US2878008A

US2878008A - Apparatus for continuous vacuum refining of sponge metallic titanium

Info

Publication number: US2878008A
Application number: US523859A
Authority: US
Inventors: Ishizuka Hiroshi
Original assignee: Individual
Current assignee: Individual
Priority date: 1955-07-22
Filing date: 1955-07-22
Publication date: 1959-03-17
Anticipated expiration: 1976-03-17

Description

March 17, 1959 HIROSHI ISHIZUKA V APPARATUS F0 Filed July 22, 1955 OF SPONGE METALLIC TITANIUM 2,878,008 R .commuous VACUUM REFINING '4 Shee'ts-Sheet l IN V EN TOR.

H/ROJH/ I JH/ZUKA W F W A TTORNEYS.

March 17, 1959 APPARATUS F OF SPONGE METALLIC TITANIUM Filed July 22, 195 5 4 Sheets-Sheet 2 F/LiE.

INVENTOR. H/ROSHI' lJH/Z UKA A TTORNEYS.

March 17, 1959 HIROSHI ISHIZUKA I 2,878,008 APPARATUS FOR commuous VACUUM REFINING OF SPONGE METALLIC TITANIUM Filed July 22, 1955 4 Sheets-Sheet 3 I I Z? A is B 2 l j 21 Y A 7 8 B [5 1e 30 4; I INVENTOR.

H/ROJH/ IJH/ZU/FA BY y F A TTORNEYS.

March 17, 1959 HIROSHI ISHIZUKA 2,87

- APPARATUS FOR CONTINUOUS VACUUM REFININGY- Y 0F SPONGE METALLIC TITANIUM Filed July 22, 1955 4 Sheets-Sheet 4 'F/EAZ,

INVEN TOR. H/ROJH/ lJl-l/Zl/KA BY we 5 ATTORNEYS.

United States APPARATUS FOR' CONTINUOUS VACUUM REFIN- ING F SPONGE METALLIC TITANIUM Hiroshi Ishizuka, Ashiya-shi, Japan Application July 22, 1955, Serial No. 523,859

2 Claims. (Cl. 266-16) i The present invention relates to an apparatus for re- "fining spongeous titanium continuously under vacuum, more particularly to an apparatus for the continuous production of high purity spongeous titanium by a process wherein titanium tetrachloride (TiCl is reacted with metallic magnesium (Mg) or sodium (Na) in a reaction cylinder in accordance with the following equations:

I titanium'industrially is performed by reacting TiCl, with Mg or Na at high temperatures in an inert gas atmosphere. In this process, the above given reaction is carried out in a reaction cylinder, usually of iron, to collect therein spongeous titanium which adheres to the inner wall of the reaction cylinder. In the case in which Mg is used as the reducing agent in the above given reaction, an excess of Mg is used. As a result, the spongeous titanium obtained contains a small amount of unreacted magnesium admixed therewith. The magnesium chloride (Mgcl obtained as by-product of the reaction cylinder is preferably removed from the bottom of the reaction, but there still remains a small amount of it in the spongeous titanium. This magnesium chloride has to be removed.

The usual practice for this removal is the vacuum separation process. The present inventor also carries out this practice. That is, in the usual process the reaction cylinder in which TiCl, and Mg are reacted together consists of an innner cylinder and an outer cylinder. Spongeous titanium precipitates and adheres to the inner wall of the inner cylinder which is then cooled to a safe temperature. The cooled inner cylinder is then inserted into the vacuum separation cylinder. The vacuum separation cylinder is a top-sealed cylinder provided with a condensing portion underneath, i.e. an outer-separating cylinder. The said inner cylinder containing therein spongeous titanium adherent to the inner wall, is first placed into said outer separating cylinder which is then evacuated to high vacuum, e.g. 10- to mm. of Hg. Then, the outer-cylinder portion'corresponding to the in- -serted inner cylinder is heated exteriorly in a heating furnace at elevated temperatures, for example, 900 to 1000 C. for more than twenty hours. The Mg and MgCl contained in the spongeous titanium are then volatilized and introduced into the lower condensing portion wherein they are condensed and solidified.

The resulting spongeous titanium then is of a high degree of purity.

After completionof the treatment, first the heating furnace is removed and cooled sufficiently. Thereafter,

atent thebute'r-separating cylinder is removed, and the inner cylinder containing the adherent spongeous titanium' is shifted to peel off and collect the spongeous titanium.

