JPS6129772B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method and apparatus for carrying out gas-liquid reactions in the presence of a dispersed catalyst. The invention has particular application in the catalytic hydroconversion of hydrocarbons and will be explained in detail below with reference to this preferred application.

A process for hydrotreating a heavy hydrocarbon charge in the liquid phase using a dispersed particulate catalyst, in particular in which the catalyst bed is in an expanded state and the expansion is caused by the formation of a liquid charge of hydrocarbons and a hydrogen-containing gas. A method is known in which this is caused by a flow from the bottom to the top.
An example of this method is the H-oil method. This type of process does not allow sufficient utilization of the catalyst. In fact, the catalyst removed from the reactor is a mixture of very highly deactivated, partially deactivated and almost fresh catalyst, and depending on the degree of deactivation, the particles of catalyst Sorting is a difficult operation.

According to one variation of this technique, a series of homogeneous layered beds can be used. Fresh catalyst is placed at the top of the reactor and divided between each layer as the process progresses. The catalyst is removed from the bottom, last layer. According to this, it is possible to improve the catalyst utilization rate before the completion of the process. In this type of reactor, the main difficulty is that the catalyst
It depends on the transfer method from one layer to another layer.

According to the first proposal, the lowering of the catalyst takes place successively through each level of the device. As a practical matter,
It is difficult to operate such devices accurately. The descent of the catalyst is erratic, and in some cases the transfer channels are seen to become clogged, and in others there is even siphoning or cessation of fluidization. For relatively accurate operation, relatively high speeds must be used for lowering the catalyst;
Catalyst utilization is quite poor.

The next proposal uses a gate valve to control the lowering of the catalyst. Due to the presence of catalyst particles, the gate valve is not watertight. Therefore, gate valves are rapidly damaged, and the provision of gate valves inside the reactor poses difficult problems for their control and maintenance in view of the temperature and pressure conditions and the type of reaction medium. .
If the gate valve is installed outside the reactor, a hole must be drilled into the side wall of the reactor, which is exposed to high temperatures and
This weakens its robustness to high pressures. Opening the gate valve then disturbs the pressure distribution in the reactor, causing siphoning and even cessation of fluidization in the relevant parts of the reactor.

The present method prevents these disadvantages by proposing a method and apparatus with significantly improved catalyst transfer. This transfer can be done periodically or continuously as desired. No mechanical transfer equipment is required.

The method according to the invention comprises: (a) flowing a mixture of liquid and gas from bottom to top, generally countercurrently across a dispersed catalyst, through a reaction zone comprising a plurality of stacked levels, the levels comprising: separated by a partition wall and containing a catalyst at least partially dispersed in the flowing liquid, each level having, on the one hand, a catalyst disposed at the associated separating partition and located in a straight path of the liquid and gas; and, on the other hand, by at least one catalyst transfer tube external to said straight passage, communicating with the adjacent storey by a plurality of openings of small cross-section allowing the passage of the transfer tubes; (b) the lower part constitutes a relatively quiet zone in which the catalyst can be deposited; (c) introducing the active catalyst into the upper level of the reaction zone; (d) passing from one level to the level below it by means of said conduit external to the straight path of the liquid and gas; (e) removing liquid reaction products and residual gas from the lower level of the reaction zone; in a method for reacting the gas of a dispersed solid catalyst with a liquid, the catalyst accumulated in the lower part of the transfer tube; is entrained towards the level immediately below using an adjustable sub-flow of liquid and/or gas injected into the catalyst transfer tube towards a port connecting the lower part of the transfer channel to the level immediately below. It is characterized by controlling the flow rate of catalyst migration from one level to the level immediately below. The catalytic reactor of the present invention also comprises an essentially vertical elongated enclosure divided into several overlapping tiers by an essentially horizontal separation wall having a plurality of relatively narrow openings. and the entire opening is of sufficient size to permit simultaneous upward migration of liquid and gas, each level having an opening through said opening on the one hand and an upward migration of liquid and gas on the other hand. In an apparatus communicating with the level immediately below by at least one relatively wide transfer pipe with a lower end arranged so as not to directly receive liquids and gases, a secondary flow of gases and/or liquids. means for injecting the catalyst into the transfer pipe, said means being positioned towards the communication opening connecting the lower part of the catalyst transfer pipe to the level immediately below, so as to entrain the catalyst towards the level immediately below. It is characterized by what has been done.

