SPARGE FOR A HIGH-PRESSURE VESSEL

Abstract

A sparge for use in a high-pressure vessel operated at elevated temperatures and having high energy agitators for suspending mineral containing particles in a slurry. The sparge injects reagent fluids into the slurry to reduce reaction times and for controlling process parameters for extracting valuable minerals from the particles. The sparge has a vapor lock to inhibit the flow of particulate material and detritus material under low or no fluid flow situations which occur commonly in the operation of high pressure autoclaves. The sparge has a fluid flow path that increases in cross-sectional area in the direction of flow of reagent fluids so as to keep reagent fluids flowing at a velocity below a critical impingement velocity that can cause metal materials of the sparge to either wear rapidly, combust and in the worst case lead to loss of containment and violent and rapid depressurization of the high pressure vessel.

Claims

1. A high-pressure vessel for extracting valuable minerals from mineral bearing particles, the high-pressure vessel comprising: a substantially cylindrical horizontally disposed reaction chamber for containing a slurry of the mineral bearing particles at elevated pressure and elevated temperature, the reaction chamber having an inlet at one end for receiving the particles and an outlet at its opposite end for delivering processed particles; a plurality of high energy agitators disposed within the reaction chamber, the agitators being distributed along the length of the reaction chamber for stirring the slurry and distributing reagent fluids; and at least one sparge disposed proximate a respective one of the agitators, and each sparge comprising: a pipe with its free end disposed within the slurry for injecting the reagent fluids into the slurry; and a vapor lock means disposed about the free end of the pipe, the vapor lock means comprising a downwardly disposed outlet whose cross-sectional flow area is: larger than the cross-sectional flow area of the free end of the pipe, to reduce the flow rate of the reagent fluids to reduce wear and to avoid combustion; and less than 5% of the area swept by the corresponding agitator to avoid backflow of slurry materials into the free end of the pipe during conditions of low or no fluid flow through the said pipe and due to turbulence of the slurry caused by the operation of the agitators wherein the cross-sectional area of the path of the flow of fluid (the “fluid flow path”) through the pipe and the vapor lock means increases in the direction of flow of the reagent fluids.

2. A process for operation of a high pressure autoclave for extracting valuable minerals from mineral bearing particles suspended in a slurry in a reaction chamber having a plurality of high energy agitators and at least one sparge associated with each agitator, each sparge comprising a pipe with its free end disposable within the slurry and a vapor lock means located about the free end of the pipe, the vapor lock means comprising a downwardly disposed outlet whose cross-sectional flow area is larger than the cross-sectional flow area of the free end of the pipe, and less than 5% of the area swept by the corresponding agitator, and, wherein the cross-sectional area of the path of the flow of fluid (the “fluid flow path”) through the pipe and the vapor lock means increases in the direction of flow of the reagent fluids, the process comprising the steps of: substantially filling the reaction chamber with liquid and the mineral bearing particles; heating the slurry to an elevated temperature and pressurizing the reaction chamber to an elevated pressure, to reduce reaction times and to control process parameters for extracting the valuable minerals; mixing the liquid and the particles with the agitators to agitate the slurry; injecting reagent fluids into the reaction chamber, proximate the agitators, with the sparges, the flow of reagent fluids being downward into the slurry through the outlet; dispersing the reagent fluids into the slurry with the agitators and reducing the rate of flow of the reagent fluids inside the pipe towards the outlet in the direction of said flow by making the cross-sectional flow area of the outlet larger than the cross-sectional flow area of the pipe; and inhibiting backflow of the slurry into the vapor lock means, during conditions of low or no flow of the reagent fluid through said pipe, by making the cross-sectional flow area of the outlet less than 5% of the area swept by the corresponding agitator.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0056] Exemplary embodiments of the present invention will now be described with reference to the accompanying drawing, in which:

[0057] FIGS. 1 to 6 are cross-sectional views of a portion of a conventional high-pressure autoclave showing prior art sparge configurations, for which exemplary embodiments of the present invention are shown in FIGS. 7 to 18, respectively;

