The method of obtaining basic carbonate salts of copper, zinc, nickel and cobalt and their oxides

 

(57) Abstract:

The invention relates to the technology for basic carbonate salts of copper, zinc, Nickel and cobalt and their oxides, which can be used as raw materials and intermediates in the production of catalysts and absorbents in the chemical and petrochemical industries. The method involves dissolution and simultaneous oxidation of metal ions from various types of raw materials (metal, inactive oxides, hydrocodon) at an elevated temperature and a predetermined molar ratio metal: ammonia: carbon dioxide to obtain a saturated solution of Aminatou with concentration, temperature and dalvenie, allowing to spend their thermal decomposition in an intensive mode and full reator. To intensify the process sozdana conditions of circulation of the solution and removal of gaseous reaction products, while liquid and gaseous reaction products production recycle and use again in the process. The performance of the continuous process stream in 3-4 times higher than in the known way and is 14000 - 27000 kg/day for copper and zinc and 7000 14000 kg/day for compounds of Nickel and cobalt. The way pototoe and dispersion. table 1.

The invention relates to the technology for basic carbonate salts and oxides of copper, zinc, Nickel, cobalt and mixtures thereof and can be used as raw materials and intermediates in the production of catalysts and absorbents used in the chemical, petrochemical, paint, hydrometallurgical and electrochemical industries.

A known method of producing hydroxocobalamin Nickel and zinc by dissolution of these metals in the ammonium carbonate solution at elevated temperature and subsequent deposition of the desired product by distillation of the ammonia, and dissolved metals are in the presence taken separately or in combination with each other nitric acid, ammonium nitrate, Nickel or zinc content of nitrate-ion 2-50% with respect to the mass of dissolved metals [1]

A method of obtaining the primary carbon dioxide by dissolving cobalt metal cobalt ammonium carbonate solution at 50-65aboutWith the separation from solution of iron-containing sludge decomposition of ammonium carbonate complex of cobalt, separating the resulting suspension, followed by washing and drying the precipitate, and to reduce the m solution with a ratio of CO2:NH31:3-4 [2]

Also known periodic method of obtaining the basic carbonate or oxide of copper, zinc or Nickel, including the decomposition of the solution to the ammonia-carbonate complex by distillation of the ammonia gas mixture at an elevated temperature in the presence of lignin sulfonate in an amount up to 0.5% of the mass of metal in the initial solution, while the main carbonate Cu, Zn or Ni is produced by decomposition of the corresponding complex at a temperature 80-91, 80-95, about 80 to 98aboutC, and the oxide of Cu, Zn or Ni at a temperature 93-100, 97-100, 100-105aboutS, respectively, then the finished product is separated and dried [3]

The main disadvantages of these methods are: low productivity of the process, the frequency and the low efficiency of each operation, the presence of large amounts of wastewater due to the need for periodic cleaning equipment [2, 3] and emissions due to the large losses of gaseous products contaminated with impurities [1, 3]

Closest to the invention to the technical essence and the achieved result is a method of producing oxides of copper or zinc, including the dissolution of the metal in ammonium carbonate solution at ambient temperature and molar autocamionale (if necessary) the resulting solution, i.e. the translation of Aminatou Cu+in ammirati Cu2+by additional oxidation of the solution in a special apparatus (aerator), thermal decomposition of the obtained Aminatou, by feeding into the reactor-evaporator saturated solution of Aminatou containing 120-160 g/l Cu2+or Zn2+at a temperature no higher than 54aboutWith a pressure of 100 kPa, the feed rate of the solution 2-3 m3/h or 0.06-0,17 about. the relative volume of the reactor in 1 h, and a saturated solution served by sputtering on the surface in the reactor core solution, the temperature of which is maintained within the range of 101-103aboutWith by circulation through an external heat exchanger. Resulting from the reaction of oxides deposited in the tapered lower part of the reactor and are removed from the system after the complete processing of a given quantity of saturated solution and stopping feed to the reactor, as well as interrupting the main solution. Gaseous reaction products, located in the upper part of the reactor pressure 35-70 kPa, output (drossellied) to the condenser, where ASG condense at a temperature 54-60aboutC, cooled to 49aboutC. the Condensate is pumped into the storage ACRE for reuse. Secondary ACRE is saturated with ammonia and plasmon carrying out the process in a continuous mode, but at a lower feed rate of a saturated solution of 1.35 m3/h, which is determined empirically, as most of the other parameters, and to establish continuous mode first oxides accumulate in the conical section of the reactor, and then only install (method selection) is required, the removal rate of the sludge.

