METHOD FOR PRODUCING IRON (III) PHOSPHATE FePO4 POWDER FROM NON-CONCENTRATED IRON SAND

Abstract

The present invention relates to the preparation of iron(III)phosphate, FePO4, from raw iron sand or non-concentrated iron sand consisting of iron titanate, iron oxide, titanium dioxide, aluminum oxide, silica, and calcium oxide. More specifically, the FePO4 material according to the present invention is in the form of a powder based on iron and phosphate.

Description

METHOD OF PRODUCING IRON (III) PHOSPHATE POWDER FePO, FROM SAND NON-CONCENTRATED IRON Invention Engineering Field The present invention relates to the manufacture of iron (III) phosphate, FePOi, from raw iron sand or non-concentrated iron sand, with Fe content less than 508. More specifically, FePOs material in accordance with this invention in the form of a powder based on iron and phosphate. Background of the Invention Iron sand, usually processed using the rotary kiln method to produce sponge iron. This method reacts iron sand with carbon monoxide, CO and hydrogen gas, H2. In the rotary kiln process, Fe(II) or Fe(III) will be reduced to Fe(o) by CO gas. This method can be very dangerous. because carbon monoxide is poisonous. In addition, the method Rotary kilns also require high operating temperatures. In this invention, iron sand processing is carried out in a hydrometallurgy through caustic fusion reactions and acid leaching to produce iron (III) hydroxide, Fe(OH)3, then deposit it as iron(III)phosphate through the reaction with phosphoric acid, H3POa4. Initial analysis on iron sand found that in raw iron sand or non-concentrate, the iron element Fe is present in the form of magnetite, Fe304, hematite Fe203, limonite Fe203.nH20 and siderite FeCcO3. The presence of the element Fe in various forms oxide requires a strategy to obtain concentrate High Fe(OH)3 and then get the compound FePOz with high purity. The reaction for making FePOs takes place through the following mechanisms: Fe203 syt 2H2S0Ox tag) 5D 2FeSOatagt 2H20tamy t & Oz9) (1) FeSOa tag) #2NA0H tam DFe (OH) 2» tag) #Na2SOx tag) (2) 2Fe (OH) ata t 2H3POatay D 2FePOatsy £ 2H20tay £ 3H2x0) (3) The prior art regarding the manufacture of FePOa is CN103754855A, patented in China on 66-12-2011. Invention about the method of making FePO4 from iron raw materials industrial. Industrial iron or iron sand concentrate is an industrial standard raw material with an iron content of quite high, namely 2,588. The method consists of 3 steps, namely the manufacture of iron concentrate solution, manufacture of iron solution phosphate concentrate, and mixing the two concentrate solutions This method requires de-ionized water, or distilled water. which has had its mineral ions removed. Another invention is entitled Simple preparation method for FePo4 Chinese patent CN103427081A dated 13-8-2013. This method uses nitric acid solution and sodium hydroxide solution. ammonium monohydrate phosphate. Ammonia solution is used for adjust the pH of the solution so that it is in the range of 1.8 - 2.4. Iron(III)phosphate, anhydrous 5FePOs is obtained through the process roasting at a temperature of 400-900 Cc. This invention also using iron concentrate raw materials that have a certain content tall. Existing inventions have not disclosed direct synthesis of FePOs from iron sand with Fe content which is still low and still in various forms its oxide compounds. Therefore, it is an object of the present invention to provide a method of making FePOs compounds directly from raw iron sand or non-concentrated iron sand with a content of Fe less than 50 8&$. Brief Description of the Invention In accordance with the present invention, there is provided a FePOy powder and method of manufacture. FePOs according to the present invention is in the form of powder which is a compound of the elements iron and phosphate. While the manufacturing method according to this invention has the stages are: grinding iron sand with NaOH on the mass ratio of iron sand:NaOH is 1:0.5 to 1:1: The mixture is heated in a furnace at a temperature of 500 - 700 SC for 2 hours: the heating results are then leached with distilled water excess during three leaching: the results of the third leaching then leached with excess HCl 378 solution at a temperature of 90 SC, filtered and the filtrate was taken: / , filtrate added with excess H202 30 $ slowly so that a FeCl3 solution is formed, the solution that is formed added with NaOH solution in a volume ratio of 