[0058] FIGS. 1 and 2 are cross-sectional views of a portion of a conventional high-pressure autoclave with a prior art bottom entry sparge, FIG. 2 is shown at a smaller scale and showing the sparge in relation to an agitator;

[0059] FIG. 3 is a cross-sectional view of the prior art high pressure autoclave of FIG. 1 and FIG. 2 shown at a still smaller scale;

[0060] FIGS. 4 and 5 are cross-sectional views of two differing orientations of top entry prior art autoclave sparges. FIG. 4 shows a top entry sparge with a vertically up sparge pipe free/discharge end located beneath the agitator and FIG. 5 shows a top entry sparge with a horizontal sparge pipe free/discharge end located beneath the agitator;

[0061] FIG. 6 is a cross-sectional view of a side entry prior art sparge with a horizontal sparge pipe free/discharge end located above the agitator;

[0062] FIGS. 7 and 8 are cross-sectional end views of a portion of a high-pressure autoclave with a bottom entry sparge in accordance with one embodiment of the present invention. FIG. 8 is shown at a smaller scale and showing the sparge in relation to an agitator and showing a vapor lock means mounted on a sparge pipe;

[0063] FIG. 9 is a cross-sectional end view of the high-pressure autoclave of FIGS. 7 and 8 shown at a still smaller scale;

[0064] FIG. 10 is a cross-sectional side view of the sparge of FIG. 7 shown in isolation;

[0065] FIGS. 11 and 12 are cross-sectional end views of a portion of a high-pressure autoclave with a bottom entry sparge in accordance with another embodiment the present invention, FIG. 12 is shown at a smaller scale and showing the sparge in relation to an agitator and showing a vapor lock means mounted on the agitator;

[0066] FIG. 13 is a cross-sectional end view of the high-pressure autoclave of FIGS. 11 and 12 shown at a still smaller scale;

[0067] FIG. 14 is a cross-sectional end view of a portion of a high-pressure autoclave with a top entry sparge in accordance with still another embodiment of the present invention;

[0068] FIG. 15 is a cross-sectional end view of the high-pressure autoclave of FIG. 14 shown at a smaller scale;

[0069] FIG. 16 is a cross-sectional end view of a portion of a high-pressure autoclave with a side entry sparge in accordance with yet another embodiment of the present invention;

[0070] FIG. 17 is cross-sectional end view of the high-pressure autoclave of FIG. 16 shown at a smaller scale;

[0071] FIG. 18 is an end perspective view of one cell of a high-pressure autoclave shown with the bottom entry sparge of FIG. 7 shown in relation to an agitator; and

[0072] FIG. 19 is a perspective view, seen from above, of a high-pressure autoclave having 6 cells and one sparge of the present invention associated with each cell.

PRIOR ART

[0073] In FIGS. 1 to 3 there is shown a high-pressure vessel in the form of a high-pressure autoclave 10 with a conventional bottom entry sparge 12 installed in a flange 14 of the autoclave commonly known in the art. The autoclave 10 also typically has an agitator 16 for stirring a slurry comprising mineral bearing ore and a reagent liquid (typically a strong acid). The autoclave 10 typically has 4-8 cells (in similar manner to the six cells shown in FIG. 19), each with one sparge 12 and one agitator 16. The sparge 12 has the limitation that it is prone to blockage with slurry materials when the flow of fluid into the autoclave 10 via the sparge 12 is low or ceases.

[0074] FIGS. 7 to 17 show sparges 20, 40, 60 and 80, in accordance with several embodiments of the present invention each of which have the advantage that backflow of slurry materials into a sparge pipe is inhibited by the use of a vapor lock means. Each embodiment shall now be described in some detail, and like numerals denote like parts.