The maximum productivity of the production flow in periodic mode 7.5 kg/m3about.h in continuous mode 11 kg/m3about.h [4]

The disadvantages of the method are not high performance process, the need for additional additional oxidation stage in a special apparatus in order to avoid the production of a product of variable composition, regulation of process parameters, mainly the method of selection when establishing a continuous mode, as well as receiving an inactive form of oxides.

In addition, the General disadvantages of the known methods is that each process intensifies any individual stage, and not all stages of the process in their relationship, as well as the inefficiency of the solution of the question of removing and disposing of waste solutions and gaseous reaction products, catego process stream due to the intensification of each stage and the overall process, providing opportunities for active oxides.

Another objective of the invention is to provide a waste-free environmentally friendly technology due to trapping gas emissions, the regeneration liquid effluent and re-use them in the process.

This goal is achieved by the fact that the method for obtaining basic carbonate salts of copper, zinc, Nickel and cobalt and their oxides, including the dissolution of metal-containing compound in an ammonium carbonate solution to obtain a saturated solution of Aminatou suitable metal, its preheating and feeding into the reactor for decomposition at elevated temperature followed by the formation of the target product, filtering, drying, condensation and return of gaseous products to the stage of dissolution, and as a metal-containing compounds use technical metal and/or an inactive oxide and/or hydroxide, and/or mixtures thereof, the dissolution is carried out at 55-58aboutC and a molar ratio of metal:ammonia: carbon dioxide 1: (1.5-to 3.5): 1 for copper and CEC and 1:(3,5-5,0):1 for Nickel and cobalt with obtaining solution Aminatou containing 1-3 mol of metal per 1 l of solution, preliminary heating of RA is,2-0,4 portions of reactor 1 h, and thermal decomposition of ammiakatov carried out at 92-99aboutTo obtain the specified product when prinuditelnom removing gaseous reaction products, thus increasing their pressure over a solution of 0.2-0.7 kPa and continuous three-five times the circulation of the solution in the reactor, and the circulation is carried out at a parallel unilateral upward flow of fluids and gases under continuous removal from the reactor of the finished product.

The method according to the invention compared with the known can improve the performance of process stream 3-4 times (up to 14000-27000 kg/day, against 3675-6750 kg/day have known for copper and zinc), mainly due to pre-heating to 100-150aboutWith a saturated solution of Aminatou under the pressure of 100-600 kPa; increasing the feed rate of the saturated solution in the reactor thermal decomposition to 0.2-0.4 relative volume of the reactor in 1 hour; the reaction of thermal decomposition of Aminatou in full of the principal of the solution in the reactor thermal decomposition, with a 92-as; three-five-circulation in a particular direction in the reactor core solution together with the formed reaction products; forced removal from the reaction

The method according to the invention differs from known helps to ensure continuity throughout the process, mainly due to the continuous circulation of the primary solution in the reactor thermal decomposition; the continuous removal from the reactor gas mixture.

Unlike well-known in the proposed method, the stage of dissolution and oxidation carried out simultaneously at elevated temperatures and different concentrations of metal ions and ammonium-carbonate solution, expressed through the correlation IU H3CO2with the formation of ions IU(II) and obtain a saturated solution of Aminatou that concentration that provides wide opportunities on raw materials used and the resulting products.

P R I m e R 1. Batch mode process. In the reactor, the solvent of 20 m3load (on the lattice) metallic copper, the reactor is filled to the "poor" copper-ammonium-carbonate solution having a temperature environment (but not more than 49aboutC) and usually containing, g/l: CuO 6, NH3160, CO2100, the molar ratio of NH3:CO2of 4.2:1. Solution with the aid of the circulating pump in the direction from top to bottom of the reactor with simultaneous produve Cu(I) and partly Cu(II). The necessary concentration of the solution is achieved by periodic recharge NH3and CO2and circulation of the solution, and air supply.

In the case of receiving only the oxide of copper (II) solution is pumped into a special container (aerator) for stabilization of the enriched solution, i.e., the transfer of cu(I) cu(II) by additional oxidation by oxygen. After which the solution is pumped into the storage saturated solution.

A new batch of "poor" copper-ammonium-carbonate solution is poured into the reactor with metallic copper and periodic process of dissolution, then oxidation ins of copper to obtain a saturated solution of Aminatou repeat.