The device is therefore characterized by a series of superimposed hierarchies. Each level is divided, on the one hand, by a common opening of small unit cross-sectional area, such as the free space of a grid located in the main channel of the fluid, and on the other hand, by a common opening located outside the main channel of the fluid, i.e. It communicates with the adjacent storey by at least one transfer tube arranged so that gases and fluids cannot easily enter it during its ascending movement. According to a first implementation, the catalyst transfer channels open here and there on the partition wall, respectively upwardly and downwardly, at points relatively distant from the partition wall. According to one variant, the upper part of the transfer channel is adjacent to the partition, and only the lower end is remote from said partition.

The perforated partitions are preferably arranged horizontally.

Each layer has the following: Namely: (1) contact zone between the lower three phases (gas, liquid, catalyst); There, the catalyst is held in suspension in a gas-liquid stream coming from a perforated partition below.

(2) Upper zone with less solid catalyst. There passes gas and liquid fresh from the lower zone before entering the upper level through the upper perforated partition.

(3) Catalyst filling port at the level of the lower zone.

(4) Catalyst exhaust pipe to the level directly below.

This conduit can take the form of an overflow pipe through which excess catalyst constantly overflows, but whose height demarcates the two zones quite clearly. This overflow pipe conveys the catalyst to a conduit opening at the bottom of the lower level. However, this overflow pipe is not essential. In fact, the catalyst transfer channel can be opened at that level of the perforated partition.

As defined above, occupancy is defined to characterize the suspension of the catalyst within the lower zone.
It is the ratio of the volume occupied by the quiescent catalyst present on the grid to the volume of the lower zone rich in suspended catalyst, as defined above. This ratio usually falls between 0.1 and 0.9.

Preferably, the gas and liquid may also be separated outside the reactor, but in the upper echelon of the device,
Above the catalyst release zone there shall be provided a relatively quiet gas-liquid separation zone with separate gas and liquid release. The lower level of the device also comprises a release zone for catalyst particles and at least one discharge tube for these particles.

Each level is separated by a partition wall that has in its part (the main passage for the charge and gas) small cross-section openings through which liquid and gas can pass from bottom to top. It is not essential that the openings be smaller than the catalyst particles. In fact, the inter-storey passage free surface is necessarily smaller below the separation barrier than the free surface of each storey, so that the passage velocity of the fluid is greater through the opening than in other parts of the storey. If a sufficiently small and totally free passage surface is chosen, this velocity will be such as to prevent any direct descent of the catalyst through the opening.

According to one variant, the aperture is not uniform;
Some are adapted to favor the passage of gases, while others favor the passage of liquids.

The openings can be of various shapes, such as circular, rectangular or square perforations, elongated slots, grids, etc. For example, its width is
It may be 0.1 to 20 mm. For example, grids of steel bars spaced apart by 0.5 to 5 mm are preferred.

Desirably, there should be no openings in the portion of the partition below the catalyst transfer conduit. Therefore,
This conduit is a relatively quieter zone outside of the main liquid and gas passages.

The catalyst particles usually have a diameter of between 0.1 and 10 mm, but this value is not limiting. The equivalent diameter is determined by the following formula:

de=6×average volume of particles/average external surface area of particles The hydrocarbon charge treated according to the invention has:
Hydrocarbons or mixtures of hydrocarbons of a very mixed type and containing undesirable elements. One application of particular interest involves the treatment of relatively heavy feedstocks (such as crude oil or distillation residues) containing impurities such as sulfur and/or nitrogen compounds, asphalt, organometallic compounds or metal compounds. can do.
The reactions carried out here are aimed at heavy charges of this type, in particular desulphurization, denitrification, hydrocracking, hydrogenation and demetallization.

Another type of reaction is the synthesis of hydrocarbons by reaction of gases such as CO and H ₂ in a flowing hydrocarbon liquid phase. Yet another type is the "hydrogenation" or treatment of coal or oily shale with hydrogen dissolved or dispersed in a flowing hydrocarbon solvent. Another type is the finishing treatment of used oil, which removes additives and organometallic particles from used oil and improves its lubricity and stability against oxidation and temperature through hydrogenation. .