DETAILED DESCRIPTION

[0075] In FIGS. 7 to 9 there is shown a bottom entry sparge 20 comprising a sparge pipe 22 with a free end 24 disposed within a high-pressure autoclave 26 through a flange 28. The sparge 20 also comprises apertures 29, located in the end of the sparge pipe 22 and about which is disposed an overhung, inverted cap 30. The inverted cap 30 is disposed facing downwardly such that mineral bearing particles under agitation in the autoclave 26 cannot settle or fall under the force of gravity into the sparge pipe 22. The inverted cap 30 forms an annular outlet 32 with the free end 24 of the sparge pipe 22.

[0076] The sparge pipe 22 could be disposed into the autoclave 26 from below, to the side or from above the agitator 16, provided the fluids exiting the sparge pipe 22 are proximate one of the agitators 16 and distributable via the agitators 16 to increase the speed of process reactions or the desired process conditions change. To ensure that a vapor lock is achieved, it is essential that the outlet 32 be oriented such that mineral bearing material and refractory brick detritus materials cannot fall or settle under the action of gravity into the sparge pipe 22.

[0077] Preferably, the cross-sectional area of the apertures 29 is greater than the cross-sectional area of the inside of the sparge pipe 22, so as to prevent an increase in velocity of fluids flowing into the autoclave 26 via the sparge 20.

[0078] Typically, the autoclave 26 is generally cylindrical with domed ends. Typically, the autoclave 26 is disposed substantially horizontally, although it could be disposed vertically.

[0079] Typically, the autoclave 26 is lined with refractory bricks or a metal alloy that is chemically resistant, to protect the metal outer layer of the autoclave 26 from the temperatures and corrosive materials contained within the autoclave 26 when in operation.

[0080] Conveniently the sparge 20 also has a diffusion ring or plate 34 disposed about the pipe 22 at the outlet 32 to ensure that the flow of denser fluids, such as cooling water, out of the sparge 20 are directed radially away from the pipe 22 rather than axially downward along the pipe 22. The diffusion ring 34 addresses the potential for localized cooling or high concentrations of reagents at the bottom of the autoclave 26 and aids dispersion to assist mixing and reaction processes.

[0081] Conveniently, the sparge 20 may have a protective coating over some or all of its wetted external surface. For example, the sparge 20 may have a ceramic metal spray coating, or a sheath outer layer or be clad to protect against the effects of corrosion and/or erosion otherwise caused by contact with corrosive and/or abrasive autoclave fluids entering via the sparge pipe 22.

[0082] Preferably, the annular outlet 32 is greater in cross sectional area than the cross-sectional area of the apertures 29—so as to prevent an increase in velocity of fluids flowing into the autoclave 26 via the sparge 20.

[0083] The free end 24, the apertures 29, the inverted cap 30 and the annular outlet 32 together constitute the vapor lock means of the present invention in this bottom entry configuration embodiment. The vapor lock is created when the flow of sparge fluids out of the outlet 32 ceases. Under such conditions the pressure of the fluids within the sparge pipe 22 are the same as the pressure of the fluids within the autoclave 26. Accordingly, there can be no fluid flow back into the sparge pipe 22. Also, there can be no flow of particles under the force of gravity since the apertures 29 are above the annular outlet 32.

[0084] FIG. 10 shows the vapor lock means of the present invention to a larger scale. The vapor lock means is constituted by the free end 24 of the sparge pipe 22, the apertures 29, the inverted cap 30 and the annular outlet 32 formed between the inverted cap 30 and the diffusion ring 34. The cross-sectional area of the annular outlet 32 is greater than the cross-sectional area of the apertures 29, which are in turn greater than the cross-sectional area of the sparge pipe 22.

[0085] The inverted cap 30 is conveniently threadedly attached to the end 24 of the sparge pipe 22. It is essential that the thread be of such a length and pitch that fluids cannot flow along the thread between the inverted cap 30 and the end 24, as such flow would permit slurry to enter into and block the sparge 20 and this would compromise the vapor lock means.

[0086] In FIGS. 9, 13, 15 and 17 the typical level of slurry contained within the autoclave 26 is shown and denoted with numeral 36 and referred to as the slurry level 36.

