DE2101855A1 - Titanium halogenide extraction and condensation plant - - comprises three component parts - Google Patents

Abstract

The reaction chamber and the condenser are fitted to a centre part, which serves as an air tight heat flow blocking device and contains a valve for the main connecting channel and additional connecting channels for the reagents to be fed into the plant, and also the vacuum connection for the condenser. In the prefd. design the condenser and reaction chamber may be connected to either side of the centre part. The equipment permits carrying out the chlorination and condensing stages of the process without the need for heating up the reaction chamber two times.

Description

1. Vsesojuznyj nau # no-issledovatel'skij i proektnyj institute aljuminievoj, magnievoj i @lektrodnoj promy # lennosti Leningrad / USSR 2. Ust'-Kamenogorskij titano-magnievyj Kombat Ust'-Eamenogorsk / USSR APPARATUS FOR TITANIUM HALOGENIDE REDUCTION AND SUBSEQUENT VACUUM DETECTION OF REDUCTION PRODUCTS The definition refers to the area the production of difficult-to-melt metals, preferably titanium sponge, and on apparatus for titanium halide reduction and subsequent vacuum deposition of the Reduction products.

In the production of titanium sponge a method is used according to the thermal reduction of titanium halide by means of magnesium in airtight closed Reaction chamber is carried out while the vacuum deposition of the reduction products with the help of ice condenser, which after cooling down and dismantling of the Reaction chamber is placed on ibr. This is the reaction chamber to perform the vacuum deposition process again to a temperature of heated to approx. 980 ° C.

The cooling and reheating of the reaction chamber as well as dismantling the same before putting on the capacitor can when performing the reduction - and the vacuum deposition process in an apparatus can be avoided, whereby -by it becomes possible to reduce the labor involved in producing titanium sponge Electric energy consumption to selenium and contamination of the reaction mass during dismantling -Avoid running the reaction chamber.

Creating an apparatus that enables both of the process To realize without dismantling and reheating the equipment is a complicated problem.

Attempts to create such apparatus are known. One design consists of an apparatus that consists of two parts assembled retort. There are gas burners in the lower part. The upper part has a lock for supplying magnesium and connecting channels for supplying titanium tetrachloride and for connection to the vacuum line.

Since the reduction process in the apparatus is in the usable kawn of the same If there is a large difference between the upper part and the lower part temperature, intermediate products become the reaction, including lower titanium chlorides, condenses in the retort the useful yield of titanium sponge is reduced and the equipment is dismantled complicated and dangerous.

This is also an apparatus known as the reaction chamber and condenser contains, the interiors of which are separated from each other and connected by a main channel In it a locking device is installed, which this channel during of the reduction process. The connecting channels for supplying reagents go through the reaction chamber cover while the channel is ready to connect the vacuum line is located in the condenser cover ;.

In these apparatuses, the reaction chamber and condenser are designed separately and the main channel goes through an interchangeable piece of pipe which is cut into the side surfaces of the reaction chamber and the condenser, while the drive for the closure device of this channel is located in the condenser and on its side surface The reaction chamber is used to carry out the reduction process is placed in a furnace and closed by a heat flow barrier, through which the pipe section of the main and connecting ducts is passed.

These apparatuses have significant design deficiencies caused by the arrangement of the apparatus elements and their connection In the construction, the main channel entry is in the growth zone the titanium sponge garnissage, where the coating grows from the latter. This is how it becomes required to reduce the degree of filling of the usable reaction chamber space sit down because <> the drive of the locking device <sits> in the condenser vacuum distillation products are located on the drive and it is difficult to remove the Apparatus to operate and assemble, as a large number of connections between the individual elements that are connected to one another in airtight manner have to.

It is the aim of the present invention to overcome the drawbacks mentioned to eliminate.

The invention is based on the object of creating an apparatus for titanium halide reduction and subsequent vacuum deposition of the induction products, in which the reaction chamber and condenser chamber are separated from one another Have a minimal number of connections, and the inlets of the main channel are arranged in such a way that the growth of titanium sponge garnish is avoided, and the drive of the main channel closure device is designed so that no vacuum deposition products can condense on it.

This object is achieved according to the invention in that the apparatus consists of several parts and contains a middle part at the open ends The reaction chamber and the condenser are connected to the air-tight Middle part airtight the reaction chamber space from the condenser space and serves as The main channel is led through the middle part, which and condenser chamber with one another. The drive of the locking device and the connecting channels are also passed through and on the middle part Surface brought out.

Thanks to this constructive solution, the reaction chamber and condenser chamber are separated from each other when using a large number of connections between the components and the apparatus is given a compact form.

The middle part is expediently with protruding into the condenser Projection executed, which with the inner surface of the capacitor an annular Forms space from which a connecting channel for connection to the vacuum line is led out This channel goes through the middle part and is led out to its outer surface ring-shaped space should be so wide that the formation of a filter bar from Londensationsproduk-th in the vacuum deposition process between the central part projection and the inner surface of the capacitor is guaranteed.