Store prepared saturated solution containing Cu(II) 150-160 g/l, at a temperature of less than 54aboutC and a pressure of less than 100 kPa served in the evaporator (15 v m3with a speed of 30-40 l/min (0.07 to 0.12 fraction of the reactor volume) by spraying on the surface of the base solution. The main solution in the reactor typically has a composition, g/l: CuO 7; NH328; CO26 and a temperature of 103about(But not above 107aboutC). When a saturated solution of emmakate copper falls on the surface of the base solution, a chemical reaction occurs leading to the formation of the ACS is in the evaporator support by circulating part of the solution through the external heat exchanger, thus the multiplicity of the main circulation of the solution is 1.5 volume of the reactor in 1 hour

The resulting reaction NH3, CO2and H2O create over the surface of the solution overpressure 35-70 kPa, which is controlled by throttling through the valve. Gas-vapor mixture discharged from the reactor, cooled to 54aboutIn the first stage and to the 49aboutWith the second stage and the condensate re-use at the stage of dissolution of the metal. Nscontainerframe H2O, NH3and CO2sent for clearance into the tail scrubber (together with gases other stages).

After processing a given amount of solution equal to the working tank of the reactor, the exit of the evaporator. When this flow of saturated solution in the reactor is stopped, but the main circulation of the solution through the heat exchanger continue 1-1,5 h for more depletion NH3and CO2. Then the precipitated copper oxide udalaut from the evaporator together with the basic solution and the product is filtered. All operations periodic process is repeated. The duration of 24 h, the performance 4530 kg/day.

Similarly receive and zinc oxide. Only in this case, if the volume of the reactor per hour, the temperature of the basic solution in the reactor 101aboutC. the duration of the process is also 24 hours, performance, 3675 kg/day.

P R I m m e R 2 (prototype). Continuous process. In the reactor, the solvent on the grid loads metallic copper in an amount to provide continuous operation for several days. Continuously into the reactor an air and copper - ammonium-carbonate solution with a speed of 1.5 m3/h (0,075 fraction of the reactor volume in 1 h). The dissolution of metallic raw materials, saturation ACRE metal ions, oxidation, obtaining saturated solution of Aminatou carried out as in example 1. A saturated solution concentration, temperature and pressure, similar to example 1, serves on the stage of thermal decomposition only with a lower speed of 1.35 m3/h (0,068-0,075 of the relative volume of the reactor 1 h), other conditions of thermal decomposition is identical to example 1. Continuous mode provides the feed rate of the saturated solution and the speed of removal of the finished product, the value of which is determined empirically, i.e., to establish a continuous process first oxides accumulate in the conical section of the reactor and depending on the rate of formation googamooga ammonia and carbon dioxide. Drainage and condensation ASG meets the standards of the technological process of example 1.

When creating conditions for continuous process limiting stage is the stage of dissolution of metals (the residence time of the solution in the reactor 10-13 h), so in this case use the extra capacity of the storage saturated solution. Basically the process parameters determined empirically. The performance of the process 4600-6750 kg/day.

P R I m e R 3. In the reactor, the solvent load on the grid technical metallic copper and/or inactive oxide and/or hydroxide of copper. Download the original raw material is produced continuously or periodically. At the same time in the reactor is poured a solution containing, g/l: CuO 6-10; NH3140-160; CO2190-240, which circulates through a solid phase in the upward direction. The multiplicity of circulation is equal to 5 (the capacity of the pump 100 m3/h). Part of the solution in circulation passes the heat exchanger, which allows to maintain the temperature of 80aboutWith, the other part of the solution passes a hollow scrubber, which serves the air for oxidation of Cu(I) Cu(II). Thus, one pump operate, heating the solution, its oxidation and transportation , and stage of condensation, with the expectation that in the reactor, the molar ratio of metal: ammonia: carbon dioxide was set to 1, a 3.5:1. The high content of carbon dioxide in solution allows you to link all the ammonia in the chemical compound with carbon dioxide (ammirati), which reduces its losses and costs for cleaning waste. The increase in the temperature of dissolution reduces the energy consumption for the further heating of the solution and use the heat of reaction of dissolution, as well as to increase the rate of formation of Aminatou 2-4 times.

A saturated solution of Aminatou divalent copper containing Cu(II) 2,35 mol/l (150 g/l) pump with a pressure of 600 kPa continuously served in the external heat exchanger where it is heated from 80 to 150aboutC. Heating the solution under pressure prevents uncontrolled decomposition of Aminatou in the heat exchanger and simultaneously increases the supply of heat to the stage of thermal decomposition of Aminatou. Then a saturated solution with the speed 0,34 fraction of the reactor volume (vpin 1 h fed into the reactor thermal decomposition.