However, the spongeo'us titanium is apt to. come in contact with the ambient air during the above given operation and the large surface areaof the'spongeous titanium is likely to be readily degraded by' reacting with oxygen, nitrogen, hydrogen, etc'. Thus, unless the spongeous titanium is rapidly cooled, it is likely to burn temperatures before it is cooled to the temperature re quired by the prior art process. The said reaction receptacle is hung down Within a casing kept in vacuum or in inert gas atmosphere.

Or, the reaction inner receptacleencased in the'casing held at high temperature and in vacuum or in inert gas,

e.g. argon atmosphere is lowered into the interior or the vacuum refining apparatus according to this invention.

In the accompanying drawings given'as illustrationof the invention: 7

Fig. 1 is a sectional elevation of the apparatus illustrating the first position of said apparatus, where the upper portions of two outer casings have just been placed respectively on the corresponding. lower portions of the casings after two pairs of lids have been closed;

Fig. 2 is a similar view of Fig. 1 illustrating the second position of the apparatus, where the two inner receptacles are descending to the respective bottoms of the vacuum distillation chamber and the condensing chamber, after the two pairs of lids have been removed laterally to their casings; I

Fig. 3 is a view similar to Fig. 1 illustrating the third position of the apparatus, where the two innerreceptacles are set respectively in their operative positions, the two hanging rods having been detached from the respective top covers of the two inner receptacles and the two pairs of lids having been removed, ready for removing the two upper portions of the outer casings;

Fig. 4 is a view similar to Fig. 1 illustrating the fourth position (i.e. the working position), where the two upper portions'of the outer casings are removed and the distillation and the condensing apparatuses are in operation. (After completion, the above order is reversed.)

Referring to the drawings, for example, the inner receptacle casing 9 holding the inner reaction receptacle at a high temperature in an inert-gas atmosphere, is placed on flange 24; the inner receptacle 2 is lowered by actuating a lateral hanging metal 5 as well as a longitudinal hanging metal 6 and a hanging rod 10 and put into an outer separation receptacle 4. The outer receptacle 4 is held in a heating furnace, and is adapted to be heated to the required temperature.

A bottom plate 3 for the inner receptacle is provided in the lower portion of the inner receptacle 2. Spongeous titanium adheres to the inner wall of the inner receptacle above the bottom plate and forms in lump form. The inner receptacle 2 having been prepared for the vacuum distillation treatment, that is, immediately after m e n of V the t qn eact n... is. su p n ed. by means of hanging rod 10 (for inner receptacle) in the I I tightened outer receptacle lid chamber 26, arrangedlaterally above outerreceptacle '4. The inner receptacle 2 1 i is then lowered as-lllustarted in the drawing by actuating "hanging rod 10. and placed into outer receptacle 4. The; I

: outer receptacle lid '7 'is'then moved to makeasuificiently air-tight seal. Then the vacuum separation is carried out.

I I After the vacuum separation. treatment has been com- I pleted, the outer receptacle lid 7 'is opened and the inner I 1 receptacle isreaised intothe inner:receptaclecasing; 9 I mounted above. The inner receptacle is sealed with the 'satio'n receptacle, lid is opened, the inner condensingre- I J Thus, the inner receptacle'zhavi ceptacle is lowered'and lix'edand then the lid is shut and,

thecondensation isfurthercontinued, I 1

g spongeous titanium admixed with Mg a d MgCl is put into the outer re-,

1 ce'ptacle 4. When heating: is carried out at high tempera'tures, e. g. 900. to 1000 (Lin high vacuum, for instance, of, 10- to mm. of Hg, Mg and MgC l 1 1 are volatilizedand enter into the inner condensationre' ceptacle 13- throughlsuction fine 11' and; are condensed f.

[and adhere in the inner condensation receptacle 13. I,

Heating elements 30 have beenadded in several loca I "tions in the drawings for the sake of illustration. 1

1' transferred even while being kept at a: high temperature I I in an. inert gasatmosphere, directly to theapparatus for i I the vacuum refining and-fixed. ;After highvacu'umand I I high temperature treatment has been completed and the bottom lid 8 for said casing and then itis separated along I i line A-:,B and is shifted for the following step.

A suction gas line is provided on the side wall of outer I receptacle 4, whichleads to aninner condensing receptacle I 1,3 I tion-plate' 12 rs provided so "that gases-I introduced by suction ,may be: setsufiiciently in the condensing receptacle: 13 and condensed and that thecondensate may be In said. inner condensing receptacle 13, a condensaprevented from falling in the suction flue .11.

