DK146032B - METHOD AND APPARATUS FOR SEPARATING CATALYST PARTICULARS FROM CRACKS - Google Patents

Description

(19) DENMARK \ 5 | /

t (i2) PUBLICATION MANUAL od 146032 B

DIRECTORATE OF THE PATENT AND TRADEMARKET SYSTEM

(21) Patent Application No: 1266/76 (51) Lnt.CI.3: B 01 D 45/12 (22) Filing Date: 23 Mar 1976 C10 G 11/14 (41) Aim. available: 25 Sep 1976 (44) Submitted: 06 Jun 1983 (86) International Application No: - (30) Priority: 24mar1975US561625 (71) Applicant: 'ASHLAND OIL INC .; Columbus, US.

(72) Inventor: George Daniel 'Myers, US, Paul Winston' Walters; US, Robert Lee 'Cottage; US.

(74) Plenipotentiary: Hofman-Bang & Boutard Patent Office (54) Process and apparatus for separating catalyst particles from cracked hydrocarbons

The invention relates to a process for separating catalyst particles from cracked hydrocarbons and of the kind set forth in the preamble of claim 1.

In a known process of this kind, the cracked hydrocarbons and catalyst particles first flow horizontally and then into a downwardly bent bending line. The gas is discharged against

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the inside of the pipe bend, and the downward direction of the current in the form, with the change of direction caused by the pipe bend,

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Φ that the flow rate must be kept relatively low.

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The invention has for its object to provide a process of the kind indicated by which the separation process is optimized by being carried out at a higher operating temperature, a higher flow rate and with a smaller catalyst loss.

This is achieved according to the invention by a method of the characterizing part of claim 1.

The invention also comprises an apparatus for carrying out the method, which is characterized by the construction of claim 5.

The invention utilizes the high velocity of the catalyst particles and of the gas conveyed in the riser. The gas having a low density in comparison with the catalyst can be raised at an angle through the lateral upstream opening and into the cyclone, while the heavier catalyst is discharged into the separation chamber by its moving energy. In this way, the gas is fed into the cyclone while the majority of the particles are discharged into the separation chamber and out of the deflected gas stream. This is in contrast to the previous systems where the total flow of gas and particles is fed into the cyclone, and to other systems where the entire flow is introduced into the separation chamber.

The separation chamber is substantially closed for flowing such a large volume of gas through it, and no substantial gas flow from the riser through the separation chamber occurs. In the separation chamber, a static backpressure is maintained which deflects the gas at an angle from the riser so that it does not pass through the separation chamber but instead passes out into the inlet of the cyclone. The solid particles, which have a higher motion energy due to their higher density, continue to flow in the upward direction in which they are advanced in the riser and are not deflected by the back pressure. Thus, they flow through the outlet opening of the stirrer into the separation chamber and collect as a base at its bottom, from which they are extracted for stripping and return. The majority of the solid materials 3 146032 are thus passed past the cyclone and do not enter at all.

A smaller portion, which may be on the order of 10-20% of the catalyst, is fed into the cyclone and is separated there.

By means of the invention, several surprising results are obtained. A particularly unique and advantageous result is the possibility of substantially higher cracking temperatures. Furthermore, the gas velocity in the separation chamber is eliminated as an operating constraint, and thirdly, a great improvement in separation efficiency and stability is achieved over a larger range of operating conditions.

Since the outgoing gas from the riser does not flow through the separator, no significant gas flow occurs in the separator. This implies that the surface or volume velocity (defined as the flow rate divided by the cross-sectional area of the flow) is essentially zero. This factor, which in some prior embodiments has constituted a critical upper limit, therefore no longer constitutes a restriction. When there is no surface velocity in the separator, there is essentially no re-feeding of particles emitted from the riser, regardless of the working speed. Furthermore, since the pressure in the separator chamber is higher than the pressure in the cyclone, there is no inclination for the cyclone to deliver gas downwardly through its downflow tube, which in itself would cause a re-entry.

Surprisingly, the operating temperature of the separator can be increased by using the invention. Many separator chambers currently in use are made of metals that can withstand internal gas temperatures of up to approx. 500 ° C. By means of the device according to the invention, it has been found that the same separator vessel can now be operated at a temperature of approx. 560 ° C, i.e. an increase of approx. 60 ° C without exceeding the metal voltage limits. This is a significant advantage, as it has been found in recent years that these higher temperatures are desirable because of their effect on cracking reactions. Thus, a change in the structure of the riser cyclone in an existing separator jacket allows processes to be unwound at optimum gas temperatures higher than those originally calculated.

