Ferric phosphate can be used in many fields, for example as a mineral-rich food additive or nutritional supplement, as an active substance in molluscicides, in the ceramic industry, or as LiFePO4 for the production of lithium-ion batteries Raw materials for cathode materials. In this regard, each application area has different requirements for iron phosphate, and in some specific applications, chemical purity is critical. In many cases, the morphology or particle size of the iron phosphate is also extremely important for successful application, for example when considering the bioavailability of the organism. Rechargeable lithium-ion batteries are power storage devices that are extensively used, especially in the field of mobile electronic devices, because lithium-ion batteries are identified by high energy density and also supply a high ranked voltage of 3.7 volts, which is comparable to conventional batteries. Lithium-ion batteries are considerably smaller sized as well as lighter than, with equivalent power result. Spinels such as LiCoO2, LiNiO2, LiNi1 ^ xCoxO2 as well as LiMnnO4 have been identified as cathode products. To enhance the dependability and also safety and security of Li-ion batteries (particularly regarding thermal overload in operation), LiFePO4 has actually been developed as a cathode material. This material is defined by better power outcome, greater specific capacitance, as well as high thermal stability in operation. Cathode materials for batteries require high pureness considering that any type of contamination that can trigger undesirable redox responses throughout procedure (charging or releasing) can negatively influence the power of the battery. The nature and focus of possible contaminations depend essentially on the top quality of the raw materials used to generate the cathode material. Succeeding measures to reduce impurities can be implemented in the cathode material production procedure, but this usually leads to increased production prices. It is therefore desirable to utilize raw materials or beginning products that are as pure as possible to create cathode products.
Ferric Phosphate Properties:
Melting point
1000 °C
density
2.870
form
gray-white orthorhombic crystals
Water Solubility
insoluble H2O; soluble HCl [MER06]
Ferric Phosphate Uses
Ferric Phosphate is used in the food industry as a nutritional supplement (iron fortifier), especially in bread. Also used as feed additive.
IFerric Phosphate is used as food and feed additive.
Ferric Phosphate Invention
In order to overcome the above-mentioned defects under the prior art, the object of the present invention is to provide a method for preparing Ferric Phosphate, which has low production cost, is environmentally friendly, and has high purity of the prepared Ferric Phosphate. The technical scheme of the present invention is: A method for preparing iron phosphate, comprising the following steps: (1) iron: placing iron in a phosphoric acid solution, heating to carry out iron reaction, and obtaining a reaction solution containing Fe(H PO ) ; ( 2) oxidation: in the filtrate of described reaction solution, add hydrogen peroxide, carry out oxidation reaction under stirring state, then add polyethylene glycol and continue to stir, make Fe (H PO ) Reaction generates Ferric Phosphate, obtains the liquid after oxidation; ( 3) hydrolysis: add distilled water to the described oxidation back liquid, carry out hydrolysis reaction; (4) filter washing: carry out solid-liquid separation to the feed liquid after the hydrolysis, and wash the separated solid phase discharge to the pH value of the washing liquid Reach near-neutrality, spin-dry to obtain solid iron phosphate; (5) Dehydration: the solid iron phosphate after spin-drying is successively dried and dehydrated to form dehydrated iron phosphate. In the described iron-forming step, the preferred range of temperature of reaction is 70-95 ° C, and the reaction times is preferably 3-8 hours. In the described ironing step, the iron used is an iron rod, and the iron rods are stacked in the reactor, and then the phosphoric acid solution is added to the reactor. The phosphoric acid used for preparing the phosphoric acid solution is preferably food grade phosphoric acid, and the water used is pure water. For the aforementioned any one of the described ferric phosphate preparation methods, the oxidation step can all be operated according to the following content: at the reaction temperature, carry out the stirring of the reaction solution, slowly add hydrogen peroxide with a trickle while stirring, add a The polyethylene glycol solution is added after the hydrogen oxide, and the starting time of adding the polyethylene glycol solution is 50-70 minutes after starting to add hydrogen peroxide, until Fe (H PO ) The reaction reaches the end of the process. The mass concentration of the polyethylene glycol solution is 30-55%. The reaction temperature of the oxidation