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WO1996039241A1 - Ensemble filtrant au carbone poreux pour le traitement du chlorure de zirconium - Google Patents

Ensemble filtrant au carbone poreux pour le traitement du chlorure de zirconium Download PDF

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Publication number
WO1996039241A1
WO1996039241A1 PCT/US1996/008286 US9608286W WO9639241A1 WO 1996039241 A1 WO1996039241 A1 WO 1996039241A1 US 9608286 W US9608286 W US 9608286W WO 9639241 A1 WO9639241 A1 WO 9639241A1
Authority
WO
WIPO (PCT)
Prior art keywords
filter
chlorinator
filter assembly
cooler
zirconium chloride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1996/008286
Other languages
English (en)
Inventor
Robert S. Yih
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
TDY Industries LLC
Original Assignee
Teledyne Industries Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Teledyne Industries Inc filed Critical Teledyne Industries Inc
Publication of WO1996039241A1 publication Critical patent/WO1996039241A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
    • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
    • B01D46/2407—Filter candles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2055—Carbonaceous material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/0002—Casings; Housings; Frame constructions
    • B01D46/0005—Mounting of filtering elements within casings, housings or frames
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/56—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with multiple filtering elements, characterised by their mutual disposition
    • B01D46/58—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with multiple filtering elements, characterised by their mutual disposition connected in parallel
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/04—Halides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/14—Obtaining zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2265/00—Casings, housings or mounting for filters specially adapted for separating dispersed particles from gases or vapours
    • B01D2265/02—Non-permanent measures for connecting different parts of the filter
    • B01D2265/024—Mounting aids
    • B01D2265/025—Mounting aids making use of ramps or cams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2271/00—Sealings for filters specially adapted for separating dispersed particles from gases or vapours
    • B01D2271/02—Gaskets, sealings

Definitions

  • the present invention relates to a process for separating zirconium chloride vapor from other materials present in a carbochlorination of zircon sand and, more particularly, to a filter assembly adapted for use with a chlorination reactor containing suspended particulate solids and gaseous compounds which are entrained therewith so that the gaseous or vapor phase compounds are separated from the particulate solids.
  • the present invention concerns a porous carbon filter assembly adapted for use with a plenum connected in fluid communication with a chlorinator reactor operative to reduce zircon sand into residue and chlorinator off gases of zirconium chloride and silicon chloride vapors so that chlorinator off gases can be separated effectively from the suspended particulate solids present in the reactor.
  • the present invention is also used in combination with a de-sublimation apparatus connected downstream of and in fluid communication with the porous carbon filter assembly so that the gaseous zirconium chloride can condense, i.e., de-sublime, into a solid zirconium chloride.
  • zirconium metal is produced from solid zirconium chloride.
  • feedstock 2 for this process is zircon sand 4 bearing the chemical name, zirconium silicon oxide (ZrSi0 4 ) , is mixed with carbon for use in a carbo-chlorination reaction zone.
  • Feedstock 2 is placed in a standard feed hopper 4 and is then conveyed by a conveyor 6 into a conventional sand chlorinator reactor 8, which is typically a fluidized bed reactor.
  • Feedstock 2 which is heated by induction coils 10 resting within the sand chlorinator reactor 8 on the fluidized bed so that chlorine gas (Cl 2 ) can percolate therethrough.
  • Chlorine gas acts as an oxidizing agent that reacts with feedstock 2 to produce a residue and chlorinator off gases, particularly gaseous zirconium chloride vapor (ZrCl , and gaseous silicon chloride, SiCl 4 .
  • the chlorinator off gases are produced in sand chlorinator reactor 8, they mix with fine suspended particulate solids that are introduced into sand chlorinator reactor 8 when the zircon sand is deposited thereinto.
  • the chlorinator off gases rise within sand chlorinator 8 and are cooled by a cooler 12. The residue is discarded from the bottom of chlorinator reactor 8.
  • Filter assembly 16 includes a plurality of filter elements 18, each of which are a cloth bag secured over a metal cage. Filter assembly 16 divides an interior of primary filter plenum 14 into an upstream plenum region 20 which is in fluid communication with sand chlorinator reactor 8 and a downstream plenum region 22 in fluid communication with upstream plenum region 20 through filter elements 18. A pressure differential between upstream plenum region 20 and downstream plenum region 22 can cause the chlorinator off gases as well as particles of carbon to migrate through cloth bag filter elements 18.
  • the chlorinator off gases are fed into a top center portion of primary condenser 24 so that the gaseous zirconium chloride can "de-sublime” into a solid zirconium chloride as it enters and moves through the cooled condenser chamber 26.
  • de-sublime is utilized herein to describe a phase change that the gaseous zirconium chloride undergoes and is considered an opposite phase change to sublimation.
  • Sublimation describes a situation whereby a compound or element changes from its solid phase directly to its gaseous phase without ever passing through its intermediate liquid phase.
  • “De-sublimation” is hereby defined as a situation where a compound or element changes directly from its gaseous phase to its solid phase without ever passing through its intermediate liquid phase.
  • the cool condenser chamber 26 along with the particles of seed material causes the gaseous zirconium chloride to de-sublime into a solid zirconium chloride.
