Method and device for the production of gallium from waste semiconductor gallium phosphide |
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IPC classes for russian patent Method and device for the production of gallium from waste semiconductor gallium phosphide (RU 2226563):
 Furnace for refining magnesium / 2222623
The invention relates to metallurgy, in particular to the furnaces for refining magnesium
 Melting and casting device for producing small castings / 2211419
The invention relates to foundry and can be used for small castings of high-level radioactive metals and alloys, particularly dentures and jewelry
 Laboratory oven for optical research / 2202747
 The device for preparation and analysis of samples of liquid alloys / 2174207
The invention relates to metallurgy, and is intended for receipt and analysis of samples of liquid alloys in the laboratory of metallurgical processes on the surface of the alloy and may find application in research laboratories
 The method and apparatus of the infiltration of gas phase chemical substances and chemical vapor deposition (options), the product obtained in this way, the feeder of the first of a reagent gas into the furnace for infiltration and deposition from the gas phase and the friction disk / 2173354
The invention relates to high-temperature composite materials obtained by the infiltration of gas phase chemical substances and deposition of matrix binder material in the porous structure of the
 The setup for studying objects at high temperatures / 2149330
The invention relates to test equipment and can be used to test objects containing explosives and toxic substances, at different heat exposure, including fires
 Installation of a wet-type flue gas desulfurization and the usage of solid substances obeserver / 2140809
The invention relates to an apparatus and method of the wet-type desulfurization of flue gases, and in particular, to the installation of a wet-type desulfurization of flue gases and to a method of use of solid obeserver substances for economical removal of oxides of sulfur in the combustion gases leaving the combustion equipment such as boilers, with high quality desulfurization, less abrasion of the pump for circulating the absorbing fluid and a nozzle for spraying a smaller deterioration in the quality of the product because of the aluminum and fluorine components in the absorbing fluid, reduced capacity for crushing hard obestsenivaya substances such as limestone, and excellent handling on changes in the amount of exhaust gas or the concentration of SO2
 The method of regulation of heat removal from the surface of the heat exchanger with external fins / 2133424
The invention relates to heat engineering, in particular to a method of regulating heat removal from the surface of the heat exchanger with external fins, and can be used in non-ferrous metallurgy, more specifically, when the cooling of gases formed during roasting zinc concentrate
A method of processing copper-containing waste / 2226559
The invention relates to integrated processing copper-containing waste to produce a number of commercial products
A method of processing slag from steel production / 2226220
The invention relates to a method for processing slag from steel production and, in particular, iron-containing materials, such as furnace slag, BOF slag, dust from steel production, scale rolling mills or waste-ferrous secondary metals, in which the molten slag from steel production, respectively, iron-containing material is mixed with chrome ores or chromium - and Nickel-containing the dusts to establish the slag basicity of 1.2-1.6, and the temperature of the bath is supported above 1600
 With, mainly in the range of 1600-1800With, and introducing carbon-containing a bath of liquid iron or form it
 The output of sulfate ions from solutions of zinc production / 2224035
The invention relates to the field of hydrometallurgical zinc production, in particular to the purification of solutions of soluble sulfates of magnesium and alkali metals, and also to neutralize the excess sulfuric acid in the balance zinc production
 The method of processing waste from electrolytic refining of aluminium / 2222642
The invention relates to ferrous metallurgy and can be used for processing of anode sludge formed during electrolytic refining of aluminum
A method of processing metallurgical slag dump / 2222619
The invention relates to metallurgy, specifically to the technology of processing of metallurgical slag dump, mainly electrometallurgical production, and can be used to extract magnetic, weakly magnetic and non-magnetic components from these materials
 A method of processing a nickel-cadmium scrap / 2222618
The invention relates to the processing of raw materials, in addition to ores, e.g. scrap, to produce ferrous metals or their compounds, in particular, from spent Nickel-cadmium batteries
 Method of recycling waste cardboard packaging for liquid and device for its implementation / 2222617
The invention relates to the recycling of waste from packaging for liquid or other wastes containing fibrous material, metal and plastic
 A method of obtaining a chloride of lead / 2222494
The invention relates to a technology for lead compounds, namely a process for the production of lead salts, particularly chloride of lead
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The invention relates to the technology of waste processing semiconductor of gallium phosphide to extract expensive and scarce gallium. Method for the production of gallium from waste semiconductor gallium phosphide includes vacuumforming decomposition when heated in a graphite crucible at a temperature of 1050-1200 With at a residual pressure of 0.133-6,666 PA (1 10-3-510-2mm RT.CT.) separating the formed phosphorus from gallium in the zone of decomposition by condensation of vapors of phosphorus in the condenser with subsequent oxidation to the phosphate anhydride and dissolving it in water. The method is carried out using a device which includes a heater, a quartz reactor, graphite crucible, located in the reactor, the vacuum system, metallic water-cooled condenser, a supply of oxygen and inert gas. The input pipe of the vacuum system is located after the condenser and the inlet of the oxygen - before the condenser. The method and the device allow to increase the degree of extraction of gallium from waste semiconductor gallium phosphide and reduce waste. 2 S. p. f-crystals, 1 Il., 1 tab is th AndIIIBVin particular, the semiconductor gallium phosphide and may be used in the electronic industry, ferrous metallurgy and other industries engaged in the processing kalisoderjasimi raw materials.