The reaction conditions are usually temperature: 270 to 450°C, pressure: 20 to 300 atmospheres, and flow rate of liquid charge: 0.1 to 10 volumes per 1 volume of catalyst.

Catalysts are of known types already used in similar reactions, for example in neat form or on supports such as alumina, silica-alumina, silica, magnesia, bauxite, red mud, clay, diatomaceous earth. It is a compound of group metal and/or group metal held in

As examples of metal compounds, mention may be made of oxides and preferably sulfides of molybdenum, tungsten, nickel, cobalt and/or iron. These catalysts are of conventional type and can be manufactured by known methods.
The process can also be carried out in whole, in series or in parallel combinations of several distributed catalytic reactors of the type described. It is also possible to arrange one or more fixed bed reactors in succession to one or more distributed catalytic reactors of the type described, which fixed bed reactors do not allow for completion of the reaction. or to carry out different reactions, such as saturated hydrogenation, hydrodesulphurization, hydrodenitrification, hydrocracking, catalytic cracking, hydrorefining or hydrofinishing.

FIG. 1 shows a cross-section through three successive levels of the reactor. The liquid charge of hydrocarbons and hydrogen are distributed in grids 1, 2, 3, 4 and chambers 5, 6, 7,
8 and 9, it flows through the central part of the device from bottom to top. On each level, in each chamber, the catalyst is present dispersed and entrained by the liquid and gas flow over a height equal to or slightly higher than h ₁ . The upper part of each chamber is h ₂
It shows a wider area over the height of . A portion of the catalyst thus escapes from the chamber 8 and enters the lateral conduit 10 defined by the side wall and internal partition 11 of the reactor.
fall into the. This lateral conduit 10 is a very quiet zone. The catalyst therefore descends under gravity and accumulates in this conduit 10. Catalyst accumulated in conduit 10 is removed from opening 12 at the base of conduit 10.
It forms a slope against the ground.

According to the invention, in order to more precisely control the flow rate of the catalyst passing from the conduit 10 into the chamber 7, the catalyst forming the slope is preferably separated into a separate tube, for example made of a reactive or inert gas or liquid. can be entrained by sub-streams of The higher the flow rate of this side stream, the higher the flow rate of catalyst that should be fed from conduit 10 to chamber 7.
The flow rate of the secondary fluid could be measured and controlled externally by known means.

FIG. 2 shows an embodiment that allows the introduction of this secondary stream exiting through the conduit 15 at right angles to the opening 16.

FIG. 3 shows another embodiment. The partition wall 18 accommodates a slope formed by the catalyst, but this slope is not entrained in the main flow of fluid. By means of conduit 17 it is possible to inject a sub-stream of fluid which entrains the catalyst in the direction of arrow A towards chamber 7. The flow rate of fluid in conduit 17 is adjusted to control the transition from one level of catalyst to another, which transition may be continuous or periodic.

FIG. 4 shows the upper part of the device by way of example.
The catalyst tank 19 can optionally be placed under atmospheric pressure by means of gate valves 20,21. Gate valve 21
When the is open, the catalyst travels down the conduit 22 and passes through the opening 23. A secondary stream of liquid or gas, not shown here, carries the catalyst to chamber 24.
accompany you inside. Since the liquid velocity decreases in the widened zone, no catalyst is entrained into this zone. Liquid, substantially free of catalyst, can therefore be discharged through conduit 26 and gas can be discharged through conduit 27. If necessary, the liquid may be passed through a device such as a hydrocyclone to achieve complete liquid-catalyst separation.

The catalyst gradually falls into conduit 28.

Discharge of the spent catalyst in the lower part of the device is carried out simply by passing it through a side line leading to the spent catalyst tank. A device such as that described above may be extensively modified without departing from the scope of the invention. Depending on this, the number and location of the descending catalyst pipes may be different, and the volume of each layer may be the same or different.

A preferred implementation is as described below.

The contacting device comprises a series of layered tiers separated by partitions consisting of perforated plates, grids or any other device that ensures communication between the compartments delimited by the partitions. Each septum consists of at least one preferably vertical cylinder with an upper part abutting the perforated septum and a bent lower part opening into the lower compartment to a considerable extent horizontally, for example as shown in FIG. The catalytic converter has descending tubes or "legs" of catalyst.