reaction is 18-45 ℃. For the preparation method of any one of the aforementioned ferric phosphate, the hydrolysis step can be: add the distilled water required for hydrolysis, stir after 5-10 minutes, be heated to 70-90 DEG C, and be incubated for 50-70 minutes. For the preparation method of any one of the aforementioned ferric phosphate, the filtration and washing steps can be as follows: using a filter press to perform solid-liquid separation, and the solid-phase discharge is introduced into a centrifuge for one or more centrifugal washing and drying. , when the pH value of the washing liquid discharged from the centrifuge is 5.9-6.1, stop water washing and continue to spin dry to obtain solid iron phosphate. The dehydration step can be: the solid iron phosphate obtained by the filtration and washing step is removed by flash evaporation to remove surface water, producing dry FePO . Anhydrous ferric phosphate. The beneficial effects of the present invention are: using iron phosphate and hydrogen peroxide oxidation to replace the strong acidified iron in the traditional process, the cost of raw materials is lower than that of using strong acid, because other metal cation impurities and other acid radical impurities will not be introduced, on the one hand, in order to obtain High-purity ferric phosphate provides a strong guarantee, does not lead to residual strong acid radicals, and does not need to deal with by-products. Therefore, it is not necessary to set up additional process steps such as purification and adjusting the pH of the product, and the production cost can be further reduced. Chemical pollutants such as sulfur dioxide are produced, which is beneficial to reduce or avoid pollution to the environment.
Ferric Phosphate Specific Embodiment
The process flow of the method for preparing iron phosphate of the present invention includes reacting iron and phosphoric acid to generate ferrous dihydrogen phosphate Fe(H PO ) (that is, iron), and reacting ferrous dihydrogen phosphate and hydrogen peroxide to form a ferric phosphate suspension (that is, Oxidation), heating to obtain iron phosphate solid (i.e. hydrolysis, filtration, washing), through drying and dehydration (i.e. dehydration) to form anhydrous iron phosphate.
Concrete production technological process can be: (1) ferrite process configuration 16-25% phosphoric acid solution: phosphoric acid (preferably food grade) is slowly stirred into pure water, and is mixed with standard phosphoric acid solution.
In the reactor, stack the iron rods of the specification, add an appropriate amount of standard phosphoric acid solution, be heated to 70-95 ℃ and carry out the iron reaction Fe+2H3PO4=Fe(H2PO4)2+H2, after the reaction 3-8 hours, measure dihydrogen phosphate When the content of ferrous Fe(H2PO4)2 reaches about 18-20%, the reaction solution is filtered until it is clean and transparent without suspended sediment, and the obtained filtrate is used for the oxidation process.
(2) oxidizing operation The filtrate is squeezed into the reactor, heated to 18-45 ℃, start stirring, slowly add hydrogen peroxide (can be technical grade) with a trickle, react after 50-70 minutes, continue to stir, Add 30-55% polyethylene glycol solution of dispersant until the reaction is complete. The amount of hydrogen peroxide added is set according to the needs of the reaction, which can usually be slightly larger than the amount of reaction completed by the process. The amount of dispersant added can be based on process conditions. determined experimentally or empirically.
The reaction equation is: 2Fe(H2PO4)2+H2O2=2FePO4+2H3PO4+2H2O.
(3) hydrolysis process Add an appropriate amount of distilled water to the solution after oxidation, stir after about 5-10 minutes, be heated to 70-90 DEG C, be incubated after 50-70 minutes, fully hydrolyze, and fully analyze the iron phosphate crystal.
(4) Pressure filtration washing process The hydrolyzed feed liquid is separated by pressure filtration with a filter press, the filtrate is collected, the filtered solid phase material is introduced into the centrifuge, washed with water, and then dried, and after the collection and washing Washing and drying are repeated until the pH value of the washed solution reaches the above range.
(5) Drying and dehydration process The surface water of the solid ferric phosphate after being spun in the centrifuge is removed by flash evaporation to produce dry ferric phosphate dihydrate FePO4·2H2O. Then, the iron phosphate dihydrate is introduced into the stove, and dehydrated at a high temperature of 380-420 ° C to form iron phosphate.
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The production base is located in Zhangqiu chemical industry park and Tai’an high-tech chemical industry park. laboratory and workshop in strict accordance with the GMP standard and the product fit national ISO9001 and ISO2000 standards.
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