  • the solid zirconium chloride having a density substantially greater than the remaining chlorinator off gases falls to a funnel-shaped bottom portion of primary condenser 24 where it is subsequently directed into a chloride receptacle 28.
  • gaseous zirconium chloride de-sublimes in primary condenser 20.
  • the gaseous silicon chloride and the remaining gaseous zirconium chloride is directed to a secondary condenser 30.
  • most of the remaining gaseous zirconium chloride is de-sublimed with the aid of a cool secondary condenser chamber 34 in the presence of particles of a seed material.
  • the solid zirconium chloride falls to a funnel-shaped bottom portion of secondary condenser 30 and is subsequently deposited into a second zirconium chloride receptacle 28'.
  • Second filter assembly 16' includes a second filter elements 18' which are cloth bag filters connected to metal cages similar to filter elements 18 described above. Typically, however, second filter assembly 16' is identical in construction but smaller in size than filter assembly 16. Although it is not required that filter assembly 16 and second filter assembly 16' be identical in construction, economics and simplicity of maintenance support this arrangement.
  • cloth bag filter elements are fragile and tend to break down over relatively short periods of time. Although purging can help to reduce replacement costs of the cloth bag filters, the high pressure nitrogen stresses the cloth bag material in an opposite direction of the flow of the chlorinator off gases, thus shortening service life of these filter elements. With a shortened service life, maintenance costs increase because of the materials and labor associated with changing the cloth bag filter elements. For some plenum designs, the plenum must be cut open to gain access to the cloth bag filter elements. Furthermore, because of cloth material, temperatures in the chlorinator reactor must be maintained relatively low due to the risk that the cloth material might ignite on fire.
  • Another problem with this prior art process is associated with the use of seed material.
  • This process requires the use of seed material to act as a "physical catalyst" for the gaseous zirconium chloride to de-sublime into the solid zirconium chloride particulate.
  • This catalytic effect is similar to "seeding" of clouds whereby the seed material provides a surface area upon which gases can condense.
  • This seed material although helpful for de-sublimation, must eventually be removed from the solid zirconium chloride and discarded as a waste product. When fine carbon is used as the seed material, the product is undesirably colored. Silica sand is also used as seed material.
  • the fluffy solid zirconium chloride tends to clog the funnel-shaped bottom portion of the condenser. As a result, production must be halted so that the condenser can be cleaned before operations can again be continued. Furthermore, the fluffy solid zirconium chloride tends to fill the chloride receptacles faster than the more dense zirconium chloride and, thus, extra labor is required for frequent exchanging of empty chloride receptacles for the full ones.
  • An improved process should include a new and improved filter assembly to filter chlorinator off gases from the suspended particulate solids. It would also be advantageous if this filter assembly would have superior performance characteristics such as improved dust collection efficiency, a longer service life, reduced maintenance requirements, and simple installation requirements. It would be further advantageous if the filter elements of this filter assembly be fabricated from a porous material having a much higher ignition temperature than cloth material. Further, it would be desirable to employ higher temperature processing so that high production efficiencies could be achieved.
  • a still further object of the present invention is to provide a porous carbon filter assembly which is versatile for use in high temperature, highly corrosive environments where an oxidizer reactor is employed to reduce a substance to oxidizer off gases and residue.
  • Yet another object of the present invention is to provide a porous carbon filter assembly which minimizes leakage of fine suspended particulate solids between an upstream plenum region of the filter plenum and a downstream plenum region of the filter plenum.
  • a further object of the present invention is to provide a porous carbon filter assembly which minimizes the pressure drop between the upstream plenum region of the filter assembly and the downstream plenum region of the filter plenum.
  • Yet still a further object of the present invention is to provide a porous carbon filter assembly that resists accumulation of the suspended particulate solids on outer surfaces of the porous carbon filter elements disposed in the downstream plenum region.
  • Another object of the present invention is to provide a porous carbon filter assembly that can be used in combination with a de-sublimation apparatus so that seed material for de-subliming gaseous zirconium chloride into a sufficiently dense, solid zirconium chloride can be eliminated.
  • a still further object of the present invention is to provide a porous carbon filter assembly that can be used in combination with a de-sublimation apparatus so that waste produced as a result of making zirconium chloride can be reduced.
  • Yet another object of the present invention is to provide a porous carbon filter assembly that can be used in combination with a de-sublimation apparatus so that the production rate of solid zirconium chloride can be increased compared to the prior art processes utilizing cloth bag filters and the introduction of seed material.
  • a still further object of the present invention is to provide a porous carbon filter assembly that can be used in combination with a de-sublimation apparatus whereby frequency of clogging of a condenser located downstream of the de-sublimation apparatus is decreased thereby reducing down time and cost of lost production due to increased maintenance associated with cleaning the clogged condenser.
  • the first exemplary embodiment of the filter assembly of the present invention is adapted for use with a plenum connected in fluid communication with an oxidizing reactor which contains suspended particulate solids and is operative for reducing a substance to gaseous compounds produced from the reduced substance and residue.
  • the oxidizing reactor can be a conventional zircon sand chlorinator reactor. The gaseous compounds produced would, therefore, be zirconium chloride and silicon chloride.