The reaction charge consists of a mixture of liquid and gas,
Traverse each level from bottom to top through each perforated bulkhead. The ebullated bed catalyst in each level passes from top to bottom through descending "legs" in a manner that will be explicitly described below.

Thus, each layer has: (1) A lower contact zone between the three phases (gas, liquid, catalyst) in which the catalyst is held in suspension in the gas and liquid streams coming from the grid below. This lower zone constitutes the actual boiling bed.

(2) A solid catalyst-poor upper zone through which gases and liquids from the lower zone pass before entering the upper strata. It is a virtually inactive zone on the reaction surface.

(3) At least one curved line at the bottom of the zone arranged so that the catalyst does not flow naturally into the base of the conduit to allow the catalyst to pass from one level to another. Conduit or “leg”.

(4) preferably in the lower part thereof, preferably in the bend, the secondary fluid is at least in large part;
at least one secondary fluid injection tube opening into the leg and oriented to exit in the direction of the inner opening of the leg;

Each layer is characterized by the following points:

(1) The occupancy rate of each floor, which may be the same or different. It is the distribution of the volume of the strata occupied by the boiling catalyst bed. This rate is
It is between 0.1 and 0.9, preferably between 0.5 and 0.8.

(2) Expansion coefficient characterized by the ratio of the volume occupied by the stationary catalyst bed to the volume of the boiling catalyst bed. This expansion rate is not imposed by engineering or process considerations, but rather results from the totality of hydrodynamic factors that regulate the flow of fluid and solid catalyst. In the examples considered, the expansion ratio was between 20 and 70%, but was often close to 50%.

FIG. 5 is a cross-sectional view of three successive levels of a reactor operating in accordance with the principles of the present invention.
The reaction liquid and reaction gas are in grids 31, 32, 3.
3, 34 and chambers 35, 36, 37, 38, 39 through the device from bottom to top.

In each chamber, under the action of liquid and gas flows,
The catalyst forms a so-called "boiling bed" or "boiling catalyst bed".

Some of the catalyst escapes from the main stream of fluid and accumulates in the transfer or descending tubes 40, 41, 42 and becomes available for supplying catalyst to the chambers below.

The lower portions of the descending conduits 40, 41, 42 are arranged so that the catalyst cannot virtually escape naturally (i.e. in the absence of a carrier fluid flow admitted through the conduits 44, 52, 53) and Form a slope at the base of the tube. The bent configuration of the lower portions of these descending tubes and the presence of catalyst accumulated in these descending tubes create an impediment to the re-ascent of the reaction fluid through the legs.

FIG. 6 shows one embodiment of the lower part of the transfer tube or descending tube.

The vertical cylindrical descending pipe 40 is bent at its lower part so that accumulated catalyst can form a slope within the bend. Descending pipe 40 communicates with chamber 36 by an opening 43. An anti-eddy current device is constituted by plate 51. As seen in the figure, the bend can be extended by a short length of conduit. As can also be seen with respect to the same figure, in the absence of a flow of conveying secondary fluid, during the course of operation, the catalyst accumulates in the descending tube at a slope of an average angle .beta. with the horizontal line. If the descending pipe is installed at an angle α < β, the catalyst will naturally escape, since the angle α is the angle between the horizontal line and the top of the bend at the bottom opening of the descending pipe when viewed from the bottom opening. I can't leave.

Preferably, the descending tube or leg opens into the lower chamber above the boiling bed rather than at it itself. In this case, the descending pipe opens at the (vertically defined) midpoint of the lower chamber and not at the level of the grid at the bottom of said lower chamber.

At the bottom of the bend, a conveying secondary fluid, consisting of a liquid (e.g. a hydrocarbon fraction) which has already undergone a conversion process, preferably in the same device or in a different type of device, is introduced into the opening 43 by a conduit 44. The catalyst can be allowed to flow out through the pipe and the flow rate can be adjusted.

The ratio of the volume of secondary fluid used for lateral transport of the solid catalyst to the volume of fluid treated in the reactor during the same period is always small, for example comprised between 0.01:1 and 0.0001:1. .

The level of the boiling bed in each chamber is measured by known means such as, for example, a gamma radiation sonde.