' y In the gases separated by-suificient condensation in 'thecondensinginner receptacle '13 in a condensation re t ceptacle, there is practically no solid substance, but in I some cases presumably there maybe a small quantity of; solid materials. I In order to avoid the above-said con- 'tamination, a lamellar preventing sheet'18 is provided,

through which gases are passed and led to the vacuum pump.

When the sufficiently condensed and separated mixture of Mg and MgCl has been sufficiently deposited in the condensation inner receptacle, the inner receptacle is required to be exchanged. For this purpose, a condensation inner receptacle casing 21 is provided, wherein the condensation inner receptacle is suspended in airtightness. The condensation inner receptacle casing 21 is placed on the flange 25 on line A'B. Then the condensation inner receptacle is suspended in said casing to be removed. A new inner receptacle is then suspended and inserted.

For example, in order to withdraw the inner receptacle 13 containing Mg and MgCl adherent therein, out of the condensation receptacle 14, the condensation inner receptacle casing 21 is mounted along line A--B' and a vacuum is created in said casing. The lid 19 for condensing inner receptacle casing 21 is shifted into the lid chamber 28 provided laterally with a condensation inner receptacle lid which is arranged in air-tightness on the inner condensation receptacle and accommodated in the position of inner condensation receptacle lid 19. The inner condensation cylinder 13 is attached after the hanging rod 22 is inserted and then is received by the inner condensation receptacle casing. The lid is air-tightly sealed by shifting the casing bottom lid 20 in the bottom lid chamber 29 for the inner condensing receptacle casing, the casing whereupon is separated on the line A'-B' and is removed.

Then, the inner condensing receptacle casing containing a new inner condensing receptacle is set on line A'-B' above the condensation receptacle, the bottom lid for inner condensation receptacle is opened and the conden- 1 1 'Anoutlet 16 for suction gas is provided on the'inner I receptacle .lid 151 for condensing on top of condensing inner receptacle'13, and the inner receptacle 13 is 'ap- I I propriately suspended by means ofhanging rod 22,-thus I being adapted to: be taken out of or inserted into the con- I 'densin'g receptacle 14; I I 1 1 1 I I Thecondensing receptacle 14 can be cooledsufficiently by .a condensation cylinder 17." 1

According to this inventi0n,'as above-said; the reaction receptacle in whichspongeous titanium adheres can be admixed MgQl has been 'gasified and separated, the

spongeous; titanium iswithdrawn andshifted adherent in, the reaction receptacle at a high: temperature before it has'been cooled ton low temperature and the opera-I I I tionj can;thus' be carried; out: continuously. Moreover, the thus gasified Mg and Mg'Cl are condensed in a con I nected condensation receptacle and-are condensed and de I I 1 posited intoa movable receptacle which is withdrawn and charged. The vacuum separation is, thus, performed con tinuously. I

withdrawal of the inner receptacle for the vacuum sepaseparation receptacle and'by performing the charging and "withdrawal of said. inner receptacle under exclusion of I I contact'with atmospheric air; And as theinncr receptacle I is withdrawn and afresh receptacle is replaced, after the vacum treatment has been colmpl'etedflhe operation can be made continuously with out contact with the out;

side air.

Moreover, the condensation of vacuum separated Mg and MgCl is effected in a connected condensation receptacle. The shifting of the receptacle, i. e., the condensation receptacle containing Mg and MgCl condensed therein and adherent thereto, can be carried out continuously without allowing contact with the outside air as in the above mentioned case relative to the inner receptacle.

The present invention relates to an apparatus wherein the usual batch procedure is carried out continuously and rapidly while avoiding the deterioration of the quality of the products. With this apparatus, a high grade product can be easily obtained industrially and economically. According to this apparatus, the absorption of O, N and H 0 does not occur, the purity of product is high, the damage of pumps due to the presence of HCl is low, economy in heat, labor and time can be achieved and the mass production of uniform products is assured at high yield. The apparatus according to this invention can be used for the vacuum separation not only in connection with the reduction of TiCl, by Mg but also with the reduction by means of Na.

The present invention which is applicable also to other similar metals enables the continuous operation which has heretofore been considered impossible and aims particularly to provide continuous production of titanium especially in. vacuum refining. Thus the great industrial value of the present invention is readily ap parent.