  • the filter assembly of the present invention includes a filter structure and a support structure.
  • the filter structure is fabricated from a porous carbon material, preferably of a type that has a characteristic of being resistant to accumulation of the suspended particulate solids on the filter structure.
  • the support structure is sized and adapted to be disposed and secured in an interior of the plenum to define an upstream plenum region in fluid communication with the oxidizing reactor and a downstream plenum region.
  • the support structure is operative to releasably retain the filter structure thereon in a manner so that when the suspended particulate solids and gaseous compounds are urged as a result of a pressure differential within the oxidizing reactor and the downstream plenum region to move into the plenum from the oxidizing reactor, the gaseous compounds in the upstream plenum region are permitted to pass through the filter structure and into the downstream plenum region. Simultaneously therewith, the suspended particulate solids in the upstream plenum region are prevented from passing through the filter structure and into the downstream plenum region thereby separating the gaseous compounds from the suspended particulate solids.
  • the filter structure includes at least one filter element having an elongated body member and a flange although it is preferred that the filter structure includes a plurality of filter elements.
  • the elongated body member extends longitudinally along and centrally about a longitudinal axis between a first end and an opposite second end.
  • the flange extends radially from the longitudinal axis and around the first end which defines an opening into a bore centrally disposed about the longitudinal axis.
  • the bore is formed into the body member and, preferably, terminates proximate to the second end. It is preferred that the body member and the bore are cylindrically shaped while the flange is preferably annularly shaped.
  • Each filter element includes a collar connecting the flange and the body member.
  • the support structure includes a plate fabricated from a stiff, corrosion-resistant material.
  • the plate has a flat first surface facing into the downstream plenum region and a flat second surface oriented opposite and parallel to the first surface and facing into the upstream plenum region.
  • the plate also has at least one hole formed therethrough between the first and second surfaces which is sized and adapted to receive the filter element.
  • the body member of the filter element is slidably received in the hole.
  • the support structure also includes at least one retaining device operative to releasably retain the filter element to the plate.
  • the retaining device has a retainer element formed with an aperture therethrough and preferably a pair of fasteners.
  • the retainer element is sized and adapted to extend across the first end and the flange of the filter element with the aperture sized and adapted to register with the bore of the filter element.
  • the pair of fasteners are operative to releasably interconnect the retainer element and the plate when the retainer element is placed over and across the first end and the flange of the filter element with the aperture in registration with the bore.
  • the support structure includes at least one annular support member being disposed concentrically about the hole and connected to the plate.
  • the support member has an inner wall defining a frustoconically-shaped bore so that, when the filter element is slidably received into the hole, the inner wall and the outer collar surface are facially opposing each other.
  • the filter assembly of the present invention preferably includes at least one of frustoconically-shaped ring seal, a gasket element and a weave spring element.
  • the ring seal is sized and adapted to be interposed between the inner wall and the outer collar surface when the filter element is slidably received into the hole.
  • the gasket element has a gasket opening formed therethrough and is sized and adapted to be interposed between the retainer element and the first end of the filter element with the gasket opening registering with the bore and the aperture when the retaining device releasably retains the filter element to the plate.
  • the weave spring element has a centrally-disposed port formed therethrough and is sized and adapted to be interposed between the retainer element and the gasket element with the port in registration with the aperture and the gasket opening when the filter element is slidably received into the hole.
  • the second exemplary embodiment of the present invention is a porous carbon filter assembly adapted for use in combination with a de-sublimation apparatus.
  • the de-sublimation apparatus is connected downstream of and in fluid communication with the porous carbon filter assembly and is used to de-sublime the gaseous zirconium chloride into a solid zirconium chloride while permitting other gaseous or vapor phase products to pass through.
  • the de-sublimation apparatus includes an inner cooler device, an outer cooler device, an inlet and an annular outlet.
  • the inner cooler device includes an elongated tubular member having an outer cylindrical surface and extending along a vertical longitudinal axis.
  • the inner cooler device is operative to cool the outer cylindrical surface.
  • the outer cooler device has an inner cylindrical surface concentrically surrounding the outer cylindrical surface of the tubular member in a spaced apart relationship to define an annularly-shaped conduit therebetween.
  • the outer cooler device is operative to cool the inner cylindrical surface.
  • the inlet enters into the annularly-shaped conduit and is disposed at an upper portion of the annularly-shaped conduit.
  • the inlet is adapted to convey chlorinator off gases from the porous carbon filter assembly and into the upper portion of the annularly-shaped conduit.
  • the annular outlet exits from the annularly-shaped conduit and is disposed at a bottom portion of the annularly-shaped conduit whereby the chlorinator off gases enter into the annularly-shaped conduit through the inlet and swirls downwardly therethrough while contacting the cooled outer cylindrical surface of the tubular member and the cooled inner cylindrical surface of the outer cooler device along the annularly-shaped conduit.
  • This action causes a substantial amount of the gaseous zirconium chloride of the chlorinator off gases to de-sublime into solid zirconium chloride without the addition of seed material before the solid zirconium chloride and remaining chlorinator off gases and vapors exit the annularly-shaped conduit from the annular outlet.