The main solution in the decomposition reactor and having a temperature of 99aboutWith continuously circulate in the upward direction with the help of a remote pump and teploobmenu from solution under the action of temperature and continuous forced ventilation to remove gaseous products of reaction of NH3, CO2H2O providing pressure over a solution of 0.7 kPa. Gas-vapor mixture (ASG) is directed to condensation and cooled to 45aboutWith, the result is an ammonium carbonate solution containing, g/l: NH3140-160; CO2190-240, which is then sent to the stage of dissolution of oxidation.

Forced removal of ASG and its cooling can increase the rate of decomposition of Aminatou by 20-40% and return on stage dissolution (bypassing the stage of recovery NH3) about 40-60% of the original solution.

At the same time to exit the calibration gas from the reactor thermal decomposition enter the estimated number of NH3and CO2to compensate for their losses and intensification of the process of decomposition of Aminatou, by linking NH3, CO2and H2O in a solution of carbonate and ammonium bicarbonate, increasing the pressure in the system and reduce losses for gas cleaning, pumping, etc.

The air from the stage of dissolution-oxidation and the remaining gases after condensation clear in the absorber water, which are also directed to the stage of dissolution. Thus carry out the recycling in the scheme of the excess water, ammonia and carbon dioxide, which stabilize the operation of all stages of the process.

The performance of process stream sostavljaet 22760 kg/day.

Technological scheme has automated control and regulation of process parameters and material flows, adjusted for continuity and isolation of the process stream.

P R I m e R 4. All operations and stages of technological process carried out as in example 3, with the difference that in the reactor download technical metallic zinc and/or inactive oxide and/or zinc hydroxide, the solution at the stage of dissolution-oxidation has a temperature of 83aboutAnd the molar ratio of Zn: NH3:CO21:1,5:1; a saturated solution with a concentration of zinc of 3.0 mol/l (191 g/l), temperature 145aboutC and a pressure of 500 kPa is served with rate 0,23 about. share vp/h in the reactor thermal decomposition, where the basic solution having a temperature of 99aboutWith, circulate with multiplicity 5, and the gas-vapor mixture removed from the reactor, providing a pressure above a solution of 0.4 kPa, and then condense, cooling to 47aboutC.

Get active zinc oxide having a specific surface 18-28 m2/g; flow performance 23600 kg/day.

P R I m e R 5. All operations and stages of technological process the ski or carbonyl), the solution at the stage of dissolution-oxidation temperature is 85aboutAnd the molar ratio of Ni:NH3:CO21: 5,0: 1; a saturated solution with a concentration of Ni(II) 1.5 mol/l (88 g/l), temperature 140aboutC and a pressure of 450 kPa served with speed 0,20 about the share of vp/h in the reactor thermal decomposition, where the basic solution having a temperature of 98aboutWith, circulate with multiplicity 5, and the gas-vapor mixture removed from the reactor, providing a pressure above a solution of 0.5 kPa, and then condense, cooling to 48aboutC.

Get active Nickel oxide having a specific surface area of 18-22 m2/g, the flow capacity is 11330 kg/day.

P R I m e R 6. All operations and stages of technological process carried out as in example 3, with the difference that was charged to the reactor technical metal cobalt and/or inactive cobalt oxide, the solution at the stage of dissolution-oxidation has a temperature of 55aboutAnd the molar ratio of Co:NH3: CO21:4,5:1; a saturated solution with the concentration of Co(II) 1.0 mol/l (60 g/l), temperature 135aboutC and a pressure of 420 kPa served with speed 0,23 about. share vp/h in the reactor thermal decomposition, where the basic solution having a temperature of 98aboutWith, cirsten condense, cooling to 48aboutC.

Get active cobalt oxide having a specific surface 17-24 m2/g, the performance of the process stream is 6800 kg/day.

P R I m e R 7. All operations and stages of technological process carried out as in example 3, but with the difference that the loading of the feedstock in the reactor, the stage of dissolution and oxidation of metal ions with getting saturated solution of Aminatou copper and saturated solution of Aminatou zinc carried out separately in example 3 and 4, respectively. Thus the solution at the stage of dissolution-oxidation has a molar ratio of Cu:NH3:CO31:3,5:1 and Zn:NH3:CO21:2,5:1, respectively; the concentration of the saturated solution (copper and zinc) is 2.1 mol/l (135 g/l).

