The method of obtaining translesanas phosphate magnesium
(57) Abstract:The invention relates to the production of phosphate salts of magnesium, particularly to a method of obtaining high-water translesanas phosphate magnesium [Mg3(PO4)2nH2O] suitable for use as hydrated on the units for production of desalinated water, and it may also find application as catalysts, adsorbents and light fillers. Abounding trehzameshchenny phosphate magnesium with a highly developed surface of the crystalline separated from the suspension mixed aqueous solution at t = 60-70oC and pH 7,0-7,5 by mixing a previously prepared solution of caustic potash or potash with phosphoric acid with the molar ratio of potassium to phosphorus in the solution is 3:1, which is then mixed with a solution of magnesium sulphate, the molar content of magnesium which is equivalent to the molar content of potassium in the initial solution of a mixture, and from the mother liquor of the slurry after separation from it of magnesium phosphate secrete potassium sulfate by vacuum crystallization residue. The technical result consists in obtaining abounding translesanas phosphate magnesium with highly active poverhnostnie, specifically to a method for abounding translesanas phosphate magnesium [MD3(RHO4)2mo2About] suitable for use as hydrated on the units for production of desalinated water, and it may also find application as catalysts, adsorbents and light fillers.A known method of producing remanifest in French patent 2431460 on the application 7515401 from 15.06.79, including a method of obtaining potassium phosphate and magnesium by reacting aqueous acidic solutions containing phosphate ions with potassium chloride and magnesium compounds with the properties of the base, characterized in that dissolve in acidic solution containing 20-160 g P2O5100 g of water, the amount of magnesium compound with the properties of the base, is stoichiometrically required for the formation of demanifest, and part of the total required quantity of potassium chloride, the resulting suspension is slowly injected after the addition of the remaining quantity of potassium chloride (the total amount reaches the molar ratio of K2O:P2O3from greater than 1:1 to a value slightly less than the saturation concentration), at a temperature below 40oFrom: the stoichiometric kolichestvennaia 130 g MgCl2in 1000 g of water in the reaction mixture; then separate the product from the mother liquor, washed it and dried.The main disadvantage of this method is the complexity and multi-stage process and the lack of ways to control the dosing of the reagents in the practical implementation of the method. No indication of the quality of the final product and not solved the problem of processing obtained in the mother liquor.A known method of producing oxide hydrate translesanas phosphate magnesium auth. St. 636182 from 7.04.77, by reacting solutions of magnesium sulfate, dogsleding of sodium phosphate and sodium bicarbonate followed by filtration and drying of the product, characterized in that in order to simplify the process and reduce its activity, solutions served simultaneously and the process is conducted at 45-60oWith, you get a product according to the experiment of the following composition: MgO - Of 28.9%; P2O3OR 34.7%; H2O - 36,2%.The disadvantage of this method is a product with a low content of water of crystallization and the lack of solutions for the regeneration of the mother liquor obtained after separation from the suspension of the target product. No the ukta.The technical object of the present invention to provide a wet translesanas phosphate magnesium with highly active surface of the obtained crystalline.The technical result is reached that abounding trehzameshchenny phosphate magnesium with a highly developed surface of the crystalline separated from the suspension mixed aqueous solution at t=60-70oC and solution pH equal to 7.0 and 7.5, by mixing a previously prepared solution of caustic potash or potash with phosphoric acid with the molar ratio of potassium to phosphorus in the solution is 3:1, which is then mixed with a solution of magnesium sulphate, the molar content of magnesium which is equivalent to the molar content of potassium in the original solution mixing. From the mother liquor of the slurry after separation from it of magnesium phosphate secrete potassium sulfate by vacuum crystallization residue.In the above-mentioned conditions of the suspension is excreted in the sediment water trehzameshchenny phosphate of magnesium, holding composed of up to 85% of crystallization and external moisture. When multiple dehydration of the hydrated phosphate of magnesium by heating it to 150-160oWith subsequent repulpable his podcastalley patterns.An example of practical implementation of the proposed method.1. Experience with caustic potash