  • the process comprises the step of conveying a zirconium silicon sand into a chlorinator reactor containing suspended particulate solids.
  • the next step includes subjecting the zircon sand to gaseous chlorine at elevated temperatures in order to reduce the zircon sand to residue and chlorinator off gases of zirconium chloride and silicon chloride vapors.
  • the next step then includes filtering the chlorinator off gases from the suspended particulate solids through a porous carbon filter assembly.
  • the final step is de-subliming the filtered gaseous zirconium chloride into a solid zirconium chloride. It is preferred that this process include the de-sublimation apparatus as described above, maintained at a high enough temperature to permit desublimation of the zirconium chloride without appreciable contamination from solidified silicon tetrachloride.
  • FIG. 1 is a schematic diagram of a prior art process for reducing zircon sand in a sand chlorinator reactor into a residue and chlorinator off gases of zirconium chloride and silicon chloride so that the gaseous zirconium chloride can subsequently be de-sublimed into a dense solidified zirconium chloride powder;
  • FIG 2 is a schematic diagram of a new and improved process of the present invention for reducing zircon sand in a sand chlorinator reactor into a residue and chlorinator off gases of zirconium chloride and silicon chloride which employs a filter assembly of the present invention so that the gaseous zirconium chloride can subsequently be de-sublimed into a solid zirconium chloride without using seed material;
  • Figure 3 is a perspective view of a filter assembly of the present invention disposed within a primary filter plenum;
  • Figure 4 is a perspective view of a filter element of the filter assembly shown in Figure 3;
  • Figure 5 is a cross-sectional side view in elevation of the filter element taken along line 5-5 in Figure 4;
  • Figure 6 is a top plan view of the filter element shown in Figure 4;
  • Figure 7 is a bottom plan view of the filter element shown in Figure 4;
  • Figure 8 is an enlarged cross-sectional view of one of the filter elements disposed in a support structure which is taken along line 8-8 in Figure 3;
  • Figure 9 is a graph reflecting the improved dust collection efficiency of the filter assembly of the present invention that employs porous carbon filter elements as compared to prior art filter assemblies that employ cloth bag filter elements;
  • Figure 10 is a side view in elevation of a de-sublimation apparatus cut away to show its internal structure as well as the fluids and the direction of fluid flow therewithin;
  • Figure 11 is a cross-sectional side view in elevation of the sublimation apparatus centrally mounted onto a top of a condenser showing its internal structure as well as the fluids and direction of fluid flow of fluids therewithin;
  • Figure 12 is a bottom plan view of the sublimation apparatus.
  • Figure 13 is a cross-sectional view of the sublimation apparatus along line 13-13 in Figure 11.
  • a filter assembly of the present invention is adapted for use in combination with a plenum connected in fluid communication with a chlorinator reactor that contains suspended particulate solids and is operative for reducing zircon sand into a residue and chlorinator off gases of zirconium chloride and silicon chloride.
  • a chlorinator reactor that contains suspended particulate solids and is operative for reducing zircon sand into a residue and chlorinator off gases of zirconium chloride and silicon chloride.
  • the filter assembly of the present invention is fabricated from a porous carbon material, the filter assembly of the present invention is particularly useful in high temperature and/or highly corrosive environments. Furthermore, although the detailed description of the filter assembly of the present invention describes the filter assembly as having a plurality of filter elements, a skill artisan would appreciate that a single filter element could also be practiced without departing from the inventive concepts herein described.
  • a first exemplary embodiment of a filter assembly 40 of the present invention is generally introduced in Figures 2 - 8.
  • filter assembly 40 is used in combination with primary filter plenum 14 connected in fluid communication with sand chlorinator reactor 8 which contains suspended particulate solids and is operative for reducing zircon sand, ZrSi0 4 , into residue and chlorinator off gases.
  • the chlorinator off gases are zirconium chloride, ZrCl 4 , and silicon chloride, SiCl 4 .
  • Filter assembly 40 is adapted for use to separate the chlorinator off gases from the suspended particulate solids and includes a filter structure in a form of a plurality of filter elements 42 and a support structure 44.
  • Each of filter elements 42 is fabricated from a porous carbon material.
  • a porous carbon filter material was selected for the first embodiment of filter assembly 40 of the present invention with properties listed in Table 1 below.
  • each of filter elements 42 has an elongated, cylindrically-shaped body member 46 and a flange 48.
  • Body member 46 extends longitudinally along and centrally about a longitudinal axis "A" between a first end 50 and an opposite second end 52.
  • Flange 48 is annularly-shaped and extends radially from longitudinal axis "A" and around first end 50.
  • First end 50 defines an opening 54 into a cylindrically-shaped bore 56 which is centrally disposed about longitudinal axis "A”. Bore 56 extends into body member 46 and terminates proximate to second end 52.
  • support structure 44 includes a plate 58 which is fabricated from a stiff, corrosion-resistant material such as stainless steel.
  • Plate 58 is sized and adapted to be disposed and secured in an interior 60 of primary filter plenum 14 to define an upstream plenum region 62 in fluid communication with sand chlorinator reactor 8 and a downstream plenum region 64.