[0087] In FIGS. 11 to 13 there is shown a bottom entry sparge 40, which is similar to the bottom entry sparge 20, with like numerals denoting like parts.

[0088] The sparge 40 differs from the sparge 20 in that the sparge 40 has an overhung inverted cap 42 mounted onto the agitator 16 and disposed about a free end 44 of the sparge pipe 22 to form the outlet 32. In this manner, the inverted cap 42 rotates with the agitator 16 and is not attached in any way to the sparge pipe 22. Also, the free end 44 of the sparge pipe 22 includes only a single aperture 46, although multiple apertures akin to the apertures 29 could be provided.

[0089] The free end 44, the aperture 46, the inverted cap 42 and the annular outlet 32 together constitute the vapor lock means of the present invention. The vapor lock is created when the flow of sparge fluids out of the outlet 32 ceases. Under such conditions the pressure of the fluids within the sparge pipe 22 are the same as the pressure of the fluids within the autoclave 26. Accordingly, there can be no fluid flow back into the sparge pipe 22. Also, there can be no flow of particles under the force of gravity since the aperture 46 is above the annular outlet 32.

[0090] In FIGS. 14 and 15 there is shown a top entry sparge 60, which is similar to the sparge 20, with like numerals denoting like parts.

[0091] The sparge 60 differs from the sparge 20 in that the sparge 60 does not have an inverted cap. The sparge 60 has a sparge pipe 62 which enters the autoclave 26 from above or to the side of the agitator 16 and terminates at an end plate 64 which is disposed downwardly. The sparge pipe 62 differs from the sparge pipe 22 in that it has an elbow 65 proximate its free end. The sparge pipe 62 has apertures 66, conveniently in the form of flutes, disposed above the end plate 64. The cross-sectional area of the apertures 66 is preferably greater than the cross-sectional area of the sparge pipe 62 so as to avoid increasing the speed of the fluids delivered by the sparge pipe 62 into the autoclave 26. The end plate 64 is equivalent to the diffusion ring 34.

[0092] The sparge 60 also differs from the sparge 20 in that it does not have an annular outlet. In this embodiment, the apertures 66 form an outlet for the flow of sparge fluids. Also, the apertures 66 are disposed so that mineral bearing material and refractory brick detritus materials cannot fall under the action of gravity into the sparge pipe 62.

[0093] The sparge pipe 62 could be disposed into the autoclave 26 from the side or from above the agitator 16, provided the fluids exiting the sparge pipe 62 are proximate one of the agitators 16 and distributable via the agitators 16 to increase the speed of process reactions. Also, it is essential that the outlet 32 be directed downwardly so that mineral bearing material and refractory brick detritus materials cannot fall under the action of gravity into the sparge pipe 22.

[0094] The end plate 64, the elbow 65 and the apertures 66 together constitute the vapor lock means of the present invention. The vapor lock is created when the flow of sparge fluids out of the apertures 66 ceases. Under such conditions the pressure of the fluids within the sparge pipe 62 are the same as the pressure of the fluids within the autoclave 26. Accordingly, there can be no fluid flow back into the sparge pipe 62. Also, there can be no flow of particles under the force of gravity since the apertures 66 are below the level of the elbow 65 and the rest of the sparge pipe 62.

[0095] In FIGS. 16 and 17 there is shown a side entry sparge 80, which is similar to the sparge 20, with like numerals denoting like parts.

[0096] The sparge 80 differs from the sparge 20 in that it has a sparge pipe 82 disposed substantially horizontally into the autoclave 26. The sparge pipe 82 terminates at a blank end 84. The sparge pipe 82 also has an opening 86 in its lower extent for the egress of sparge fluids. The opening 86 is disposed to inhibit the ingress of mineral bearing material and refractory brick detritus materials falling under the action of gravity into the sparge pipe 82.

[0097] The blank end 84 and the opening 86 together constitute the vapor lock means of the present invention. The vapor lock is created when the flow of sparge fluids out of the opening 86 ceases. Under such conditions the pressure of the fluids within the sparge pipe 82 are the same as the pressure of the fluids within the autoclave 26. Accordingly, there can be no fluid flow back into the sparge pipe 82. Also, there can be no flow of particles under the force of gravity since the opening 86 is disposed downwardly and below the level of the remainder of the sparge pipe 82.