400 mm solution containing 86 grams of KOH was mixed with a concentrated solution of phosphoric acid containing 50 g of N3RHO4that corresponds to a molar ratio of potassium to phosphorus 3:1. Prepared phosphatecalcium solution under vigorous stirring at t=60oWith neutralized prepared parallel to 400 mg of a solution of magnesium sulphate, containing 195 g MgSO47H2Oh, what an equivalent molar content of potassium in the original solution mixing. After complete mixing of the solutions prepared pH of the mixed stock solution was increased to 7.0 and from it almost completely knocked out wet hydrated translesanas of magnesium phosphate. The weight of the washed filter cake was 420 g, which corresponds to the weight content MD3(RHO4)2- 16,3%; H2On - 83,7%. After drying and calcining at t=150oWith the weight digidratirovannogo phosphate magnesium amounted to 89 g, which corresponds to the weight of the chemical composition in the sediment MD3(RHO4)2- 87.3 PER CENT; N2O - 12,5%. When reprocessing digidratirovannogo phosphate magnesium water in the tech what's repetition of the process of dehydration filtered hydrated and re-process it with water weight digidratirovannogo and saturated with water it remained virtually unchanged at 88-89 g after dehydration and 320-330 g after saturation with water.From the mother liquor, after separation translesanas phosphate magnesium by vacuum crystallization residue at t=50oWith allocated precipitated 120 g of potassium sulfate.2. Experience with K2CO3(potash)
420 g of a solution containing 106 g2CO3mixed with a concentrated solution of phosphoric acid containing 50 g of N3RHO4that corresponds to a molar ratio of potassium to phosphorus in solution 3:1. When mixing acid with a solution of potash been emitted from a solution of 34 g of CO2which if necessary can be captured and recovered in liquid or solid CO2.The obtained phosphorus-potassium solution was mixed with t-60oWith g cooked in parallel 400 ml solution of magnesium sulphate, containing 195 g MgSO47H2O, which corresponds to a molar equivalent to the content of potassium in the original califorina solution. After complete mixing of the solutions prepared pH of the mixed solution was raised to 7.0, it dropped into the sediment hydrated translesanas of magnesium phosphate. The weight of the filtered precipitate amounted to 424 g, which corresponded to the content of SB3(RHO4)2AND 16.2%, N2About 83.8 percent. After drying and Prony MD3(RHO4)2- 87.8% and N2About to 12.2%. After processing digidratirovannogo sediment water for 20 min weight the filtered precipitate was 325From the mother liquor, after separation of phosphate magnesium by vacuum crystallization residue and one stripped off cooling fluid to the 50oWith the highlighted residue 123 g K2SO4. 1. The method of obtaining translesanas phosphate of magnesium, comprising the mixing equivalent ratio of solutions of phosphate and magnesium salts, characterized in that the high-water trehzameshchenny phosphate magnesium with highly active surface of the crystalline separated from the suspension mixed aqueous solution at t= 60-75oC and pH 7,0-7,5 by mixing a solution of caustic potash or potash with phosphoric acid with the molar ratio of potassium to phosphorus equal to 3: 1, which is then mixed with a solution of magnesium sulphate, the molar content of magnesium which is equivalent to the molar content of potassium in the original solution blending.2. The method according to p. 1, characterized in that from the mother liquor of the slurry after separation from it of magnesium phosphate secrete potassium sulfate by vacuum crystallization residue.
FIELD: industrial inorganic synthesis.
SUBSTANCE: monocalcium phosphate, widely applied in agriculture, is prepared by mixing extraction phosphoric acid with calcium-containing component followed by granulation and drying of product. During mixing of components, appropriate temperature and moisture are maintained to ensure viscosity of mixture 3-7 mPa*s, and granulation and drying are carried out simultaneously in drum-type granulator drier. Calcium-containing component is either calcium carbonate or mixture thereof with limestone, whose does not exceed 15% of total weight of calcium-containing raw material. Moisture content in worked out drying agent leaving drum-type granulator drier equals 70-80 g per 1 kg dry air.
EFFECT: simplified process flowsheet, enabled granule size control, and increased strength of granules.