  • a support beam 65 is connected to primary filter plenum 14 in interior 60 and plate 58 is releasably fastened to support beam 65 by a conventional bolt and nut set 67, although other types of conventional fasteners could be used in lieu thereof.
  • Plate 58 has a flat first surface 66 facing into downstream plenum region 64 and a flat second surface 68 oriented opposite and parallel to first surface 56 and facing into the upstream plenum region 62.
  • An array of holes 70 are formed through plate 58 between first and second surfaces 66 and 68. Each of holes 70 is sized and adapted to slidably receive a respective one of filter elements 42.
  • Support structure 44 is operative to releasably retain filter elements 42 to plate 58 in a manner so that, when the suspended particulate solids and chlorinator off gases are urged as a result of a pressure differential between sand chlorinator reactor 8 and downstream plenum region 64 to move into primary filter plenum 14 from sand chlorinator reactor 8, the chlorinator off gases in upstream plenum region 62 are permitted to pass through the plurality of filter elements 42 and into downstream plenum region 64. Simultaneously therewith, the suspended particulate solids in upstream plenum region 62 are prevented from passing through filter elements 42 and into downstream plenum region 64 thereby separating the chlorinator off gases from the suspended particulate solids.
  • Each of filter elements 42 includes a collar 72 connecting flange 48 and body member 46.
  • Collar 72 has an outer collar surface 74 tapering from an outer peripheral surface 78 of flange 48 towards an outer body surface 76 of body member 46.
  • Outer collar surface 74 tapers at an angle "a", best shown in Figure 8, relative to longitudinal axis "A” between outer peripheral surface 78 of flange 48 and outer body surface 76 of body member 46.
  • angle "a” is equal to 45°, angle "a” can be selected in a range of 35° and 55°.
  • support structure 44 includes a plurality of retaining devices 80 which are operative to releasably retain respective ones of filter elements 42 to plate 58.
  • Each retaining device 80 has a retainer element 82 formed with an aperture 84 therethrough and a pair of fasteners 86.
  • retainer element 82 is a rigid disk with a pair of fastener holes formed therethrough and the pair of fasteners 86 are conventional threaded bar and nut sets.
  • each of the threaded bars is advanced into plate 58 while an opposite end of each of the threaded bars matably engages respective ones of the nuts to secure retainer element 82 through its fastener holes over respective ones of filter elements 42 and to plate 58.
  • Retainer element 82 is sized and adapted to extend across first end 50 and flange 48 of a respective one of filter elements 42.
  • Aperture 84 is sized and adapted to register with bore 56 of respective ones of filter elements 42.
  • a shroud 88 depends downwardly from retainer element 82 and radially equidistantly from longitudinal axis "A".
  • Shroud 88 is sized to cover outer peripheral surface 78 of flange 48 when retainer element 82 is releasably interconnected to plate 58.
  • the pair of fasteners 86 are operative to releasably interconnect respective ones of retainer elements 82 to plate 58 when retainer element 82 is placed over and across first end 50 and flange 48 of filter element 42 with aperture 84 in registration with bore 56 thereby releasably retaining filter element 42 to plate 58.
  • Being able to releasably interconnect filter elements 42 to plate 58 affords easy and simple installation of individual ones of filter elements 42 to plate 58.
  • support structure 44 includes a plurality of annular support members 90.
  • Each of support members 90 is disposed concentrically about a respective one of holes 70 and is connected to plate 58. Also, each of support members 90 has an inner wall 92 which defines a frustoconically-shaped bore 94. When respective ones of filter elements 42 are slidably received into respective ones of holes 70, inner wall 92 and outer collar surface 74 are facially opposing each other. Respective ones of inner walls taper at angle “b" relative to longitudinal axis "A" when respective ones of filter elements 42 are slidably received into respective holes 70 so that inner walls 92 and outer collar surfaces 74 can facially oppose each other. Although it is preferred that angle “b” equals 45°, angle “b” can be selected from a range between range of 35° and 55°. A skilled artisan would appreciate that in order for respective ones of inner walls 92 to facially opposed respective ones of outer collar surfaces 74, angle “a” and angle “b” are equal.
  • Filter assembly 40 of the present invention includes a plurality of frustoconically-shaped ring seals 94, gasket elements 96 and weave spring elements 98.
  • Each ring seal 94 is sized and adapted to be interposed between respective ones of inner walls 92 and outer collar surfaces 74 when filter elements 42 are slidably received into respective ones of holes 70.
  • Each gasket element 96 has a gasket opening 100 formed therethrough. Gasket element 96 is sized and adapted to be interposed between respective ones of retainer elements 82 and first ends 50 of filter elements 42. When interposed, gasket opening 100 registers with respective ones of bores 56 and apertures 84 when retaining devices 80 releasably retain respective ones of filter elements 42 to plate 58.
  • Each weave spring element 98 has a centrally-disposed port 102 formed therethrough and is sized and adapted to be interposed between retainer element 82 and gasket element 96. When interposed, port 102 registers with aperture 84 and gasket opening 100 when respective ones of filter elements 42 are slidably received into respective ones of holes 70. Ring seals 94, gasket elements 96 and weave spring elements 98 are employed to seal filter assembly 40 in a manner so that leakage of suspended particulate solids from upstream plenum region to the downstream plenum region is minimized.
