and above at room temperature. Increasing the duration of the process over 30 minutes has virtually no effect on the extraction percentage of zinc.

Variation of Extraction Yield and Droplet Size during Emulsification Solvent Extraction of Wet-Process Phosphoric Acid

This research focuses on emulsification solvent extraction for purifying wet-process phosphoric acid. The effects of various parameters, including stirring speed, phase ratio and emulsification time on the extraction yield and droplet size distribution were investigated. The optimal conditions were determined. The influence of time and physical properties of solvent on average droplet diameter was fitted by dimensional analysis. The results showed that the mathematical model has a strong agreement with the experimental data. This model was reliable to predicting the droplet size in different conditions of manufacturing emulsion.

STUDY OF PROCESSE OF OBTAINING MONOPOTASSIUM PHOSPHATE BASED ON MONOSODIUM PHOSPHATE AND POTASSIUM CHLORIDE

Results of studies of the process of conversion of the flotation potassium chloride of the Tyubegatan deposit with solutions of sodium dihydrogen phosphate obtained on the basis of purified extraction phosphoric acid from phosphorites of the Central Kyzylkum to potassium dihydrogen phosphate are presented. The effect of the ratio of the components, S:L on the formation of potassium dihydrogen phosphate at temperatures of 25°C and 100°C was studied. Optimal technological parameters for isolation of potassium dihydrogen phosphate were determined. Rheological properties of solutions formed in the process of obtaining potassium dihydrogen phosphate were identified. The obtained results were confirmed by X-ray phase and IR-spectroscopic methods of analysis. Elemental composition of potassium dihydrogen phosphate was established by electron microscopy.

Research of the process of obtaining potassium dihydrophosphate using diethylamine

The article studies the physico-chemical analysis of the conversion process of local raw materials of potassium chloride and extraction phosphoric acid obtained on the basis of phosphorites of Central Kyzylkums, in the presence of diethylamine. As a product, potassium dihydrogen phosphate was obtained, which is used as a complex fertilizer in many branches of the chemical industry and in agriculture. The influence of technological parameters on the conversion process is investigated.

Methodology of Organization of Closed Water Circulation of Enterprises for the Production of Extraction of Phosphoric Acid and Mineral Fertilizers

Methodology of Organization of Closed Water Circulation of Enterprises for the Production of Extraction of Phosphoric Acid and Mineral Fertilizers

New Approach for Trace Thallium Removal in High Purity Ammonium Rhenate Solution by P204 Extraction

Thallium (Tl) is an extremely toxic rare metal to the eco-environment. Trace thallium impurity in ammonium perrhenate is harmful to the high-temperature mechanical properties of rhenium metal used for aeroengine single crystal blade. The di(2-ethylhexyl) phosphoric acid (P204) extraction to remove thallium in ammonium perrhenate solution without additive was innovatively proposed. The migration behavior of trace thallium with the concentration of P204, saponification degree and organic/aqueous phase (O/A) ratio, distribution law of thallium in the extraction system of P204, and mechanism of thallium removal were revealed. It was found Tl removal was rapidly increased to 98.5%, at conditions of P204 0.75 mol/L saponified 70% by ammonia, Tl 3.27 mg/L, O/A 1:1, T 298.15 ± 2 K, 250 rpm, and 3 min. McCabe-Thiele Tl extraction equilibrium isotherms indicates Tl concentration of raffinate less than 18.7 μg/L, a theoretical extraction of two stages and a theoretical stripping of two stages are required when both O/A work lines were at 1.0. Therefore, the method of the P204 solvent extraction system can effectively extract Tl in the forms of TlA(org), TlA3(org), TlOHA2(org), and Tl(OH)2A(org). Meanwhile, the new approach can be a promising process for ammonium rhenate refining.

Influence of Impurities on the Process of Obtaining Calcium Carbonate during the Processing of Phosphogypsum.