Such a design of the middle part allows easy Operate the vacuum line and ensure operational safety of the apparatus during the vacuum separation.

It is also useful to have the reaction chamber and condenser facing one another interchangeably, i.e. they should be able to work with the equipment that to carry out the processes for the titanium halide / reduction is intended as also with the equipment necessary to carry out the operations of vacuum deposition the reduction products is determined, functional to cooperate.

Such a design of the apparatus makes it possible to use the condenser to use with vacuum distillation products for the operations of reduction, whereby the reagents are fully utilized.

Here, the middle part is expediently symmetrically 1 related executed on the cross-sectional plane and with twice the number of connection channels that exit from the middle part on each side, which is attached to the reaction chamber - and the Condensate room adjoins, with a blind flange provided on each of these channels is to make these channels depending on the techno-legal processes going on in the reaction chamber and take place in the condenser.

With such a design of the middle part, the assembly work and the contact between the condensate and the outside air is eliminated the quality of the titanium sponge made using the previous process remaining magnesium is increased.

In accordance with the present invention, there has been provided an apparatus for reducing titanium halide and subsequent vacuum separation of the reduction products created the high useful yield on titanium sponge and operational safety guaranteed as well service and assembly easier.

Embodiments of the invention illustrated by drawings are described below; It shows Fig. 1 a longitudinal section through the apparatus according to the invention for titanium halide reduction and subsequent vacuum Isolation of the reduction products with the reaction chamber inserted in the electric furnace, FIG. 2 a longitudinal section through the central part of the apparatus according to the invention on an enlarged scale, FIG. 3 the top view of this central part with partial detail, FIG. 4 shows a section along line IV-IV of FIG. 3, FIG. 5 shows the node A of FIG. 1 on an enlarged scale, FIG. 6 shows a longitudinal section through the central part, which according to the invention is designed symmetrically with respect to the cross-sectional plane , and FIG. 7 shows the top view of the central part shown in FIG. 6 and a section along line VII-VII of FIG. 6.

The apparatus shown in Fig. 1 for titanium halide reduction and subsequent vacuum deposition of the reduction - products according to the invention has a multi-part construction, the lower part serving as the reaction chamber 1 and the upper part serving as a condenser 2. Between these there is a central part 3, at the open ends of which the reaction chamber 1 and the condenser 2 are connected.

The reaction chamber @ consists of heat-resistant steel according to the measure A pipe 4 is attached to the lower part of the reaction chamber and is used for draining is determined by magnesium chloride. Tube 4 can be closed airtight by hood 5 will.

In the reaction chamber @ is above the fastening level of the pipe 4 False base 6 is provided, which prevents metallic titanium from entering the locking device This pipe has arrived. On the upper part of the reaction chamber there is flange 7 for the connection welded with middle part 3.

Reaction chamber 1, which is used to carry out the technological processes in the thermal reduction of titanium tetra chloride with magnesium and the subsequent Vacuum distillation of the titanium sponge obtained during the reduction process is located in the electric furnace 8, which is distributed over three zones in the height direction Has stimulating elements in the go-home of the furnace 8 there are channels 9 for the Ktüilluftum -lauf and temperature sensors 10 are installed, which the tempe Monitor the temperature of the reaction chamber wall. Channel 11 connects the usable furnace space The lower part of the furnace can be sealed airtight with the aid of the hood 12 Channels 9 are connected to cooling air nozzles 13, the locking devices 14 contain for this nozzle 13 and control flaps 15, with the help of which the amount of cooling air is regulated.

The condenser 2 is built in the same way as the reaction chamber 1 and also has a tube 16, bottom 17 and connecting flange 18. The condenser 2 and reaction chamber 1 are gfgfn each other exchangeable, ie they have the same shape and identical individual parts that are connected to other equipment elements of the apparatus - electric oven 8, cooling device and middle part 3.

As can be seen from FIG. 2, the middle part @ consists of a Welded construction with connecting flanges 19.

In its center is the main channel 20, which connects the interior of the reaction chamber 1 with that of the condenser 2 and which is covered by a closure device during the reduction. According to the invention, the drive of this closure device is led out through the middle part 3 to its outer surface. In the example under consideration the main channel 20 is covered by flap 21, which is connected to pivot lever 22 which is in turn attached to shaft 23 (Fig. 3 and 4) Outer surface is led out. This pipe 24 is covered by a hood 25. Two pipes are led through the middle part 3, which are used as a connecting channel 26 (Fig. 2) for the supply of liquid magnesium and a connecting channel 27 (Fig. 4) for the Titanium tetrachloride are used. These pipes are led out to the outer surface of the central part 3 and can be made airtight by means of blind flanges 28 and 29 closed In the middle part 3, annular chamber 30 (Fig. 2 and 4) is provided, which is separated airtight from the interior of the middle part 3. Annular chamber 30 is located in the upper cylindrical projection 31 and is connected to the usable space of the condenser 2 via openings @ 32 30 can be connected to the vacuum line via connection channel 33 (FIGS. 1 and 2).