  • Filter assembly 40 of the present invention with porous carbon filter elements 42 was secured in interior 60 of primary filter plenum 14 and the process was implemented. Empirical tests were conducted to compare the dust collection efficiency of porous carbon filter elements with cloth bag filter elements. Thorium was measured in the solid zirconium chloride taken from chloride receptacles as the standard by which to determine dust collection efficiency. Results of these empirical tests are shown in Figure 9 and plotted as a function of temperature. In all instances, the porous carbon filter elements proved to be an improvement in dust collection efficiency as compared to cloth bag filters. As mentioned above, the porous carbon material employed for the present invention resists accumulation of the suspended particulate solids on outer surfaces of the porous carbon filter elements disposed in the downstream plenum region.
  • porous carbon filter material is a ceramic-like, it is extremely more durable than cloth bag filter elements. Installation of the porous carbon filters is also easier.
  • the ceramic properties of the porous carbon filter elements allow the process to operate at higher temperatures. In fact, cooler 12 employed in the prior art process of Figure 1 is no longer needed for the new and improved process of Figure 2. Since there is now limited risk of fire, zirconium chloride production can be increased by using higher process temperatures. Again, because of the ceramic properties of the porous carbon filter elements, many harsh corrosive environments have little detrimental effects to the performance of the porous carbon filter elements.
  • porous carbon filter elements could be used in other harsh environment processes that employ oxidizer reactors which might reduce a substance to oxidizer off gases and residue.
  • Figures 1 and 2 other structural differences between the prior art zirconium chloride production process ( Figure l) and the new and improved process of the present invention ( Figure 2) are different filter assemblies and the incorporation of a de-sublimation apparatus 210 shown in Figure 2.
  • a major advantage of incorporating de-sublimation apparatus 210 into the production process is the elimination of seed material from the feed stock which is discussed in further detail below.
  • a second exemplary embodiment of a filter assembly 40 used in combination with a de-sublimation apparatus 210 is generally introduced in Figures 10 - 13.
  • de-sublimation apparatus 210 is used in combination with primary filter plenum 14 that incorporates a porous carbon filter assembly 40 therein.
  • Primary filter plenum 14 is connected downstream of and in fluid communication with sand chlorinator reactor 8 which contains suspended particulate solids and is operative for reducing zirconium silicon sand into a residue and chlorinator off gases of zirconium chloride and silicon chloride.
  • De-sublimation apparatus 210 is connected downstream of and in fluid communication with porous carbon filter assembly 40 and is adapted for use to de-sublime the gaseous zirconium chloride into a solid zirconium chloride. Shown in Figures 10 - 13, de-sublimation apparatus 210 includes an inner cooler device 212, an outer cooler device 214, an inlet 216 and an annular outlet 218.
  • Inner cooler device 212 includes an elongated tubular member 220 having an outer cylindrical surface 222.
  • Tubular member 220 extends along a vertical longitudinal axis "A'".
  • Inner cooler device 212 is operative to cool outer cylindrical surface 222.
  • Outer cooler device 214 has an inner cylindrical surface 224 concentrically surrounding outer cylindrical surface 222 of tubular member 220 in a spaced apart relationship to define an annularly-shaped conduit 226 therebetween.
  • Outer cooler device 214 is operative to cool inner cylindrical surface 224.
  • Inlet 216 enters into annularly-shaped conduit 226 and is disposed at an upper portion 228 of annularly-shaped conduit 226 as shown in Figure 11.
  • Inlet 216 is adapted to convey chlorinator off gases (represented as solid-line arrows) from porous carbon filter assembly 40 and into upper portion 228 of annularly-shaped conduit 226.
  • Annular outlet 218 exits from annularly-shaped conduit 226 and is disposed at a bottom portion 230 of annularly-shaped conduit 226.
  • Chlorinator off gases enters into annularly-shaped conduit 226 through inlet 216 and swirls downwardly while contacting cooled outer cylindrical surface 222 of tubular member 220 and cooled inner cylindrical surface 224 of outer cooler device 214 along annularly-shaped conduit 226 thereby causing gaseous zirconium chloride of chlorinator off gases to de-sublime into solid zirconium chloride (represented by dots) before the solid zirconium chloride and remaining chlorinator off gases exit annularly-shaped conduit 226 from annular outlet 218.
  • gaseous zirconium chloride of chlorinator off gases to de-sublime into solid zirconium chloride (represented by dots) before the solid zirconium chloride and remaining chlorinator off gases exit annularly-shaped conduit 226 from annular outlet 218.
  • the various arrow legends indicate different types of fluids and the direction in which the arrows point is the direction of the fluid flow for that particular fluid.
  • Annular outlet 218 is disposed at and defined by an outer bottom peripheral end 232 of tubular member 220 and an inner bottom peripheral end 234 of inner cylindrical surface 224 of outer cooler device 214.
  • inlet 216 is oriented in a manner whereby the chlorinator off gases (solid-line arrows) enter annularly-shaped conduit 226 transversely of vertical axis "A'" and tangentially to a radius "r" extending from vertical axis "A" 1 .