Then streams of saturated solutions of Aminatou copper and zinc combine together (in automatic mode or, if necessary, manual control) in the intermediate reservoir and fed to the inlet of the heat exchanger. Then heated under pressure and the flow in the reactor thermal decomposition of a mixture of saturated solution of Aminatou copper and zinc exercise, as in example 3 except that a solution having a temperature of 147aboutC and a pressure of 250 ciruit with multiplicity 4,5, and gas-vapor mixture removed from the reactor, providing a pressure above a solution of 0.2 kPa, and then condense, cooling to 47aboutC.

Get active oxides of copper and zinc; the performance of the process stream is 26800 kg/day.

P R I m e R 8. All operations and stages of technological process carried out as in example 3, but with the difference that the solution at the stage of dissolution-oxidation temperature is 65aboutAnd the molar ratio of Cu:NH3:CO21:3,0:1, saturated solution with a concentration of Cu(II) 1.5 mol/l (95 g/l), temperature 125aboutC and a pressure of 350 kPa served with speed 0,40 about. share vp/h in the reactor thermal decomposition, where the basic solution having a temperature of 92aboutWith, circulate with a ratio of 3.8, and gas-vapor mixture removed from the reactor, providing a pressure above a solution of 0.3 kPa, and then condense, cooling to 46aboutC.

Get a basic carbonate of copper; the performance of the process stream is 17300 kg/day.

P R I m e R 9. All operations and stages of technological process carried out as in example 3, with the difference that was charged to the reactor feedstock and hold stage dissolution-oxidation, maintaining the temperature is s zinc Zn ion concentration of 2.0 mol/l (130 g/l), temperature 125aboutC, a pressure of 350 kPa and a speed of 0.20. share vp/h fed into the reactor thermal decomposition, where the basic solution having a temperature of 94aboutWith, circulate with a ratio of 3.7, and gas-vapor mixture removed from the reactor at a pressure above a solution of 0.6 kPa and then condense, cooling to 48aboutC.

Get a basic zinc carbonate; the performance of the process stream is 19560 kg/day.

P R I m e R 10. All operations and stages of technological process carried out as in example 3, with the difference that was charged to the reactor feedstock, conduct stage dissolution-oxidation and receive a saturated solution of Aminatou Nickel in example 5, which then temperature 125aboutC, a pressure of 350 kPa and a speed of 0.28 about. share vp/h fed into the reactor thermal decomposition, where the basic solution having a temperature of 93aboutWith, circulate with a ratio of 3.6, and gas-vapor mixture removed from the reactor at a pressure above a solution of 0.5 kPa and then condense, cooling to the 49aboutC.

Get the basic Nickel carbonate; the performance of the process stream is 14260 kg/day.

P R I m e R 11. All operations and technological stage is the dissolution-oxidation when the temperature of the solution 75aboutWith and get a saturated solution of Aminatou cobalt ions Co(II) in example 6, and then temperature 125aboutC and a pressure of 350 kPa saturated solution of Aminatou cobalt served with speed 0,30 about. share vp/h in the reactor thermal decomposition, where the basic solution having a temperature of 92aboutWith, circulate with a ratio of 3.5; gas-vapor mixture removed from the reactor at a pressure above a solution of 0.6 kPa and then condense, cooling to 48aboutC.

Get a basic carbonate of cobalt; the performance of the process stream is 10640 kg/day.

P R I m e R 12. All operations and stages of technological process carried out as in example 3, but with the difference that was charged to the reactor feedstock exhaust catalyst mass ratio of CuO:ZnO:Al2O335:30: 35, the solution at the stage of dissolution-oxidation has a temperature of 75aboutAnd the molar ratio Me:NH3:CO21:3,0:1; a saturated solution with a concentration of metal ions 2.32 mol/l (150 g/l) temperature 125aboutC and a pressure of 300 kPa is served with rate 0,20 about. share vp/h in the reactor thermal decomposition, where the basic solution having a temperature of 93aboutWith that circulate with kratnost is, cooling to 50aboutC.

Get a mixture of basic carbonates of copper and zinc and the active alumina; the performance of process stream 24600 kg/day.

