A method of producing metals and other elements

 

(57) Abstract:

The invention relates to metallurgy, in particular to a method for the element or metal, or alloy of halide, or mixtures thereof. The halide or mixtures thereof in contact with the stream of liquid alkali or alkaline earth metal, or mixtures thereof in a quantity sufficient to convert the halide in the nonmetal or metal or alloy and to maintain the temperature of the reactants at a temperature below the lower boiling point of the alkali or alkaline earth metal at atmospheric pressure, or temperature sintering of the obtained non-metal, or metal, or alloy. How, in particular, is applicable to the receipt of titanium. The invention enables to provide a continuous method and create a recirculation system reductant. 4 C. and 9 C.p. f-crystals, 1 table, 4 Il.

The invention relates to the production of basic material from his halides and is particularly suitable for such metals and non-metals, for which recovery of the halide to the item is exothermic.

Of particular interest in this regard is titanium, and the present invention will be described with specific reference to titanium, but it is cachestoreprivate of the halide with the release of considerable heat. For the purposes of this application the elementary materials include metals and non-metals listed above or in the table.

Currently obtaining titanium is carried out by reduction of titanium tetrachloride, which is obtained by chlorination of relatively high-grade ore of titanium dioxide. To obtain a satisfactory chlorination of source material can be physically concentrate rotrstenai ore; other sources of titanium dioxide, such as ilmenite, titanium containing iron ore and most other materials, which is the source of titanium, require chemical enrichment.

Attempts were made in the reduction of titanium tetrachloride to metal using a variety of reducing agents, including hydrogen, carbon, sodium, calcium, aluminum and magnesium. It was proved that the recovery of the magnesium titanium tetrachloride may serve as a commercial method of producing titanium in the form of metal. However, the implementation of periodic process requires considerable manipulation of the material, this creates opportunities for contamination and changes from boot to boot. The biggest opportunity to reduce AI manipulation of material. There is a great need to create a method which allows for continuous economical production of titanium powder, suitable for use without further processing by powder metallurgy or by vacuum arc melting to form an ingot. Today, there are two commercial method of producing titanium, which are the way of Kroll and the way of the hunter.

In accordance with the method of Kroll titanium tetrachloride chemically restore magnesium at a temperature of 1000oC. the process is carried out in periodic mode in a metal retort in an inert atmosphere or helium, or argon. To obtain molten bath of magnesium magnesium is loaded into the vessel and heated. Over a bath of molten magnesium at room temperature dropwise dispersed liquid titanium tetrachloride. In the gas zone above the bath of molten magnesium liquid titanium tetrachloride evaporates. There is a superficial reaction with the formation of titanium and magnesium chloride. The way hunter is similar to the way Kroll, but for the reduction of titanium tetrachloride to metallic titanium and receiving sodium chloride instead of using magnesium sodium.

anyone titanium. Titanium is melted into the mass, which wraps the part of the molten magnesium chloride (or sodium). This molten mass is called titanium sponge. After cooling, the metal retort hardened titanium sponge metal is broken, crushed, cleaned and then dried in a stream of hot nitrogen. The titanium powder is usually produced by grinding, bead blasting, casting or by means of centrifugation. The usual technique consists in the initial absorption of hydrogen titanium for making titanium sponge brittle and further facilitate the grinding process. After the formation of a powder of titanium hydride particles digitalout and get a usable product. Processing of titanium sponge into a usable form is a complex process that requires a lot of work and two to three times increases the cost of the product.

During the processing stages, some particles of the sponge, such large, as for example, particles having a size of several centimeters, may ignite in air and as a consequence turn into oxynitride titanium, which during the melting process is usually not destroyed. The obtained inclusion of solid material in the part of shotley, which leads to the breakdown of aircraft.

The methods described above have several significant disadvantages, which largely contribute to the high cost of products made from titanium. Production of titanium periodic way integral requires large capital and labor. To obtain titanium in the form of ready to use titanium sponge must be subject to significant additional processing, which leads to increased cost, increased risk for workers and the increasing difficulties in quality control download. None of the methods do not use large energy exothermic reaction, although for the production of titanium requires significant energy costs (approximately 6 kWh/kg of the obtained metal). In addition, these methods have a significant amount of waste, which cause concern for the environment.

The invention

Accordingly, an object of the present invention is the provision of a continuous method and system for the production of non-metals or metals, or their alloys, which have significant advantages in terms of capital is Otsego invention is the provision of a method and system for the production of metals and nonmetals by exothermic recovery halide in preventing sintering of metal or non-metal on the device, used to receive them.