[0098] Conveniently, like the sparge 20, the sparges 40, 60 and 80 can have a protective coating over its entire wetted external surface. For example, the sparges 40, 60 and 80 may have a ceramic metal spray coating, or a sheath outer layer or be clad to protect against the effects of corrosion and/or erosion otherwise caused by contact with corrosive and/or abrasive autoclave fluids entering via the sparge pipe 22.

[0099] The sparges 40 and 60 could be provided with a diffusion ring or plate, similar to the diffusion ring 34 of the sparge 20.

[0100] Preferably, the sparge pipe 22 extends a distance into the autoclave 26 that is relatively long length compared to its diameter.

[0101] In the context of the present invention “relatively long” with reference to the sparge pipe 22 means that the portion of the sparge pipe 22 residing within the autoclave 26 is greater than about 300% of external diameter of the sparge pipe 22.

[0102] Typically, the sparge pipe 22 has a relatively thick wall compared to its diameter. However, the sparge pipe 22 could be made from relatively thin wall material.

[0103] In the context of the present invention “relatively thick” with reference to the wall of the pipe means that the pipe wall is greater than about 10% of the radial dimension of the pipe.

[0104] Typically, the sparge pipe 22 is made from stainless steel metals, chemically resistant alloy materials (such as tantalum) or the like.

[0105] The autoclave 26, fitted with six of the sparges 20 of the present invention, is shown in FIG. 19. A single cell of the autoclave 26 is shown in FIG. 18. The autoclave 26 may be of generally conventional design and construction in the accommodation of the sparge 20, 40, 60, 80. Typically, there is one sparge 20, 40, 60 or 80 per cell, although there could be two or a few sparges 20, 40, 60 or 80 per cell. However, typically, there is only one agitator 16 per cell.

[0106] In relation to the vapor lock means it is preferred that the cross sectional area increases from that of the sparge pipe 22, 62 and 82 to the outlet 32, the apertures 66 and the opening 86 respectively so as to reduce the velocity of the sparge fluids entering into the autoclave 26 and reduce the risk of combustion of the sparge pipe 22, 62 and 82. The increase in cross sectional area has the effect of ensuring that velocity of sparge fluids is kept below a critical impingement velocity of approximately 20 m/s—above which critical velocity, with other conducive factors, oxygen or other flammable fluids injected into the autoclave 26 may cause combustion of the metal (such as titanium, stainless steel and some alloys) of the sparge pipes 22, 62 and 82 and the vapor lock means.

[0107] That is to say, it is preferred that the cross sectional areas of the sparge pipe 22, 62 and 82 and the vapor lock means increase in the direction of flow of the reagent fluids so as to avoid high flow rates that can cause metal materials of the pipe to either wear rapidly or even to combust and in the worst case lead to loss of containment and violent and rapid depressurization of the autoclave 26. Careful design is used to maintain maximum fluid flow rates in high pressure autoclaves, typically below 20 m/s, to substantially reduce the risk of combustion of sparge pipe metal materials in the presence of high concentration oxygen and typical pressures. However, the critical velocity of reagent fluids in high concentration oxygen is pressure dependent, for example at 5.6 MPa (56 bar) the critical impingement velocity of high concentration oxygen is only 8 m/s.

[0108] Preferably, the cross-sectional area of the sparge pipe 22, 62 and 82 and the vapor lock means generally increases in the direction of flow of the reagent fluids being injected into the autoclave 26.

[0109] Preferably, the cross-sectional area of the vapor lock means is at least 100% larger than the cross-sectional area of the sparge pipe 22, 62 and 82.

[0110] More preferably, the cross-sectional area of the vapor lock means is at least 200% larger than the cross-sectional area of the sparge pipe 22, 62, 82.