The protrusion 31 of the middle part 3, which protrudes into the capacitor 2, forms with the inner surface of the capacitor 2 the 10 to 20 min wide annular space 34. This makes it possible for a filter layer to be formed, which is produced by vacuum deposition emerging Condensation products exist between the edge of the projection 31 of the middle part 3 and the inner surface of the capacitor 1 forms.

The airtight central part 3 is surrounded by ring-shaped partitions 35 (Fig. 2 and 4) subdivided into a series of rooms, which are connected to one another through openings 36 are connected, forming the central part - interior space. The annular Partition walls 35 of the middle part 3, its base and its interior serve as a heat flow barrier between usable condenser space and usable reaction chamber space. They protect also main channel 20 against cooling in order to prevent it from being in the Vacuum separation of titanium sponge condenses products.

It is provided for evacuating the gas from the middle part - in -nan space stub 37 (Fig.a). Stub 38 guided through the middle part flange serves to supply inert gas and to measure the pressure in the reaction chamber. 1 The middle part 3 connecting the reaction chamber 7 and the condenser @ has screw connections 39 (FIG. 5), with between rubber sealing rings 40 are inserted into the connecting flanges to ensure airtightness of the connection. to prevent destruction of the sealing rings in the flanges 209830/0441 designed ring-shaped channels 41 for cooling water supply.

The cooling device is on the flanges 18 of the condenser 2 (FIG. 1) mounted, the water caissons 42, annular spray line 43 and collection chamber 44 for the water supplied via the annular spray line 43 has Ktiiilwasser is via distribution line 45 to the gaissons 42 and the annular spray line 43 water flows out of chamber 44 via nozzle 46 between caissons 42 and wall of the condenser 2 is air cushion 47, which is open on the top and is connected to the outside air at the bottom via opening 48 in chamber 44.

The apparatus works as follows.

The apparatus is, as shown in Fig. 1, mounted flap 21 with the help of the drive of the locking device -opened and connects the room of the reaction chamber 1 with that of the condenser 2.

Connection channel 33 is connected to the vacuum line, air is inflated from the apparatus and it is checked whether the apparatus is assembled airtight The apparatus is filled with inert gas via nozzle 38 (Fig. 2), up to 0.05 to 0.2 at overpressure is reached.

The apparatus is used in furnace 8 and at approx. 8000C temperature The required amount of liquid magnesium is then heated via channel 26 Poured into the apparatus and blind flange 28 placed on nozzle 26.

Flap 21 is closed and channel 27 (Fig. 4) is predetermined Amount of titanium tetrachloride.

The reaction in the apparatus produces 2 Mg + TiCl4 = 2 MgCl2 + Ti metallic titanium and magnesium chloride.

As a result of the exothermic reaction, the apparatus is on the whole, from liquid magnesium is heated @.

The heating of the upper part of the apparatus is switched off and cooling air is blown onto the reaction zones via channels 9 (FIG. 1).

The intensity with which the air is inflated can be regulated so that the temperature of the reaction chamber wall is in a range from 780 to 8600C. Metallic Titanium sinks to the bottom of the reaction chamber and forms one above the false bottom 6 Titanium sponge block. Magnesium chloride sinks into the lower part of the apparatus and becomes periodically removed via tube 4.

After 60 to 65% of the imported magnesium according to the above Reaction are used, the supply of titanium tetrachloride is stopped.

This brings the reduction process to an end and the apparatus becomes prepared for vacuum separation of the reduction products.

A special furnace can be used in the vacuum deposition process, in which the warm apparatus is used after coming out of the furnace in which the reduction process The vacuum deposition process can, however, also be carried out proceed in the Ofon which can be seen from Fig. 1 and which is described above and is intended to perform both processes. The following is the preparation of the apparatus for performing the vacuum breaking process using of the furnace shown in Fig. 1 described.

On tube 4 hood 5 is placed. With the help of the hood 12 and the Device 14 is furnace 8 closed airtight.

Flap 21 is opened, with the result that main channel 20 connects the reaction chamber and condenser space. A blind flange 29 is placed on channel 27 (Fig. 4) through which titanium tetrachloride was fed, and a hood on the exit point of the shaft 23 Inert gas is pumped out of the interior of the apparatus via connecting channel 33. At the same time, gas is pumped out of the interior of the central part via nozzle 37 (FIG. 2) and from the interior of the furnace via channel 11 (FIG. 1).