The article is devoted to the study of the influence of residual sulfuric and phosphoric acids on the process of processing large-tonnage phosphogypsum (PG) waste into calcium carbonate. In the Russian Federation, about 10 percent of existing phosphogypsum waste is processed into construction materials. Acidic impurities (phosphoric and sulfuric acids) in their composition are an obstacle to the use of phosphogypsum for the production of binders. This study finds that impurities also reduce the chemical activity of phosphogypsum. At the same time, the paper focuses on the potential of phosphogypsum for the production of calcium carbonate. This article investigated the amount of impurities in phosphogypsum. The results show that during automatic washing of phosphogypsum, losses are approximately 30–35 wt. %. It was also found that phosphogypsum by 22% consists of impurities of phosphoric and sulfuric acid. These acids are characteristic waste products of extraction phosphoric acid (EPA) production. By ASTM C471M-20ae1, the content of calcium sulfate dehydrate and hemihydrate before and after washing was determined. A thermodynamic calculation of the proposed interaction of phosphogypsum with carbonates showed that the characteristic reaction is possible. The conversion process of phosphogypsum to get the corresponding calcium carbonate was carried out at 70 °C. Data on the chemical composition of the reaction products, obtained by X-ray fluorescence analysis on a Shimadzu EDX-7000 spectrometer, showed that some reactions proceed incompletely and need the selection of optimal conditions. The potential commercial benefits of processing phosphogypsum by carbonization were defined for products such as calcium carbonate or its derivatives.

Rapid separation of High-viscosity phosphorous Acid/Tributyl phosphate extraction system by a stable anticorrosive Super-PA-phobic mesh

Inefficient, slow separation resulting from the high viscosity of phosphoric acid (PA) is a crucial problem that limits the process economy of industrial PA extraction. In this work, a super-PA-phobic stainless-steel mesh (SPPSSM) with excellent anticorrosion properties and stability is prepared and used for rapid separation in various PA/tributyl phosphate (TBP) extraction systems. The separation efficiency in batch operation of a PA-enriched raffinate (PER) and TBP-enriched phase (TEP) mixture formed from pure PA and TBP exceeds 97.59%, and the maximum TEP flux is 19.2593 L·m−2·h−1 at 60 °C. The maximum TEP flux of 886.1571 L·m−2·h−1 is obtained for a 20 wt% TBP kerosene solution and 20 wt% PA aqueous solution. A continuous separation device using the SPPSSM as the core component maintains a recovery rate of more than 95.57% in long-term operation, confirming its performance stability and robustness. The stable selective penetration of the SPPSSM originates from its super-PA-phobicity, which results from its rough surface with low surface energy; the SPPSSM repels PA but allows TBP to pass through. The separation ability of the SPPSSM is determined by the viscosity, density, and surface tension of the two liquid phases after extraction. It can be predicted using an equation based on the filtration mode after correction by a coefficient representing the Reynolds and Weber numbers. This work proposes a material for the rapid separation of PA/TBP in extraction systems and broadens the application field of superwetted materials under harsh conditions.

The mass transfer and mechanism of H3PO4 from low concentration HCl-route wet-process phosphoric acid by the mixture of n-butanol and isopropyl ether

• The mixed solvent of nBA and IPE was first used to extract H 3 PO 4 from HCl-route WPA. • The relation of E i, tal and N for all tested components were summarized. • The thermodynamic data of extraction process was calculated. • The mechanism and stage of H 3 PO 4 extraction were analyzed. Solvent extraction of phosphoric acid from wet process phosphoric acid produced by decomposing low grade phosphate with hydrochloric acid was investigated by the mixture of n-butanol (nBA) and isopropyl ether (iPE). The experimental results show that the mixture has good performance on P 2 O 5 extraction and Ca 2+ purification from HCl-route wet-process phosphoric acid. Optimization of extraction process shows that nBA has good performance for H 3 PO 4 separation at the condition of 5:1 O/A phase ratio, 293 K extraction temperature, 9:1 V B /V E ratio and 15 min extraction time. Based on the Van't Hoff equation, the enthalpy changes of P 2 O 5 extraction was calculated to be −16.41 kJ.mol −1 . The results from liquid-liquid mass transfer show three stages can achieved about 90 wt% P 2 O 5 extraction regardless of the countercurrent and cocurrent extraction. And the relation of total extraction percent and cross-flow extraction stages for all tested components were summarized. Moreover, the extraction mechanism between H 3 PO 4 and nBA was discussed by researching the extraction equilibrium under different conditions. The result showed that phosphoric acid was extracted in the form of H 3 PO 4 ·nBA, H 3 PO 4 ·2 nBA and H 3 PO 4 ·3 nBA complexes. Stripping operations using Deionized water as a extractant for phosphoric acid was also investigated at different conditions.