3 cl, 3 ex
FIELD: inorganic chemistry, chemical technology.
SUBSTANCE: invention relates to technology for preparing fodder calcium phosphates, namely to producing monocalcium phosphate. Method involves mixing wet-process phosphoric acid with a calcium-containing component in the presence of recycle, granulation and drying the product. Mixing process is carried out for two stages. At the first stage wet-process phosphoric acid with the concentration 62-65% of P2O5 is fed and process is carried out at recycle index = 1:(0.3-0.5) up to decomposition degree of calcium-containing raw = 0.89-0.92 at this stage. The second stage is combined with granulation and carried out its in high-speed mixer in water addition to obtain moisture in mixture 9.5-13%. The rate and time for mixing are regulated to provide the decomposition degree of calcium-containing raw = 0.93-0.99, and temperature at the next drying stage is maintained in the level 105-115°C. Method provides simplifying the process, reducing energy consumption and preparing product with the high content of P2O5 in water-soluble form and low content of fluorine.
EFFECT: improved method for preparing.
2 cl, 3 ex
FIELD: production of pure phosphoric acid and calcium monohydrophosphate.
SUBSTANCE: proposed method includes decomposition of phosphate ore by first hydrochloric acid solution at concentration not exceeding 10 mass-%, separation of liquid decomposition product into insoluble solid phase containing admixtures and separate aqueous phase containing phosphate, chloride and calcium ions in form of solution, neutralization of aqueous phase separated from liquid decomposition product by adding calcium compound for obtaining insoluble settled-out calcium phosphate by means of phosphate ions, separation of neutralized aqueous phase into aqueous phase containing calcium and chloride ions in form of solution and settled solid phase on base of water-insoluble calcium phosphate and dissolving of at least part of separated settled solid phase in second aqueous hydrochloric acid solution containing hydrochloric acid in the amount exceeding its content in first hydrochloric acid solution, thus forming aqueous solution containing phosphate, chloride and calcium ions extracted by organic extracting agent at extraction in "liquid-liquid" system. Proposed method makes it possible to avoid fine grinding or roasting of ore.
EFFECT: enhanced efficiency of extraction for production of pure concentrated phosphoric acid solution with no contamination of surrounding medium.
24 cl, 2 dwg, 1 tbl, 4 ex
FIELD: paint and varnish industry.
SUBSTANCE: anticorrosive pigment comprises , in mass per cents, 3.0-4.7 of calcium chromate and waterless dicalciumphosphate as the balance.
EFFECT: improved anticorrosion capabilities.
SUBSTANCE: method of processing of residual products containing phosphoric acid to calcium phosphates comprises its mixing with calcium-containing compounds, separation of derived slurry with filtration and drying. The limestone is used as calcium-containing compound, initially it is fed for mixing in quantity necessary for monocalcium phosphate, then derived slurry is divided to two flows in ratio 1:(1.5-4), the major flow is mixed with lime taken in quantity necessary for dicalcium phosphate formation, derived slurry is separated with filtration and minor flow of monocalcium phosphate slurry is added to separated dicalcium phosphate before drying and granulating. Preparation of monocalcium phosphate slurry is carried out in two stages, at first stage the phosphoric acid is mixed with limestone up to mixture pH =2.9-3.1, at second stage - up to mixture pH =3.5-3.7, during mixing of monocalcium phosphate slurry with lime pH is maintained in the range 5.4-5.6. Drying and granulating are carried out at the same time in drum granulator-dryer.
EFFECT: method enables to process the residual products to granulated calcium phosphates with usage the lowest-cost raw materials.