In order to increase the height of the boiling bed in a chamber, it is sufficient to introduce a secondary fluid, either continuously or intermittently, into the descending pipe supplying this chamber with catalyst. It is possible to make the level of the ebullated bed dependent on the intake flow rate of the secondary fluid by known means.

It may be desirable to periodically or continuously remove a portion of the catalyst from the reaction enclosure and replace it with fresh or regenerated catalyst. To remove the spent catalyst,
This is done from the last layer counting from the top. Replenishment of new or regenerated catalyst is carried out into the first tier counting from the top. To remove the spent catalyst from the last layer, the apparatus shown in FIG. 7 is used.

Since the catalyst must be kept stationary, the lowermost grid 45, which has finer perforations than the perforations of the other grids, penetrates the lower inner wall of the reactor and connects to the elevator pot 47. A descending pipe 46 is connected to the upper part of the pipe. Catalyst accumulates in pot 47 by gravity.

One or more side pipes 48 make it possible to inject a first stream of a secondary fluid, preferably consisting of already treated liquid, which is preferably connected to the axis of the riser pipe 50. conduit 4 with an axis coincident with
(1) introducing the catalyst into another reaction zone, or (2) introducing it into a regeneration zone. or (3) allow the catalyst to rise again for storage until completion of the process.

The length and cross-sectional area of the descending tube 46 is such that a weak flow of secondary liquid ascending from the elevator pot into the descending tube has a hydraulic pressure that prevents the transfer of fluid from the reaction enclosure toward the elevator pot. must be calculated to be sufficient to produce a reduction.

Ultimately, it is the flow rate of the secondary fluid admitted through side pipe 48 that regulates the withdrawal flow rate within the reaction enclosure. Removal may be continuous or intermittent.

Thus, an improved device for the implementation of multi-level ebullated beds has been described.

The arrangement of the transfer tube or descending tube of FIGS. 5 and 6, and in particular the omission of the septum 11 in FIG. 1, offers the following advantages over the arrangement of FIG.

(1) Separation of heavy particles is better carried out. This allows preferential removal of the most inactivated particles. This is particularly useful in processes where demetallization is to be carried out.

(2) The reactor can be drained, filled and operated more completely and more rapidly.

(3) The level of the boiling bed within each level can be varied easily and independently, giving flexibility to the process.

(4) There is a considerable amount of active fraction from the reactor.

Up to this point, we have described the manner in which various fluids are transferred from one level to another and the devices that enable adjustment of the catalyst flow rate within each of the conduits 10. However, the individual adjustment of the flow rates of the fluid sub-streams must be adjusted to avoid imbalances in the catalyst charge contained in each chamber.

Under established operating conditions, at each level:
The amount of catalyst received from the upper tier must equal the amount of catalyst leaving the tier.
This can be carried out by monitoring the level of the catalyst bed being forced down into the successive conduits 10 and 13 and manipulating the flow rate of the secondary fluid to keep this level constant. . Therefore, if the level of catalyst in conduit 13 drops, the amount of catalyst fed to chamber 7 is increased so that the overflow of catalyst from chamber 7 to conduit 13 is increased to compensate for the drop in level in conduit 13. Must increase. This is achieved by increasing the flow rate of the catalyst through the opening 12 and, for example, by increasing the flow rate of the secondary fluid coming through the conduit 15 according to FIG. 2 and through the conduit 17 according to FIG. be done.
The effect of this is to reduce the level of catalyst in conduit 10 and thus increase the amount of catalyst fed into chamber 7. In this way, one after the other, the level of catalyst in each of the conduits is readjusted from bottom to top. Control linking the level of catalyst in each of the conduits to the flow rate of the secondary fluid at the base of the conduit immediately above can be performed automatically in a known manner.

The invention described in connection with the reaction between hydrocarbons and hydrogen has application in all cases where gases and liquids are reacted in the presence of a dispersed catalyst.
Examples of such reactions include:

(1) Various oxidations in the liquid phase in the gas phase in the presence of solid catalysts, in particular the oxidation of acetic acid solutions with oxygen-containing gases in the presence of catalysts whose main components are, for example, iron oxide or palladium oxide.

(2) synthesis from compounds in solution, e.g. synthesis of butanediol from acetylene on a solid catalyst based on formaldehyde and copper acetylide in the aqueous phase, or also allyl alcohol on a fixed catalyst impregnated with rhodium; Synthesis of butanediol from CO + H ₂ mixture.