[0111] It is important that there be no flow path into the sparge pipe 22, 62 and 82 upstream of the vapor lock means. This is because any joins that form part of the sparge 20,40,60,80 or the vapor lock means produce a potential flow path for high pressure fluids from inside the autoclave 26 to inside the sparge pipe 22, 62 and 82. Accordingly, bolting through the sparge pipe 22, 62 and 82 is not permitted. Any joins that form part of the sparge or vapor lock means must be sufficient so as to ensure that fluid cannot bypass through the wall of the sparge pipe 22, 62 and 82 directly to or from the autoclave 26.

Use

[0112] In use, the sparge 20, 40, 60 or 80 is installed into the autoclave 26 via the flange 28. The flange 28 provides a seal with the sparge pipe 22, 62 and 82 and prevents high pressure fluids escaping the autoclave 26.

[0113] The sparges 20 and 60 are installed into the flange 28 from inside the autoclave 26. Whereas, the sparges 40 and 80 can be inserted into the autoclave 26 through the flange 28 from outside the autoclave 26.

[0114] Under normal sparge operation of the bottom entry sparge 20, sparge fluids flow upwardly through the sparge pipe 22 out of the end 24 of the sparge pipe 22, through the apertures 29, and out of the inverted cap 30 through the outlet 32 and into the autoclave 26 proximate the diffusion ring 34. The diffusion ring 34 serves to direct higher density sparge fluids, such as water, away from the sparge pipe 22. The agitator 16 then mixes the sparge fluids throughout the slurry 36 to increase the speed of reaction or control production processes.

[0115] For the bottom entry sparge 40, sparge fluids flow upwardly through the sparge pipe 22 out of the free end 44, into the inverted cap 42, out of the outlet 32 and into the autoclave 26 as the inverted cap 42 rotates with the agitator 16. The agitator 16 then mixes the sparge fluids throughout the slurry 36.

[0116] For the top entry sparge 60, sparge fluids flow downwardly through the sparge pipe 62, impinge against the end plate 64, flow out of the apertures 66 and into the autoclave 26 proximate the agitator 16, which then mixes the sparge fluids throughout the slurry 36.

[0117] For the side entry sparge 80, sparge fluids flow through the sparge pipe 82 and out of the opening 86 and into the autoclave 26.

[0118] The sparge fluids may be dilute acid or dilute alkali, water, steam or a gas such as oxygen, for example. The sparge fluids must not be permitted to combust or cause any material within the autoclave 26 to combust—otherwise the autoclave 26 has the potential to explode.

[0119] In each embodiment of the present invention, during low or no flow of sparge fluid, the pressure within the sparge pipes 22, 62 and 82 is the same as the pressure inside the autoclave 26 and hence a vapor lock is achieved preventing backflow of fluid from the autoclave 26 into the sparge pipes 22, 62 and 82.

[0120] Also, because of the disposition and orientation of the outlets 32, the apertures 66 and the openings 86 particulate materials within the autoclave 26 cannot fall under the force of gravity into the sparge pipes 22, 62 and 82, thus substantially preventing blockage of the sparge pipes 22, 62 and 82.

INDUSTRIAL APPLICABILITY

[0121] The sparge 20, 40, 60, 80 of the present invention is suitable for use in increasing the rate of reaction processes within a high-pressure vessel such as an autoclave for the recovery of valuable minerals from ore without the use of pyrometallurgical methods and processes.

[0122] The sparge 20, 40, 60, 80 of the present invention resides and operates in the fields of high pressure mineral processing via autoclaves and elevated temperature for the recovery of valuable minerals from ore.

[0123] The consequence of the use of the sparge 20, 40, 60, 80 of the present invention is that reagent fluids can be injected into the autoclave without the risk of the sparge pipe 22, 62 and 82 becoming blocked with slurry or detritus material even under low or no flow conditions, thus avoiding downtime otherwise required to clear prior art sparge pipes used in autoclaves.