What I claim:

1. Apparatus for continuous vacuum distillation which comprises, in combination, a distillation apparatus provided with an outer casing to accommodate therein an According to the present invention, the charging and' J ration can be carriedoutrapidly in vacuum or inertgas. atmosphere and can also be performed at elevated 'tem I per'atures by putting the inner 1 receptacle containing 'spongeous titanium therein adherent into the vacuum inner receptacle in which the mixture to be subjected to vacuum distillation is contained therein adherent to the wall, a pair of lids provided above said inner receptacle when said inner receptacle is in its operational position within the distillation apparatus, said pair of lids being adapted to keep said outer casing air-tight, and a separate condensation apparatus connected to said distillation apparatus, said condensation apparatus comprising an outer casing to accommodate therein an inner receptacle, adapted to receive substances which have been gasified by the vacuum distillation performed in said vacuum distillation apparatus, a pair of lids provided above the last mentioned inner receptacle when said last mentioned inner receptacle is in its operational position within the condensation apparatus, said last mentioned pair of lids being adapted to keep the last mentioned outer casing air-tight, and there is provided a vacuum pump for evacuation, whereby said distillation apparatus and said condensation apparatus are connected together, means adapted for mounting thereon an inner receptacle encased in an inner receptacle casing and means for introducing said inner receptacle into said distillation apparatus while maintaining exclusion of air from said distillation apparatus.

2. Apparatus for continuous vacuum distillation which comprises, in combination, a distillation apparatus provided with an outer casing to accommodate therein as inner receptacle in which the mixture to be subjected to vacuum distillation is contained therein adherent to the wall, a pair of lids provided above said inner receptacle when said inner receptacle is in its operational position within the distillation apparatus, said pair of lids being adapted to keep said outer casing air-tight, and a separate condensation apparatus connected to said distillation apparatus, said condensation apparatus comprising an outer casing to accommodate therein an inner receptacle, adapted to receive substances which have been gasified by the vacuum distillation performed in said vacuum distillation apparatus, a pair of lids provided above the last mentioned inner receptacle when said last mentioned inner receptacle is in its operational position within the condensation apparatus, said last mentioned pair of lids being adapted to keep the last mentioned outer casing air-tight, and there is provided a vacuum pump for evacuation, whereby said distillation apparatus and said condensation apparatus are connected together, means for air-tightly encasing an inner receptacle in a casing so as to permit the removal of said inner receptacle encased in its casing from the distillation apparatus while maintaining exclusion of air from said distillation apparatus.

References Cited in the file of this patent UNITED STATES PATENTS

Claims

1. APPARATUS FOR CONTINUOUS VACUUM DISTILLATION WHICH COMPRISES, IN COMBINATION, A DISTILLATION APPARATUS PROVIDED WITH AN OUTER CASING TO ACCOMODATE THEREIN AN INNER RECEPTACLE IN WHICH THE MIXTURE TO BE SUBJECTED TO VACUUM DISTILLATION IS CONTAINED THEREIN ADHERENT TO THE WALL, A PAIR OF LIDS PROVIDED ABOVE SAID INNER RECEPTACLE WHEN SAID INNER RECEPTACLE IS IN ITS OPERATIONAL POSITION WITHIN THE DISTILLATION APPARATUS, SAID PAIR OF LIDS BEING ADAPTED TO KEEP SAID OUTER CASING AIR-TIGHT, AND A SEPARATE CONDENSATION APPARATUS CONNECTED TO SAID DISTILLATION APPARATUS, SAID CONDENSATION APPARATUS COMPRISING AN OUTER CASING TO ACCOMDATE THEREIN AN INNER RECEPTACLE, ADAPTED TO RECEIVE SUBSTANCES WHICH HAVE BEEN GASIFIED BY THE VACUUM DISTILLATION PERFORMED IN SAID VACUUM DISTILLATION APPARATUS, A PAIR OF LIDS PROVIDED ABOVE THE LAST MENTIONED INNER RECEPTACLE WHEN SAID LAST MENTIONED INNER RECEPTACLE IS IN ITS OPERATIONAL POSITION WITHIN THE CONDENSATION APPARATUS, SAID LAST MENTIONED OUTER CASING BEING ADAPTED TO KEEP THE LAST MENTIONED PAIR OF LIDS AIR-TIGHT, AND THERE IS PROVIDED A VACUUM PUMP FOR EVACUATION, WHEREBY SAID DISTILLATION APPARATUS AND SAID CONDENSATION APPARATUS ARE CONNECTED TOGETHER, MEANS ADAPTED FOR MOUNTING THEREON AN INNER RECEPTACLE ENCASED IN AN INNER RECEPTACLE CASING AND MEANS FOR INTRODUCING SAID INNER RECEPTACLE INTO SAID DISTILLATION APPARATUS WHILE MAINTAINING EXCULSION OF AIR FROM SAID DISTILLATION APPARATUS.