EXAMPLE The process of the invention was carried out in a reactor having 5 overlapping layers. Through the reactor, on the one hand, the liquid phase consisting of hydrocarbons and hydrogen gas pass from bottom to top, and on the other hand, the solid catalyst passes from top to bottom. The catalyst has a generally regular spherical shape with a diameter of 1 to 3 mm, most often 2 to 2.5 mm. The perforated partitions placed horizontally between each of the levels have circular perforations with a diameter of 3.5 mm (larger diameter than the particles of catalyst used here). The area of the perforations represents approximately 30% of the area of the perforation zone.
The flow rates of the liquid and gas phases correspond to a surface flow rate of the liquid (ratio of the volumetric flow rate to the cross-sectional area of the reaction zone of the reactor) equal to 5 cm/s and a surface flow rate of the gas equal to 1 cm/s, respectively. There is. Under this condition, the catalyst occupancy is 30%. Thus,
The process as described above allowed the catalyst to be routinely circulated from bottom to top, from layer to layer, continuously with a regular flow rate of 3.6/hr.

In the apparatus described above, limited vacuum distillation residues were treated as follows.

Density ¹⁵ ₄ : 1.01 Freezing point: 38°C Sulfur: 5.35% by weight Vanadium: 87 ppm by weight Nickel: 34 ppm by weight Initial boiling point: 480°C Reaction conditions are as follows: Temperature: 390-410°C Hydrogen pressure: 120 atm Space velocity: 1 per reaction space per hour The catalyst contains molybdenum sulfide-cobalt sulfide on spherical alumina.

Gasoline (yield: 42% by weight), gas oil fraction (yield: 16% by weight), and desulfurized heavy oil (yield: 78% by weight,
Sulfur content: 1.7% by weight or less, Nickel: 12ppm,
Vanadium: 14ppm) was obtained.

According to the invention, the catalyst accumulated in the lower part of the transfer pipe is injected into an adjustable sub-flow of liquid and/or gas towards the communication opening connecting the lower part of the transfer pipe to the level immediately below. The flow rate of the transfer of catalyst from one level to the level directly below is controlled by entraining it towards the level immediately below, so that the lowering of the catalyst in the transfer tube is carried out regularly and the flow rate of the catalyst is controlled. Clogging of the transfer tube can be avoided. Further, since there is no need to use a gate valve for catalyst descent control, there is no possibility of the above-mentioned problems associated with the provision of a gate valve. Thus, according to the present invention, all the problems of the prior art as explained at the beginning of this book can be solved.

[Brief explanation of the drawing]

The drawings show an embodiment of the present invention, and FIGS. 1 to 7 are vertical longitudinal sectional views showing a part of the reactor. 1, 2, 3, 4, 31, 32, 33, 34...
Grid (separation wall), 5, 6, 7, 8, 35,
36, 37, 38...room (floor), 10, 13,
40, 41, 42... Conduit (catalyst transfer pipe), 1
2, 14, 16, 23, 43...Opening (communication opening), 15, 17, 44, 53...Substream flow conduit.

Claims (1)