P R I m e p 13. All operations and stages of technological process carried out as in example 3, but with the difference that the loading of the feedstock in the reactor, the stage of dissolution and oxidation of metal ions with getting saturated solutions of Aminatou Nickel and cobalt are conducted separately in examples 5 and 6, and the temperature of the solution at the stage of dissolution 85aboutWith 55aboutWith, respectively, a molar ratio of Me:NH3:CO21:3,5:1 (with a ratio of Ni:Co 4: 1; then streams saturated solutions of Aminatou Nickel and cobalt together (example 7 and fed into the reactor for the decomposition speed of 0.28 about. share vp/h under 100aboutC, a pressure of 100 kPa with a concentration of 1.5 mol/l (130 g/l); the temperature of the basic solution in the reactor is 92aboutWith the multiplicity of its circulation 4,0; gas-vapor mixture removed from the reactor, providing a pressure above a solution of 0.7 kPa, and then the calibration gas condensate, cooling to 50aboutC.

Get a mixture of basic carbonates of Nickel and cobalt (with a ratio of Ni: Co4:1); productive the specific examples of the method are summarized in table.

In the proposed method, the ratio of metal: ammonia: carbon dioxide with a high content of CO2compared with a similar ratio in a known way, you can associate the greatest amount of ammonia in the chemical compound, thereby to optimize the process, to reduce ammonia losses and costs for cleaning waste.

Set temperature at the stage of dissolution-oxidation govern (except exchanger) introducing a fresh source of solution and removal of the saturated solution in order to ensure continuity of the process. Lowering the solution temperature (below 55aboutC) reduce the dissolution rate and increase (above 85about) to the decomposition of the formed ammiano, i.e., to reverse the process.

Insufficient concentration of the saturated solution (below 1 mole per 1 liter of solution) and a lower rate of feed to the reactor decay (less than 0.2 fraction of reactor volume in 1 h) leads to a significant decrease in the performance of the process; however, when the solution concentration above 3 mol/l increased the content of the finished product in the solution, which makes its removal from the reactor; the feed rate of solution in the reactor above logicnet process.

Limit values of the temperature and pressure of saturated solution at the inlet of the reactor for the decomposition is the boundary of existence of a saturated solution of Aminatou in predetermined concentrations in optimum condition and prevent its premature decomposition.

Three to five times the circulation of the solution in the reactor decay per hour at the specified temperature 92-99aboutWith intensified reaction in the whole volume of the reactor, which greatly increases the efficiency of the process, and also contributes to the reduction and to improve the dispersibility of the finished product. The circulation of the solution below the specified limit leads to subsidence and compaction of the finished product, and above the limit inefficient and inappropriate.

The pressure of the gas mixture above the solution in the range of 0.2-0.7 kPa regulates the necessary and sufficient amount of gaseous reaction products, thereby enables to shift thermodynamic equilibrium towards formation of the desired products.

Thus, known methods, typically performs one specific task, comprehensive solution to the problem does not give any of the currently existing methods.

Offer itbrain technology for a wide range of products, at the same time (if necessary) easy to move production from one type of finished product to another on units with serial equipment; get connection controlled, with a given ratio of active components (active oxide, basic carbonate salts, and mixtures thereof) optimal particle size and density, does not contain harmful impurities, i.e., meets the essential requirements of raw materials for the production of catalysts and absorbents, used for production of not only metals, and oxides, hydroxides or mixtures thereof, up to the use of waste, for example, spent catalysts; to create waste-free environmentally friendly production.

The METHOD of OBTAINING BASIC CARBONATE SALTS of COPPER, ZINC, NICKEL AND COBALT AND THEIR OXIDES, including the dissolution of metal-containing compound in an ammonium carbonate solution to obtain a saturated solution of Aminatou suitable metal, its preheating and feeding into the reactor for decomposition at elevated temperature followed by the formation of the target product, filtering, drying, condensation and return of the gaseous products at the stage of dissolution, ATI continuous process stream, as metal-containing compounds use technical metal and/or an inactive oxide and/or hydroxide and/or mixtures thereof, the dissolution is carried out at 55 85oC and a molar ratio of metal ammonia: carbon dioxide 1 1,5 3,5 1 for copper and zinc and 1 3,5 5,0 1 for Nickel and cobalt with obtaining solution Aminatou containing 1 to 3 mol of metal per 1 l of solution, preliminary heating of the solution is carried out at 100 to 150oC and a pressure of 100 to 600 HPa, the flow of the heated solution is produced at a rate of 0.2 to 0.4 fraction of reactor volume in 1 h, and thermal decomposition of Aminatou carried out at 92 99oTo obtain the desired product if you force the removal of gaseous reaction products, thus increasing their pressure over a solution of 0.2 0.7 kPa, and continuous 3 - 5 times the circulation of the solution in the reactor, and the circulation is carried out at a parallel unilateral upward flow of fluids and gases under continuous removal from the reactor product.

 

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