Another objective of the invention is the provision of a method and system for the production of non-metal or metal from their halides, where the method and system recycle reducing agent, resulting in essentially decreases the impact of the process on the environment.

The invention consists of specific novel features and combinations of parts, hereinafter described in detail and illustrated in the accompanying charteroak and features shown in the attached claims, it should be understood that the details without deviating from the essence or without damaging the advantages of the present invention can be made various changes.

Brief description of drawings

To facilitate understanding of the invention in the accompanying drawings is illustrated his preferred option, after studying which together with the subsequent description of the invention, its construction and action and many advantages will be readily understood and appreciated.

Fig. 1 is a process flow diagram showing as an example a continuous method of producing metallic titanium from titanium tetrachloride.

oC.

Fig. 3 represents the energy balance for the way in which the reagents out of the combustion chamber at a temperature of about 850oC.

Fig. 4 is a schematic representation of the method of Kroll or hunter, which are methods of the prior art in this field.

Detailed description of the invention.

The method of the invention can be implemented using any alkali or alkaline earth metal, depending on the type of recoverable transition metal. In some cases, there may be used a combination of alkaline or alkaline earth metals. In addition, in the present invention can be used any halide or combination of halides, although in most cases it is preferable chloride, being the cheapest and most readily available. As an example, not to limit, but only for the purpose of illustration, of an alkaline or alkaline earth metals may be selected from sodium, because it is the cheapest and most preferred, with the same purpose and choose chloride.

In respect of recoverable non-metals or metals should be noted that you can reset the same to obtain an alloy of a given composition by providing a mixed metal halides, taken in the desired molecular ratio in the beginning of the process. The purpose of the example in the table presents the heat of reaction for g sodium for recovery of non-metal halides or metal, applicable to the method of the invention.

The method will be illustrated again for the purpose of illustration, and not limitation, using a metal titanium tetrachloride obtained from.

In Fig. 1 shows a flow chart of the process in General. In the reaction the combustion chamber 10, where the current flow of sodium from its source (not shown) Inuktitut pair of titanium tetrachloride from its source in the form of distillation column 11, mixed sodium and titanium tetrachloride. In the electrolytic cell 12 receives the sodium. The reduction is strongly exothermic, the formation of molten reaction products of titanium and sodium chloride. The molten reaction products cooled rapidly in the flow of sodium. The particle size and reaction rate adjust by measuring the rate of flow of vapors of titanium tetrachloride, dilute vapors of titanium tetrachloride with an inert gas such as He or Ar, measurements of the flow of sodium and mixing parameters; where the combustion chamber includes concentrates the liquid, and the resulting temperature, which is basically influenced by the heat of reaction can be adjusted by using sodium and maintain it below the sintering temperature of the obtained metal, such as titanium, or at a temperature of approximately 1000oC.

Flow volume of sodium contains in this case, the reaction products, titanium and sodium chloride. These reaction products are removed from the flow of sodium through conventional separators 13 and 14, such as cyclones or filters in the form of particles. There are two separate options for the separation of titanium and sodium chloride.

The first option involves removal of the products of titanium and sodium chloride in the individual stages. Specified shall be implemented by maintaining the temperature of the flow such that the titanium was solid, and sodium chloride is molten, which can be performed by adjusting the ratio of flow rates of titanium tetrachloride and sodium in the combustion chamber 10. In this embodiment, first remove the titanium, then the volume flow is cooled for solidification of sodium chloride and then sodium chloride is removed from the separator 14. In this embodiment, the heat process for distillation of titanium tetrachloride is removed from the flow immediately after the separator titanium 13.

is skoe the ratio of the flow rate of titanium tetrachloride to the flow rate of sodium for so the temperature of the volume of sodium remained below the temperature of solidification of sodium chloride. In this embodiment, titanium and sodium chloride will be removed at the same time. Sodium chloride and any residual sodium that is present in the particles are then removed in a water-alcohol flushing.

After separation, the sodium chloride is then recycled to the electrolytic cell 12 for regeneration. Sodium return in the volume of the process stream for introduction into the combustion chamber 10, and chlorine is used in chlorate ore 15. It should be noted that although both the electrolysis of sodium chloride, and subsequent chlorination of the ore will be carried out with the use of technology, well known in this field, such as integration and recycling side of the reaction product specified is impossible in the way of Kroll or the way of the hunter due to the periodic nature of these methods and obtain as an intermediate product of titanium sponge. The operators of the way Kroll and method of the hunter becoming the titanium tetrachloride for use in the production of titanium. The integration of these separate ways, provided invented a chemical production method, has significant benefits both in terms of costs and the threads.