[Scope of Claims] 1 (a) Flowing a mixed liquid and gas from bottom to top, generally in countercurrent to a dispersed catalyst, through a reaction zone having a plurality of stacked layers, the layers are separated by a partition wall and include a catalyst at least partially dispersed in the flowing liquid, each level having, on the one hand, a catalyst disposed at the associated separating partition wall and located in a straight path of the liquid and gas; communicating with the adjacent storey by means of a plurality of openings with a small cross-section allowing the passage of gases and, on the other hand, by at least one catalyst transfer tube located outside said straight passage, transfer tubes; the lower part of which constitutes a relatively quiet zone in which the catalyst can be deposited; (b) liquids and gases are passed through small cross-sectional openings in each level and the corresponding separation partition; (c) introducing the active catalyst into the upper level of the reaction zone; (d) passing from one level to the level below it by said conduit external to the straight path of liquid and gas; (e) removing the catalyst from the lower strata of the reaction zone; and (f) thus removing the liquid reaction products and residual gas from the upper strata of the reaction zone. in a method in which the catalyst accumulated in the lower part of the transfer tube is reacted with an adjustable submergence of liquid and/or gas injected towards a communication opening connecting the lower part of the transfer tube to the level immediately below. A method characterized in that the flow rate of the transfer of catalyst from one level to the level immediately below is controlled by entraining the flow towards the level immediately below. 2. The method according to claim 1, wherein the liquid is a hydrocarbon liquid and the gas is a hydrogen-containing gas. 3. A process according to claim 2, wherein the charge also contains carbon monoxide and the synthesis produces additional hydrocarbons. 4. Claim 2 in which the charge also contains coal and the synthesis produces additional hydrocarbons.
The method described in section. 5. A process according to any one of claims 1 to 4, wherein the catalyst comprises at least one compound of group metals and/or group metals. 6 Supply catalyst to the given hierarchy (N position)
controlling the flow rate of the liquid and/or gas substream injected into the transfer tube in response to variations in the level of catalyst accumulated during the (N+1) discharge of said level; 6. A method according to any one of claims 1 to 5, wherein a decrease in the flow rate of the secondary stream injected into the tube (in N) causes an increase in the flow rate of the secondary stream injected into the tube, and vice versa. Method. 7. The method according to any one of claims 1 to 6, wherein the perforations in the partition wall have a unit width of 0.1 to 20 mm. 8. According to any one of claims 1 to 7, the transfer tube is open on both sides of the partition wall at each point of the relevant hierarchy that is vertically relative to said partition wall. the method of. 9. The method according to any one of claims 1 to 8, wherein the upper part of the transfer tube opens at the level of the partition wall, and the lower part opens at a certain distance downward from the partition wall. 10 Catalyst in a transfer tube with a lower part bent in a significant horizontal direction, allowing the accumulation of catalyst in said lower part and impeding the re-ascent of liquid and gas in the transfer tube. A method according to any one of claims 1 to 9, which descends as follows. 11. The method of claim 1, wherein the bent lower portion of the transfer tube is located a fixed distance above the lower bulkhead of the level to which the transfer tube supplies catalyst. 12. A method according to any of claims 1 to 11, wherein the volume ratio of the fluid forming the secondary stream to the treated fluid is between 0.0001:1 and 0.01:1. 13 comprising an essentially vertical elongated enclosure divided into several superimposed tiers by separating partitions having a plurality of essentially horizontal and relatively narrow openings; is of sufficient size to allow upward migration of liquid and gas at the same time, and each level is such that it does not directly receive ascending liquid and gas on the one hand through said openings and on the other hand. In an apparatus communicating with the level immediately below by at least one relatively wide transfer tube having a lower end located at characterized in that the means is arranged toward a communication opening connecting the lower part of the catalyst transfer pipe to the level immediately below, and is adapted to entrain the catalyst toward the level immediately below. Catalytic reactor. 14. The device according to claim 13, wherein the perforations in the partition wall have a unit width of 0.1 to 20 mm. 15. Claim 13, wherein the bulkhead consists of grids of steel bars separated by a gap of 0.5 to 5 mm.
The device according to item 1 or 14. 16 Furthermore, opposite to the lower opening of the transfer tube on the side of the reaction zone, there is provided a partition wall opening at the apex and directed from bottom to top, which protects said opening against the flux produced by the liquid and gas in ascending motion. Apparatus according to any one of claims 13 to 15, comprising: 17 Furthermore, for each level, the injection rate of the gas and/or liquid sub-stream into the catalyst feed pipe for that level is controlled and the level of solid particles in the catalyst outlet line for that level is controlled. Claim 1 comprising a device consisting of a detector.
The apparatus according to any one of Items 3 to 16. 18. Apparatus according to any one of claims 13 to 17, wherein each separating partition comprises several transfer tubes. 19. Claim 13, wherein each transfer tube comprises a vertical cylindrical conduit bent at the bottom.
19. The apparatus according to any one of paragraphs 1 to 18. 20. The apparatus of claim 19, wherein the lower end of each transfer tube is substantially horizontal. 21. Claims 13 to 20, in which the lower opening of each transfer tube in a given level is located at a level significantly higher than the level of the perforated bulkhead which downwardly demarcates said chamber. The device described in any of the preceding paragraphs. 22. Apparatus according to any one of claims 13 to 21, further comprising a hydraulic elevator pot connected to the lower part of the enclosure and allowing evacuation of the catalyst.