The known method (22 IN 58/00, 30/04, 7/00, EN 2078842, publ. 10.05.97, ed. The Abryutin C. N., Kalashnik O. N.), whereby obtaining gallium from waste gallium arsenide spend vakuumtechnik decomposition at a temperature of 1100-1250With residual pressure n(10-1-10-2) mm RT.article.
The main disadvantage of this method is the low degree of extraction of gallium and increased energy consumption, due to the high process temperature 1100-1250With (at temperatures above 1200With begins to significantly evaporate gallium from the zone of decomposition) and not deep enough vacuum. It is known that for decomposing compounds, such as gallium phosphide (GaP), gallium arsenide GaAs, indium arsenide InAs, speed and completeness of dissociation depends on the residual pressure in the zone of decomposition, and the it is less, the greater the speed and completeness of dissociation.
The closest to the technical nature of the claimed object is a method (22, 7/00, 6126 US countermine decomposition when heated at a temperature 1250-1475And a residual pressure of 10-5-10-1mm RT.article in a graphite crucible, with the separation of the formed phosphorus from gallium in the zone of decomposition by condensation of vapors of phosphorus in the condenser, its oxidation and dissolution, and the oxidation is conducted in an aqueous solution of transition metal salt, for example, an aqueous solution of copper sulfate.
A device that is closest to the technical nature of the claimed (From 22 In 7/00, US 6126719 And, publ. 03.10.2000), including a heater, a quartz reactor, graphite crucible, located in the reactor, the vacuum system and water-cooled condenser. The reactor is connected with a water-cooled condenser and vacuum system piping.
The main disadvantage of this method and device is the low degree of extraction of gallium and the formation of large quantities of waste.
When vacuumforming decomposition, which is carried out at a temperature 1250-1475With significant evaporation of gallium from the zone of decomposition, as is already at a temperature 1329With the vapor pressure of gallium above its melt is 110-3at (Ivanov P. C. Chemistry and technology of gallium. - M.: metallurgy, 1973, c.327).
The use of large amounts of liquid (a mixture of aqueous solutions of oxidizing agent and reaction products) and solid (a mixture of recovered metal remains unreacted oxidant and reaction products) waste.
The technical result of the present invention to provide a gallium from waste semiconductor of gallium phosphide GaP with a higher degree of extraction of gallium and reducing waste.
Technical result provided by the invention, is achieved by the production method of gallium from waste semiconductor of gallium phosphide GaP, including vacuumforming decomposition when heated at a residual pressure of 0.133-6,666 PA (110-3-510-2mm RT.CT.) in a graphite crucible, with the separation of the formed phosphorus from gallium in the zone of decomposition by condensation of vapors of phosphorus in the condenser, its oxidation and dissolution, vacuumforming decomposition of gallium phosphide is carried out at a temperature of 1050-1200With the oxidation of phosphorus are oxygen with obtaining phosphoric anhydride, which is directed to dissolution in water, as well as a device that includes a heater, a quartz reactor, graphite crucible, located in the reactor, the vacuum system, metallic water-cooled condenser, and provided with a supply line of oxygen, while the inlet of the vacuum system is located after the condenser, and whooga phosphide with a higher degree of extraction is achieved by preventing the evaporation of the formed gallium in vacuumforming decomposition of gallium phosphide. This is possible due to the fact that vacuumforming decomposition is carried out at a temperature of 1050-1200C. At this temperature, almost no evaporation of gallium from the zone of decomposition. In the method-prototype process vacuumforming decomposition is carried out at a temperature 1250-1475C. thus there is significant evaporation of gallium from the zone of decomposition and subsequent condensation in the colder parts of the device, for example, piping or capacitor. The condensate, which represents a two-phase mixture of gallium phosphide and gallium (gallium phosphide can be formed due to the inverse interaction vapor gallium and phosphorus) entering the pipeline, can serve as centres of further condensation of gallium phosphide and gallium. This can lead to a complete overlap of the inner section of the pipeline, a sharp increase in pressure in the zone of decomposition and termination process vacuumforming decomposition, which also will reduce the degree of extraction of gallium.
This is possible due to the fact that the device is provided with a supply line of oxygen in the condenser, so that the inlet of the vacuum system is located after the condenser, and inlet pipe pomacle, make a pair of phosphorus released during vacuumforming decomposition, was condensed in the condenser, and into the vacuum system. The pipe line supplying oxygen is in front of the condenser, therefore, formed by the oxidation of a pair of phosphoric anhydride R2About5will be carried by the gas stream in the absorber, without contaminating the other reaction product is gallium.