  • the chlorinator off gases enter annularly-shaped conduit 226 in this manner to cause it to swirl therewithin, thereby creating a cyclone effect around and through annularly-shaped conduit 226. It is theorized that this cyclone effect contributes to effective de-sublimation of the gaseous zirconium chloride.
  • Tubular member 220 includes an elongated cylindrically-shaped inner cooler chamber 234 formed thereinto.
  • Inner cooler device 212 includes an inner cooler inlet 236 and an inner cooler outlet 238.
  • Inner cooler inlet 236 is in fluid communication with inner cooler chamber 234 so that an inner cooling fluid (represented by double-dashed arrows) can be conveyed into inner cooler chamber 234.
  • inner cooling fluid is cool, forced air produced from any conventional source.
  • Inner cooler outlet 238 is in fluid communication with inner cooler chamber 234 so that the inner cooling fluid can be conveyed from inner cooler chamber 234.
  • Inner cooler inlet 236 and inner cooler outlet 238 are located at a top location 240 of inner cooler device 212.
  • inner cooler device 212 includes a tube 242 which is disposed within inner cooler chamber 234 and extends from and is in fluid communication with inner cooler inlet 236 toward a bottom location 244 of inner cooler chamber 234 as illustrated in Figures 10 and 11.
  • Outer cooler device 214 includes an outer cooler inlet 246, an outer cooler outlet 248 and an annularly-shaped outer cooler chamber 250 formed into outer cooler device 214.
  • Outer cooler chamber 250 is in fluid communication with outer cooler inlet 246 so that an outer cooling fluid (represented by single-dashed arrows) can be conveyed into outer cooler chamber 250 and with outer cooler outlet 248 so that the outer cooling fluid can be conveyed from outer cooler chamber 250.
  • outer cooling fluid is cool, forced air produced from any conventional source including the same one used to produce the inner cooling fluid.
  • Outer cooler device 214 also includes a bulkhead 252 that depends downwardly from a top portion 254 of outer cooler device 214 and is disposed concentrically within outer cooler chamber 250 thereby dividing outer cooler chamber 250 into a first outer cooler chamber region 256 and a second outer cooler chamber region 258.
  • Second outer cooler chamber region 258 is in fluid communication with first outer cooler chamber region 256 at a bottom portion 260 of outer cooler chamber 250.
  • Outer cooler inlet 246 is in fluid communication with first outer cooler chamber region 256 so that the outer cooling fluid can be conveyed into outer cooling chamber 250.
  • Outer cooler outlet 248 is in fluid communication with second outer cooler chamber region 258 so that the outer cooling fluid can be conveyed from outer cooling chamber 250.
  • Outer cooler inlet 246 and outer cooler outlet 248 are located proximate top portion 254 of outer cooler device 214.
  • de-sublimation apparatus 210 is adapted to mount to primary condenser 24.
  • Primary condenser 24 with condenser chamber 26 formed therein is in downstream fluid communication with de-sublimation apparatus 210.
  • At least a bottom section 262 of de-sublimation apparatus 210 extends vertically into condenser chamber 26. It is preferred that de-sublimation apparatus 210 is mounted to primary condenser 24 so that it is positioned in a top center location thereof.
  • the remaining chlorinator off gases are conveyed from primary condenser 24 to secondary condenser 30.
  • some of the remaining gaseous zirconium chloride de-sublimes in secondary condenser chamber 34 of secondary condenser 30.
  • the solid zirconium chloride is then transferred to a second chloride receptacle 28' while the chlorinator off gases remaining in secondary condenser 30 is transferred through a second filter assembly 42' of the present invention employing porous carbon filter elements 42' and discarded as an effluent, primarily in a form of silicon chloride, as shown.
  • feedstock 2 for the production process is zircon sand, ZrSi0 4 .
  • feedstock 2 for the production process is zircon sand, ZrSi0 4 .
  • seed material can now be eliminated from the production process of the present invention.
  • a direct benefit of eliminating seed material from the production process is that waste which is naturally generated as a result of making zirconium chloride can be reduced.
  • the filter assembly of the present invention requires less frequent back purging than cloth bag filter assemblies and the de-sublimation apparatus produces adequately dense solid zirconium chloride that tends to decrease the frequency of clogging of the primary condenser. As a result, production rate of zirconium chloride is increased and operational down time is decreased. Cost of lost production opportunity and maintenance for cleaning clogged condensers is reduced.
  • the first step of this new and improved process is conveying a zircon sand into a chlorinator reactor containing suspended particulate solids. Then, the next step is subjecting the zircon sand to gaseous chlorine in order to reduce the zircon sand to residue and chlorinator off gases of zirconium chloride and silicon chloride which become entrained with the suspended particulate solids in the chlorinator reactor. The next step is filtering the chlorinator off gases from the suspended particulate solids through a porous carbon filter assembly at high temperature.