2:1 until a brown Fe(OH)3 precipitate is formed: precipitate Fe(OH)3 is added to the H3POs solution until a precipitate is obtained. brownish yellow: the sediment is separated and washed with distilled water until the pH is neutral: the sediment that has been The neutral pH is heated at a temperature of 600 - 800 SC for 3 hours. Short Description of Image To facilitate understanding of this invention, it is included some pictures. Here is an explanation of the pictures as stated in the invention: Figure 1, is the X-ray diffraction pattern of FePOs powder at before heating or calcination and after calcination. The diffraction pattern is compared with the standard diffraction pattern of FePOs. Figure 2, results of refinement of X-ray diffraction data with Le Bail's method Figure 3, is the result of Scanning Electron Microscope analysis from FePOs powder Complete Description of the Invention The present invention concerns iron(III)phosphate powder, FePOs, which can be used as raw material for making electrodes lithium ion batteries, sodium battery electrodes, and other chemical needs. FePOs powder is made directly from low Fe content iron sand, namely less than 50 $&$. Synthesis is carried out using the hydrometallurgical method through caustic fusion reaction with NaOH followed by water or distilled water leaching and HCl acid leaching. Reaction the formation of Fe(OH)3 is done by adding H20O», while the formation of FePOs is carried out through a reaction with H3POu. The reaction product obtained is heated to get FePOua powder. The formation of FePOs4 follows the reaction stages as follows: following: - grinding iron sand with NaOH in a mass ratio iron sand:NaOH, namely 1:0.5 to 1:1, - heating the mixture in a furnace at a temperature of 500 - 700 Cc for 2 hours, - leaching the heating results with excess distilled water for three times leaching, - continue leaching with excess HCl 3 / 8 solution at a temperature of 90 SC, - filter the leaching results and take the filtrate, - add the filtered filtrate with H202 30 $ excess slowly until it forms FeCl solution:., — add FeCl solution: with NaOH solution to volume ratio 2:1 until Fe(OH)3 precipitate forms brown, - add Fe(OH)3 precipitate: with H3PO4 solution until a brownish yellow precipitate was obtained, - separate the brownish yellow sediment and wash it with distilled water until the pH is neutral, - heating the precipitate which has a neutral pH temperature 600 -— 800 SC for 3 hours. The FePO4 powder in this invention has a diffraction pattern which corresponds to the FePOs diffraction standard, as listed in Figure 1. While the refinement of the diffraction data shows that the FePOs powder in this invention has a crystal structure trigonal and space group P3121.Crystal cell parameters of the results refinement are listed in Table 1, while the Le Bail plot The refinement results are listed in Figure 2. Powder morphology FePOs is in the form of spherical particles with a rough surface, such as shown in Figure 3. Particle size analysis based on The surface morphology image shows that the FePOa powder in this invention is in the range of about 10 microns in diameter. Table 1. Cell parameters resulting from powder diffraction data refinement FePO, in this invention FePOs cell parameters Trigonal crystal structure Gugus ruang P 31 2 1 a (A) 5,041995 b (A) 5,041995 c (A) 11, 263653 OL 90” B 90” y 120” Volume sel (A) 247, 978806 Rp (8) 2,64 Rwp (S8) 3,71

Claims

1. A method for making FePOy powder from non-ferrous iron sand concentrate, namely raw iron sand with a low Fe content low, less than 50$ which has stages as follows: a. grinding iron sand with NaOH in a mass ratio iron sand:NaOH, namely 1:0.5 to 1:1, b. heating the mixture in a furnace at a temperature of 500 - 1700 Cc for 2 hours, c. leaching the heating results with excess distilled water for three times leaching, d. continue leaching with excess HCl 378 solution at a temperature of 90 SC, e. filter the leaching results and take the filtrate, £. add the filtered filtrate with H»202 30 & excess slowly until it forms FeCl solution:., g. add FeCl3 solution with NaOH solution volume ratio 2:1 until Fe(OH)3 precipitate forms brown, h. add Fe(OH)3 precipitate with H3POs solution until a brownish yellow precipitate was obtained, 1. separate the brownish yellow sediment and wash it with distilled water until the pH is neutral, J7. Heat the precipitate which has a neutral pH at a temperature 600 -— 800 SC for 3 hours.