[0124] Also, the sparge 20, 40, 60, 80 of the present invention is designed to slow the flow of reagent fluids into the autoclave 26 to reduce the risk of combustion or wear of the metals materials used to make the sparge 20, 40, 60, 80.

REFERENCE SIGNS

[0125] The specification uses the following reference signs:

PRIOR ART

[0126] 10 high-pressure autoclave [0127] 12 sparge [0128] 14 flange [0129] 16 agitator

PRESENT INVENTION

[0130] 20 bottom entry sparge [0131] 22 sparge pipe [0132] 24 free end—sparge pipe [0133] 26 autoclave [0134] 28 flange [0135] 29 apertures [0136] 30 inverted cap [0137] 32 annular outlet [0138] 34 diffusion ring [0139] 36 slurry level [0140] 40 bottom entry sparge [0141] 42 inverted cap [0142] 44 free end—sparge pipe [0143] 46 aperture [0144] 60 top entry sparge [0145] 62 sparge pipe [0146] 64 end plate [0147] 65 elbow [0148] 66 apertures [0149] 80 side entry sparge [0150] 82 sparge pipe [0151] 84 blank end [0152] 86 opening

Vapor Lock Means

[0153] The free end 24, the apertures 29, the inverted cap 30 and the annular outlet 32 together constitute the vapor lock means of the bottom entry sparge 20 embodiment of the present invention with the inverted cap 30 mounted onto the sparge pipe 22.

[0154] The free end 44, the aperture 46, the inverted cap 42 and the annular outlet 32 together constitute the vapor lock means of the bottom entry sparge embodiment of the present invention with the inverted cap 42 mounted onto the agitator 16.

[0155] The end plate 64, the elbow 65 and the apertures 66 together constitute the vapor lock means of the top entry sparge 60 embodiment of the present invention with the sparge pipe 62 entering via the upper reaches of the autoclave 26 above the agitator 16.

[0156] The blank end 84 and the opening 86 together constitute vapor lock means of the present invention with the side entry sparge pipe 82.

Advantages

[0157] The sparges 20, 40, 60 and 80 of the present invention have the advantage that they include a vapor lock means which inhibits the backflow of particulate material and detritus material under low or no fluid flow situations which occur commonly in the operation of a high-pressure autoclave 26.

[0158] The sparges 40 and 80 have the added advantage that they can be removed and serviced without entering the autoclave 26.

[0159] The sparge 20, 40, 60, 80 has the added advantage that its fluid flow passages increase in cross sectional area in the direction of flow of reagent fluids so as to maintain the velocity of the reagent fluids below a critical impingement velocity above which materials of the pipe 22, 62 and 82 and the vapor lock means are likely to combust in the presence of high purity oxygen or experience excessive wear.

[0160] The coating of the sparges 20, 40, 60 and 80 has the further advantage of reducing wear upon their wetted external surface and increasing the interval between servicing of the sparges 20, 40, 60 and 80.

[0161] The sparge 20, 40, 60, 80 has the further advantage that there are no fluid flow paths through the wall of the sparge pipe 22 or the walls of the vapor lock.

[0162] The diffusion ring 34 and plate 64 have the advantage of directing exiting sparge fluids away from the spare pipe 22 and the bottom of the autoclave 26 and prolonging the operational life of the sparges 20 and 40 and the autoclave 26. The ring 34 and 64 is more typically beneficial where high density fluids, such as liquids, are used. The ring 34 and 64 is not very beneficial where only very low-density fluids, such as gas or steam, are used. This is because the buoyant force of the very low-density fluid is dominant over the relatively small downward momentum that the exiting fluid has.

MODIFICATIONS AND VARIATIONS

[0163] It will be readily apparent to persons skilled in the relevant arts that various modifications and improvements may be made to the foregoing embodiments, in addition to those already described, without departing from the basic inventive concepts of the present invention. For example, other forms of protective coating could be used. Also, other sparge configurations, that maintain the vapor lock principle, could be used. Further, whilst the outlet 34 of the sparge is typically shown and described an annular, it could also be other shapes, such as, for example, flute shaped as shown as the flutes 66.