  • the last step is de-subliming the filtered gaseous zirconium chloride without the addition of seed material into a solid zirconium chloride at sufficiently high temperatures to prevent contamination of the particulate zirconium chloride product with silicon tetrachloride. It is preferred that this process include the de-sublimation apparatus as described above. Accordingly, the present invention has been described with some degree of particularity directed to the exemplary embodiments of the present invention. It should be appreciated, though, that the present invention is defined by the following claims construed in light of the prior art so that modifications or changes may be made to the exemplary embodiments of the present invention without departing from the inventive concepts contained herein.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Filtering Materials (AREA)

Abstract

La présente invention concerne un ensemble filtrant destiné à être utilisé avec une chambre en communication fluide avec un réacteur de chloruration, lequel sert à transformer du sable de zircon en un résidu et en gaz de réaction, à savoir, du chlorure de zirconium et du chlorure de silicium, de sorte que lesdits gaz, qui sont entraînés avec les particules solides en suspension, soient séparées de ces derniers. L'ensemble filtrant se compose d'une structure filtrante composée de plusieurs éléments filtrants et d'une structure support. Chacun des éléments filtrants est fait d'un matériau en carbone poreux. La structure support est constituée d'une plaque en matériau rigide et résistant à la corrosion, laquelle plaque est dimensionnée et conçue pour être placée et fixée à l'intérieur de la chambre. La plaque est perçée de trous. Chaque trou est dimensionné et conçu pour accueillir à coulissement un élément filtrant. La structure support retient de manière libérable les éléments filtrants de façon que, lorsque les particules solides en suspension et les gaz de réaction sont poussés dans la chambre depuis le réacteur de chloruration, ces gaz traversent les éléments filtrants, alors que les particules solides en suspension étant incapables de traverser ces éléments filtrants. La présente invention s'utilise également conjointement avec un condensateur de désublimation, notamment pour désublimer en chlorure de zirconium solide un chlorure de zirconium gazeux. L'invention concerne également un procédé innovant de production de chlorure de zirconium solide à partir de sable de plage sans utilisation de matériau d'ensemencement.
PCT/US1996/008286 1995-06-05 1996-06-05 Ensemble filtrant au carbone poreux pour le traitement du chlorure de zirconium Ceased WO1996039241A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US46444495A 1995-06-05 1995-06-05
US08/464,444 1995-06-05

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WO1996039241A1 true WO1996039241A1 (fr) 1996-12-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114426309A (zh) * 2022-02-17 2022-05-03 沈阳鑫博工业技术股份有限公司 一种制备四氯化锆的沸腾加热方法及沸腾加热炉
EP4545164A1 (fr) * 2023-10-25 2025-04-30 Scheuch Management Holding GmbH Installation de filtration de gaz chaud pour filtrer des gaz d'échappement

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59127618A (ja) * 1983-01-06 1984-07-23 Matsushita Electric Ind Co Ltd ハニカム状フイルタの製造法
EP0237142A2 (fr) * 1986-01-10 1987-09-16 Westinghouse Electric Corporation Procédé pour filtrer des courants gazeux à haute température
WO1988003834A1 (fr) * 1986-11-18 1988-06-02 Westinghouse Electric Corporation Unite de filtration utilisee a des temperatures elevees
US4812149A (en) * 1987-12-03 1989-03-14 Westinghouse Electric Corp. Hot inert gas purging for filter blowback process
WO1989010897A1 (fr) * 1988-05-06 1989-11-16 Sommers James A Halogenures ultra-pures et leur preparation
US5171549A (en) * 1991-05-22 1992-12-15 Teledyne Wah Chang Albany Process for decreasing the level of impurities in zirconium chloride, titanium chloride and hafnium chloride

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59127618A (ja) * 1983-01-06 1984-07-23 Matsushita Electric Ind Co Ltd ハニカム状フイルタの製造法
EP0237142A2 (fr) * 1986-01-10 1987-09-16 Westinghouse Electric Corporation Procédé pour filtrer des courants gazeux à haute température
WO1988003834A1 (fr) * 1986-11-18 1988-06-02 Westinghouse Electric Corporation Unite de filtration utilisee a des temperatures elevees
US4812149A (en) * 1987-12-03 1989-03-14 Westinghouse Electric Corp. Hot inert gas purging for filter blowback process
WO1989010897A1 (fr) * 1988-05-06 1989-11-16 Sommers James A Halogenures ultra-pures et leur preparation
US5171549A (en) * 1991-05-22 1992-12-15 Teledyne Wah Chang Albany Process for decreasing the level of impurities in zirconium chloride, titanium chloride and hafnium chloride

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Week 8435, Derwent World Patents Index; AN 84-216757, XP002016039 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114426309A (zh) * 2022-02-17 2022-05-03 沈阳鑫博工业技术股份有限公司 一种制备四氯化锆的沸腾加热方法及沸腾加热炉
CN114426309B (zh) * 2022-02-17 2024-02-02 沈阳鑫博工业技术股份有限公司 一种制备四氯化锆的沸腾加热方法及沸腾加热炉
EP4545164A1 (fr) * 2023-10-25 2025-04-30 Scheuch Management Holding GmbH Installation de filtration de gaz chaud pour filtrer des gaz d'échappement
WO2025088089A1 (fr) * 2023-10-25 2025-05-01 Scheuch Management Holding GmbH Système de filtration de gaz chaud pour filtrer des gaz de combustion

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