3 cl, 1 tbl, 1 ex
SUBSTANCE: invention relates to technology of obtaining inorganic materials, namely to methods of obtaining nanosized highly pure hydroxylapatite (HAP) in form of colloid solution or gel, which can be used for production of medico-preventive preparations for stomatology, for application on bone implants. Method of obtaining nanosized colloid hydroxylapatite includes synthesis of hydroxylapatite in saturated solution of calcium hydroxide, decanted after 24-hour settling from sedimented aggregates Ca(OH)2, by adding at rate 1.5-2.2 ml/min per litre of alkali solution 10-20% solution of orthophosphoric acid with constant mixing until pH value of reaction mixture is not lower than 10.5±0.5. Mixture is mixed during 20-30 minutes, settled during 1-2 hours and decanted until liquid phase stops forming on the surface. Obtain product represents colloid solution of highly pure hydroxylapatite with concentration 1.5-2%. Increase of hydroxylapatite concentration within the range from 2 to 30% is carried out by evaporation at temperature not higher than 60°C, and for obtaining nanosized hydroxylapatite with concentration 40±2% initial colloid solution is subjected to complete freezing with further unfreezing at temperature not more than 60°C and liquid phase decanting.
EFFECT: obtaining stable product with set in advance concentration, possessing higher penetrating ability and biochemical activity.
3 cl, 4 ex
SUBSTANCE: nano-sized highly-pure hydroxylapatite (HAP) is obtained in form of alcohol colloid solution (gel), which can be used for production of medicinal preventive preparations in stomatology, for applying bioactive coating on bone implants. Method includes hydroxylapatite synthesis by adding solution of orthophosphoric acid to calcium hydroxide solution and exposure to ultrasound impact, and ethyl or isopropyl alcohol is added to colloid of highly-pure nano-sized hydroxylapatite with concentration from 5% to 40±2% in order to obtain concentration of hydrooxylapatite in alcohol from 0.2 to 20%. After that alcohol mixture is processed with ultrasound with frequency 10-50 kHz during 1-2 hours.
EFFECT: alcohol colloid of nano-sized hydroxylapatite with high stability.
2 cl, 3 ex
SUBSTANCE: method of phosphate ore processing includes one-step counterflow process of phosphate ore decomposition, characterised by P2O5 content exceeding 20% in weight, by processing it with water solution of hydrochloric acid, which has HCl concentration lower than 10% in weight, with formation of processing solution, consisting of water phase, in which calcium phosphate is in dissolved state, and of solid phase, which contains admixtures; preliminary neutralisation of processing solution, containing calcium phosphate in solution, to first pH value, which is lower than pH value, at which essential part of said dissolved calcium phosphate precipitates in form of calcium monohydrophosphate (DCP), with precipitation of admixtures; first separation of insoluble solid phase and water phase of processing solution; repeated neutralisation of water phase obtained during first separation to second pH value, exceeding said first pH value, with DCP precipitation; and second separation of repeatedly neutralised water medium, which represents water solution of calcium chloride and precipitated DCP.
EFFECT: method allows optimising ratio between dissolved P2O5 output and purity degree of final product and ensure economically profitable process, which can be realised on simple equipment.
14 cl, 3 dwg, 2 tbl, 1 ex
FIELD: medicine, pharmaceutics.
SUBSTANCE: it is described a nanopatterned calcium phosphate material on the basis of threecalciumphosphate-hydroxyapatite system for reconstruction of osteal defects. The invention concerns to the calcium phosphate ceramic materials intended for manufacturing of osteal implants and-or replacement of defects at various osteal pathologies. The material on the chemical compound is close to a natural osteal tissue (the structure corresponds to the threecalciumphosphate-hydroxyapatite system). The unique ultradisperse structure of a material is formed at the expense of use of initial calcium phosphate nanopatterned powders and the additive.
EFFECT: reception of a ceramic material with uniform structure with the average size of particles less than 100 nanometres.
1 tbl, 3 ex
SUBSTANCE: invention relates to method of receiving of nano-crystalline hydroxyapatite. According to the invention calcium nano-crystalline hydroxyapatite is received by interaction of compound of calcium and ammonium hydro-phosphate. In the capacity of calcium compound it is used sugar lime C12H22-2nO11Can, at n, which is situated in the range from 0.5 up to 2. Particles size of the received hydroxyapatite is 30-50 nm.
EFFECT: receiving of nano-crystalline powder of calcium hydroxyapatite, which contains unaggressive biocompatible accompaniment of the reaction and that provides its usage in medicine.
3 dwg, 1 tbl, 1 ex