The outer surface of the condenser is cooled by sprinkling water via the spray line 43 and by water cooling the caissons 42.

Now the vacuum separation process of the reaction mass begins.

With the help of the oven 8, the temperature of the reaction chamber - Outer wall brought to approx. 980 ° C.

Leftover magnesium and magnesium chloride are removed from the titanium sponge driven off and condense on the inner wall of the condenser 2nd sprinkling the outer wall ensures that the sublimates are mainly on the condensate -sator wall and partially condense on the surface of the middle part projection, and prevents magnesium and magnesium chloride vapors from entering the annular space 34 get there, as there is between the capacitor @ and the face above it of the central part projection forms a filter layer of condensate.

Then, according to an ordinary procedure, the sublimation is terminated of the volatile components. The heating of the apparatus is switched off Apparatus is filled with inert gas and taken out of the oven 8 to approx to cool down to room temperature, then @r is dismantled.

If a capacitor 2 is used, the r is exchanged with the reaction chamber @ can be used, the capacitor 2 is used as a reaction chamber 1 when the apparatus is dismantled The next process is used, but the previous one remains in the capacitor @ Process condensed magnesium.

As can be seen from FIGS. 6 and 7, the middle part 3 can be symmetrical with respect to the cross-sectional plane. This plane becomes the annular Bushing 49 arranged into which the rotatable throttle valve 50 is installed, which the main channel 20, which connects the space of the condenser 2 with that of the reaction chamber 1, is installed A middle part 3 constructed in this way has twice the number of connecting channels. Es to reduce the number of pipelines, the supply channels for magnesium - and titanium tetrachloride, which emerge on each side of the central part, which at the Eondensa -tor - or reaction chamber space bounds - 'concentrically in a nozzle 51 arranged. The connection channels for the reagents supply can be airtight are covered by hoods 52.Dros -selklappe 50 is attached to shaft 53, the is led out on the middle part side surface, here the shaft exit can through Hood 54 are covered.

With this type of apparatus, after performing the Process for vacuum separation of the reduction products by means of the throttle valve 50 the main channel, 20 which Reaction chamber and condenser space connects, covered, condenser 2 together with Middle part 3 dismantled, the Roaktionskammerlaus on the freed middle part side the previously titanium sponge was removed, attached and then the apparatus is anew ready for the next thermal titanium halide reduction process using magnesium using reagents contained in capacitor 2 from the previous vacuum deposition process have remained behind.

Here, the connecting ducts must be covered airtight not to go through the process with the corresponding position of the apparatus required are.

When using a symmetrically built middle part 3 and of the reaction chamber7 and condenser, which are interchangeable with one another, becomes the Number of assembly work steps reduces contact between condensate and outside air eliminates and thereby the titanium sponge yield with high quality of the commercial metal enlarged.

Although in the description of the generation @@ titanium sponge the The invention can be talked about successfully in apparatuses for carrying out analog technological processes in the production of other more refractory Metals, e.g. zirconium, can be used.

Claims (4)

PATENT CLAIMS: 1. Apparatus for 'ditanium halide reduction and subsequent Vacuum separation of the reduction products, the reaction chamber and condenser, the spaces of which are connected to one another by a main channel, which is covered during the reduction process, as well as connecting channels for introducing reagents into the reaction chamber space and for connecting the condenser to a vacuum line, characterized in that the apparatus consists of several Parts consists and contains a middle part (3), at the open ends of which Jar dip - reaction chamber (1) and condenser (2) are connected airtight, the middle part (3) separating the reaction chamber space from the condenser space and as The heat flow barrier is used, and the main channel (20) and the drive are guided through this central part the closure device and the connecting channels (26; 27,33) for the reagent supply into the reaction chamber space and for connecting the capacitor (2) to the vacuum line and led out to the outer surface of the central part (3). 2. Apparatus according to claim 1, dadurchggekonn - zeic ii net that the central part in the capacitor (2) has protruding projection (31) which is connected to the inner surface of the Condenser 'annular space (34) forms into the connecting - (2) channel (33) for connecting the capacitor to the vacuum - (33) (3) line opens, the channel going through the middle part and led out to its outer surface is vnd that the width of the annular space (34) is chosen so that the formation of a filter web from condensation products occurring during the vacuum deposition process between the edge of the projection (31) of the central part (3) and the inner surface of the capacitor (2) ensures i. 3.Apparat according to claim 1 or 2, characterized in that the reaction chamber (1) and condenser (2) against each other are designed to be interchangeable. 4. Apparatus according to claim 3, d a d u r c h g e k e n n -z e i c h n e t, since the central part (3) is symmetrical with respect to its cross-sectional plane and with twice the number of connecting channels running on each side emerge from the middle part (3), the channels being provided with blind flanges are to these channels depending on the technological processes that take place in the reaction chamber (1) and in the condenser (2) proceed to cover. L e r s e i t e