The oxidation of phosphorus in the method prototype is conducted in an aqueous solution of a salt of the transition metal, such as copper sulfate. When this occurs, the oxidation of phosphorus, translate it into a solution and restore the cation of the metal to the metallic state. The authors propose to use the resulting solution as fertilizer or be subjected to recycling. Use in the form of fertilizers involves more operations on the separation of the recovered metal from the solution and separation from a solution of excess oxidant source. For recycling the resulting solution also requires additional operations and reagents, for example, to neutralize or translated into poorly soluble compounds.
In the inventive method, the oxidation of phosphorus spend oxygen with the formation of phosphoric anhydride R2About53RHO4that is a commercial product without the use of additional operations, for example, in the chemical industry, thus the process is waste-free.
Experimentally it is found that the rate of the process vacuumforming decomposition of gallium phosphide at temperatures below 1050Insufficient to complete the process. At temperatures above 1200With the evaporation of gallium from the zone of decomposition, which reduces the degree of extraction.
At a residual pressure of less of 0.133 PA evaporation of gallium from the zone of decomposition, which also leads to a decrease in the degree of extraction. At a residual pressure of more 6,666 PA decomposition process is very slow, which requires additional energy consumption.
The inventive method was implemented in the device shown in the drawing.
The device consists of a graphite crucible 1, which is located in a quartz reactor 2, a heater 3, a water-cooled condenser 4 is connected to the quartz reactor 2, the vacuum system 5-9, the inlet of which is located after the water-cooled condenser, a supply of oxygen, which is carried out with the help of the Institute of filling the inner space with an inert gas to the valve 10, the absorber 13, the water pump 14 and cameras completeness absorption 15.
The device operates as follows. Due to the vacuum system 5-9 device, the entrance of which is located immediately after the condenser 4, thermal decomposition of lead in a dynamic vacuum. Gaseous oxygen is supplied by means of the valve 12, which is located in front of the condenser, for the oxidation of phosphorus after completion of the process vacuumforming decomposition and condensation of phosphorus in the condenser 4. The product of oxidation of the phosphorus enters the absorber 13, where it is catching water with the formation of phosphoric acid. A specific example of this method in a device for its implementation can serve as obtaining gallium from waste semiconductor gallium phosphide.
The process is carried out as follows. Weigh the waste phosphide 5,0 kg, load them into the graphite crucible 1, placed in a quartz reactor 2 in the heater 3. Make the connection of the quartz reactor 3 with the water cooled condenser 4 through the vacuum seal 5. Then to the output flange of the condenser through the vacuum seal 6 attach the piping of the vacuum system, vklyuchayushchei vacuum pump 7, open the valve 9 and the internal volume of the pump device to a residual pressure of 0.133 PA (110-3mm RT.cent.), which is controlled by a vacuum gauge 8. Serves the power supply to the heater 3 and produce its heating to a temperature of 1050C. the Process vacuumforming decomposition is carried out in four hours. After this time produce off power of the heater. After cooling of the heater to a temperature of 40-60To close the valve 9, disable mechanical vacuum pump 7. The internal volume of the device is filled with an inert gas, e.g. nitrogen to atmospheric pressure through valve 10, then the valve 10 is closed. Open the gates 11 and 12 and begin the process of oxidation (combustion) of phosphorus is condensed in a water cooled condenser 4 oxygen. The resulting phosphoric anhydride R2About5the gas stream is transferred to the absorber 13, where it is the absorption of water with the formation of orthophosphoric acid, H3RHO4. The absorber 13 is supplied by a pump 14 for circulating the absorbent - water and camera control of the completeness of absorption 15. After arancaytar 4 from the quartz reactor 2, revealing vacuum seal 5 and 6, and remove the graphite crucible 1 made of quartz reactor 2, unloaded from him obtained gallium, weigh and determine the degree of extraction of gallium, which is 99,60 wt.%. Other examples on the boundary limits of technological modes of the proposed method are presented in the table.
From the table it follows that the inventive method and device allow to obtain gallium with a high degree of extraction from waste semiconductor gallium phosphide.
Claims 1. Method for production of gallium from waste semiconductor of gallium phosphide GaP, including the vacuum-thermal decomposition when heated at a residual pressure of 0.133-6,666 PA (110-3-510-2mm RT.CT.) in a graphite crucible, with the separation of the formed phosphorus from gallium in the zone of decomposition by condensation of vapors of phosphorus in the condenser, its oxidation and dissolution, characterized in that the vacuum-thermal decomposition of gallium phosphide is carried out at a temperature of 1050-1200With the oxidation of phosphorus are oxygen with obtaining phosphoric anhydride, which direct the containing heater, quartz reactor, graphite crucible, located in the reactor with a vacuum system, metallic water-cooled condenser, characterized in that it is provided with a line feed oxygen inlet pipe of the vacuum system is located after the condenser, and inlet pipe line supplying oxygen - before metal capacitor.
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