For chlorination of titanium ore (rutile, anatase or ilmenite) in chloretone 15 use of chlorine electrolytic cell 12. At the stage of chlorination of titanium ore is mixed with coke and chemically transformed in the presence of chlorine in a fluidized bed or other appropriate kiln chloretone 15. Titanium dioxide contained in the original material, interacts with the formation of titanium tetrachloride, while the oxygen with the coke to form carbon dioxide. Iron and other impurity metals present in the ore, also develop during chlorination in their respective chlorides. Then the titanium chloride condense and purify by distillation in column 11. In accordance with common practice peeled pair of titanium chloride condense again and sold to manufacturers of titanium; however, in this integrated way flow of vapors of titanium tetrachloride are used directly in the production method.

After ensuring warmth of the process for stage distillation in the heat exchanger 16, the temperature of the volume of the process stream to regulate the desired temperature for the combustion chamber 10 in the heat exchanger 17 and then mixed with the regenerated recycle stream to use different pumps, filters, traps, monitors, etc.

Refer now to Fig. 2 and 3, which represent respectively the technological scheme for low-temperature method (Fig. 2) and high-temperature method (Fig. 3). The main differences are the temperature at which the sodium enters the chamber 10 and out of her. For similar equipment used the same numerical designation, the purpose of which is explained in Fig. 1. For example, in Fig. 2, for low-temperature method, nutria, coming into the combustion chamber 10 is at a temperature of 200oC and has a flow rate of 38.4 kg/min titanium Tetrachloride from the evaporator is at a pressure of 2 atmospheres and at a temperature of 164oC, the flow rate through line 15A is 1.1 kg/min Can be used for pressures up to 12 atmospheres, but it is important to prevent backflow, therefore, to ensure that the flow through the nozzle of the combustion chamber was not critical or muted, the preferred elevated pressure of at least 2 atmospheres. In accordance with all aspects of the methods shown in Fig. 1, 2, 3, it is important to titanium, which is removed from separator 13, was at a temperature or lower temperature and preferably Chu is the capacity of the equipment, which is one of the major challenges in ways that are commercially used at present. While maintaining the temperature of the metal titanium is below the sintering temperature of the metal titanium, titanium will not attach to the walls of the equipment, as is the case in the methods of the prior art, and therefore its physical removal can be avoided. This is an important aspect of the invention, and it is obtained through the use of a sufficient amount of the metal Na or dilution gas, or both to control the temperature of the elementary product (or alloy).

To compare, in the periodic methods that use at the present time, it is necessary that the titanium sponge was destroyed drill hammer of the collector and, if to take into account the hardness of the sponge, this will present a challenge.

High-temperature method, illustrated in Fig. 3 shows that the temperature at which the sodium enters the evaporator, is 750oC and a flow rate approximately equal to 33.4 kg/min

The product temperature of the combustion chamber in the low-temperature method of Fig. 2 is approximately 300oC, while the be the titanium is below the sintering temperature, which is approximately 1000oC, thereby to avoid the disadvantages of the methods available at the present time. The heat exchangers on both Fig. 2 and 3, indicated by the numeral 20, although the value of the removed energy for methods Fig. 2 (low-temperature) and Fig. 3 (high temperature) are different, partly because of the placement of the heat exchanger 20 in the high-temperature process before separation of sodium chloride, while in the low-temperature method, the heat exchanger 20 is located after the separation of sodium chloride, which leads, as indicated, to the various outputs of energy. On both the flow charts of Fig. 2 and 3 freshly prepared sodium indicated by line 12A, and it can come from the electrolytic cell 12, or some other, completely different, sources of sodium. In accordance with other aspects as Fig. 2, and Fig. 3 is an illustration of the types of design parameters, which can be used to produce metallic titanium in a continuous way, which avoids the problems inherent in periodic methods used commercially at the present time.