RESEARCH OF THE PROCESS OF SYNTHESIS OF DIAMMONIUM PHOSPHATE FROM EXTRACTIVE PHOSPHORIC ACID FROM BALANCED PHOSPHATESILICON SHAPES OF THE KARATAU BASIN

The article describes the process of obtaining extraction of phosphoric acid from phosphate-siliceous phosphorite shales of the Zhanatas deposit, by the sulfuric acid extraction method of obtaining EPA for use in the production of diammonium phosphate. Extraction decomposition of phosphorite by sulfuric acid proceeds with the formation of phosphogypsum and with fluorine released into the gas phase in the form of HF and SiF4 and processed into H2SiF6. The studies were carried out using circulating solutions of EPA with a concentration of 3.80-18.91% P2O5, phosphorite with a content of, (wt. %) P2O5 - 18.14; MgO - 13.43; Al2O3 -1.01; CaO - 25.1; F - 0.58; CO2 - 19.55, etc., sulfuric acid concentration of 92.5% was diluted to 50%. The norm of sulfuric acid is 100% of stoichiometry for CaO and MgO. The impurities Fe2O3 and Al2O3 present in phosphorite by 82-91% are extracted into the phosphogypsum precipitate in the form of medium phosphates. Fluorine introduced with phosphate raw materials into the extraction stage passes into the production acid by 60-70%, 10-20% – into phosphogypsum, and in a small amount 8-12% is released into the gas phase. The resulting EPA product can be used in the production of diammonium phosphate

Selective Recovery of Iron by Solvent Extraction from Ni-Laterite Leach Solutions, as Precursor for the Synthesis of High Added-Value Nanomaterials

Iron is the major impurity in the pregnant leaching solutions (PLS) derived from heap and atmospheric acid leaching of low-grade laterite ores. The PLS can be considered as a secondary resource for the synthesis of high added-value iron nanomaterials, provided that the iron is selectively separated from the polymetallic PLS solution. In this study, the feasibility of selective iron separation was investigated by applying a solvent extraction technique based on the use of Di-2-ethylhexyl phosphoric acid (D2EHPA) and Tri-butyl phosphate (TBP) extractants. The effect of several parameters such as initial pH and PLS composition was studied to identify the conditions allowing the maximum possible separation of iron with the minimum co-extraction of other valuable metals. It was found that the best separation of Fe could be obtained when the initial pH of the aqueous phase was regulated close to 1.4. The recovery of iron from the loaded organic phase was studied using sulfuric acid as stripping reagent and elemental iron as solid reducing agent. It was found that 90% of Fe(III) could be stripped out by applying the metallic iron (galvanic) stripping.

Hybrid Ultra-Low-Radioactive Material for Protecting Dark Matter Detector from Background Neutrons.

A laboratory technology for a new ultra-low background hybrid material (HM) which meets the requirements for neutron absorption with simultaneous neutron detection has been developed. The technology and hybrid material can be useful for future low background underground detectors designed to directly search for dark matter with liquid noble gases. The HM is based on a polymethylmethacrylate (PMMA) polymer matrix in which gadolinium nuclei are homogeneously distributed up to 1.5 wt% concentration in polymer slabs of 5 cm thickness. To determine the 65 impurity elements by the inductively coupled plasma mass-spectrometry (ICP-MS) technique in the Gd-based preparations in 100–0.01 ppb range, the corresponding method has been developed. Limits of determination (LD) of 0.011 ppb for uranium, and 0.016 ppb for thorium were achieved. An analysis of Gd raw materials showed that the lowest contents of U and Th (1.2–0.2 ppb) were detected in commercial Gd-based preparations. They were manufactured either from secondary raw materials (extraction phosphoric acid) or from mineral raw materials formed in sedimentary rocks (phosphogypsum). To produce the Gd-doped HM the commercial GdCl3 was purified and used for synthesis of low-background coordination compound, namely, acetylacetonate gadolinium (Gd(acac)3) with U/Th contents less than LD. When dissolving Gd(acac)3 in methylmethacrylate, the true solution was obtained and its further thermal polymerization allowed fabrication of the Gd-doped PMMA with ultra-low background.

Extraction methods of rare-earth elements from extraction phosphoric acid

Extraction methods of rare-earth elements from extraction phosphoric acid