The invention is illustrated with reference to only the titanium tetrachloride and toponymist, what mentioned above is only for illustrative purposes and it is clear that the invention relates to metals and non-metals listed in the table, which, of course, includes the fluorides of uranium and rhenium, as well as other halides, such as bromides. In addition, it is clear that although sodium is the preferred reducing agent due to its low cost and availability, it is clear that he is not the only suitable reducing agent. Suitable and thermodynamically plausible are lithium, potassium, calcium and other alkaline earth metals. Specialists in this area can easily be determined from thermodynamic tables, which metals capable of acting as a reducing agent in the above reaction; the method is mainly applicable to such reactions that are highly exothermic, as illustrated in the table, when to metal restore chloride or halide. In addition, professionals in this field is clear, and in the present invention it is assumed that the method of the claimed invention by providing a corresponding halide materials with appropriate molecular ratio of components of the desired alloy can be obtained the desired alloys.

1. The method of obtaining the elemental material or alloy of halide vapor of elemental material or mixtures thereof, comprising contacting vapor halide with a continuous stream of liquid alkali metal, or alkaline earth metal, or mixtures thereof, characterized in that said contacting is carried out by immersing halide vapor into a stream of liquid alkali metal, or alkaline earth metal, or mixtures thereof, and the liquid metal is present in a quantity sufficient to convert the halide to elemental material or alloy, and a pair of halogen is served at a pressure sufficient to create the sound speed and the resulting material or alloy support at a temperature to prevent its sintering.

2. The method according to p. 1, characterized in that the basic material is one or more of Ti, Al, Sb, Be, B, Ga, Mo, Nb, Ta, Zr, V, Ir, OS, Re and U or their alloys, while the alkali metal is Na, K or mixtures thereof, and alkaline earth metal is Mg, Ca, Ba or mixtures thereof.

3. The method according to p. 2, alicewinters material is Ti and liquid metal is Na or Mg.

5. The method according to p. 1, characterized in that a pair of halogen is homogeneously mixed with a liquid alkali or alkaline earth metal in the area surrounded by the liquid during the formation of elemental material, and a pair of halogen represent pairs of one or more of TiCl4, VCl4, NbCl5, MoCl4, GaCl3UF6, ReF6.

6. Method for continuous receipt of non-metal, or metal, or alloy, including the provision of feed vapor halide metal or non-metal, or mixtures thereof, ensuring the supply of liquid alkali or alkaline earth metal or mixtures thereof, the introduction of vapor halide, immersed in liquid alkali or alkaline earth metal or mixtures thereof, characterized in that the introduction of vapor halides perform with sound speed to obtain a powder of a non-metal, or metal or its alloy and the alkali halide or alkaline earth metal by exothermic reaction, and after separation of the powder from reagents to carry out the separation of alkali halide or alkaline earth metal into its parts, cooling and recycling the alkali or alkaline earth metal to interact with additional quantities of vapors galegeae of TiCl4, VCl4, NbCl5, MoCl4, GaCl3UF6, ReF6.

8. The method according to p. 6, characterized in that the halide is TiCl4alkaline metal is PA and the temperature of the liquid sodium away from the place where the injected pairs of halogen, support in the range of from about 200oC to about 400oC.

9. The method of producing titanium powder from sources of vapor TiCl4including the introduction of vapor TiCl4in the current flow of liquid PA by injection box office of the Ti powder from the liquid PA, characterized in that the TiCl4enter when immersed in the current thread PA, which is present in excess relative to the stoichiometric amount required for interaction with pairs of TiCl4to avoid sintering of Ti powder.

10. The method according to p. 9, characterized in that the TiCl4diluted with an inert gas to control the temperature recovery TiCl4the metal titanium.

11. Method for continuous receipt of non-metal, or metal, or alloy, including the provision of feed vapor halide and supply of liquid alkali or alkaline earth metal and recycling, the introduction of vapor halide in a liquid alkaline or deletetime is whether alkaline earth metal, characterized in that the alkali or alkaline earth metal is present in sufficient excess relative to the stoichiometric amount needed to restore the vapor halide, for removal of heat of reaction and rapid cooling of the reaction products below the sintering temperature of the obtained non-metal, or metal, or alloy, thus carry out the separation of the obtained alkali halide or alkaline earth metal into its parts - alkali or alkaline-earth metals and halogen, with subsequent recycling of the individual alkali or alkaline earth metal to interact with an additional amount of vapor halide and halogen-free to interact separated halogen ore metal or non-metal to obtain halide metal or non-metal, recycling of the halide of the metal or non-metal by introducing a halide vapor of the metal or non-metal in liquid alkali or alkaline earth metal.

12. The method according to p. 11, characterized in that the halide is a chloride of one or more of Ti or Zr.

13. The method according to p. 12, characterized in that the alkali or alkaline earth metal is present in the form of the current thread and a couple of chloride input is

 

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