The reason for this seems to be that a static boundary layer of gas now covers the container wall and substantially reduces the heat transfer from the gas to the casing. Thus, the measured cutting temperature is actually lower at the same temperature of the gas delivered from the riser.

The invention is further explained below in connection with the drawing, in which: FIG. 1 is a schematic side view of a conventional type of rising cracking system; FIG. 2 is a vertical section through a portion of the separator chamber of a rising cracking apparatus provided with a separator device according to a preferred embodiment of the invention; FIG. 3 is a horizontal section through the separator chamber of FIG. 2 along line 3-3 and FIG. 4 is a vertical section through a modified embodiment of the invention.

As previously mentioned, the invention has its greatest application in the separation of catalyst particles from gases by increasing cracking in hydrocarbon transformation processes. For this reason, the invention is shown in the figures especially for this field of application.

In the embodiment of FIG. 1, the oil applied is pumped to the bottom of the riser where it is mixed with the incoming hot catalyst from the regenerator. The contact between the hot catalyst and the oil quickly provides a very large gas volume and cracking occurs as the mixture rises in the riser.

The elongated tubular ladder extends vertically or at an inclined angle upwards to a higher up separator vessel for separating the catalyst from the gases. The separated gaseous products are diverted for fractionation to be divided into gas, gasoline, light oil, gas oil and other products. The catalyst is collected in a base as indicated by a dotted line in the lower or stripping portion of the separator chamber. Steam is directed to the chamber to remove any cracked oil from the catalyst particles. The fired but coke precipitated catalyst is fed back from the evaporator to the regenerator, where coke is burned by the supply of hot combustion air which emits flue gases as a product.

The hot catalyst is then returned. Usually, a feed hopper is provided for storing the catalyst.

In the embodiment of FIG. 2, according to the invention, the riser 10 is inserted into the separator container 11 from below and in the illustrated embodiment generally extends upwards along the vertical axis of the chamber. The space 12 in the separator vessel around and above the risers constitutes the separator chamber. At its upper end, the riser 10 opens directly into the chamber 12 through an outlet opening or port 13 which conveniently forms an end opening perpendicular to the axis of the tube and the axis of the chamber 12. A downwardly deflecting cone 14 is disposed over the open end 13 of the riser 10. below the top of the separator container. Deflection cone 14 has the task of deflecting catalyst particles discharged through outlet riser 13 to prevent them from slipping off the upper end of the container and preventing particles from falling back into the riser through its open end, which could cause re-entry.

At a short distance from, but below the riser opening 13, at least one opening 17 is provided in the riser side wall. The preferred embodiment shown is a balanced or symmetrical structure in which the riser 10 has two side openings 17 diametrically opposed to each other and each leading to its own separate two-stage cyclone separator system, as shown in FIG. Third

More specifically, each side opening 17 over a side or transverse line 18 is connected to the inlet of a first cyclone stage 19. The cyclones can generally be of conventional type and are not part of the invention. However, it should be noted that the first cyclone stages are fed only through the side openings 17 and not through the chamber 12. Through the conduits 18, particles are introduced tangentially into the respective cyclones 19, where further separation between gas and particles occurs. The particles separated in the first cyclone stage 19 are discharged through downpipes 20, one of which is shown in FIG. 2, while the gaseous effluent is discharged at the top through gas outlet lines 21, which are connected to the respective cyclones 19 over expansion joints 22.

Conveniently, the upper end of the riser 10 is provided with outer bracing devices 25 to support the free-standing weight of the cyclone separators 19 which hang down therefrom. It is also advisable to place a shoe 26 at the side facing the riser to prevent the cyclone from resting against the wall of the riser.

The gas outlet lines 21 from the first cyclone stages 19 are each connected through conduits 27 to the inlet to cyclones 28 in a second stage. When two stage cyclones are used, each of the second cyclone stages 28 can be directly connected to the gas outlet 21 from a first cyclone stage 19. The conduits 27 constitute the only inlets to the second cyclone stages 28, i.e. these cyclones are not fed through or from the chamber 12. Expansion joints are provided to accommodate the varying expansion between the two cyclones. The downstream tubes 29 of the other cyclone, one of which is shown in FIG. 2, particles which are separated in the second stage dispense to the bottom of the separation chamber 12. The downpipe 29 should conveniently open above the base so as not to be clogged by it. The gas discharge pipes 30 from the other cyclone stages 28 extend through the separator vessel 11 and are connected to a collection line leading to fractionation devices not shown.

7 146032

The separation chamber 12 is pressurized since it is directly connected to the riser 10, but the outlet opening for the catalyst is covered by the catalyst base, which in this way limits the discharge of gas from the separator. Steam is introduced to facilitate the stripping process (see Fig. 1). The steam supply is very moderate, for example of the order of 680 kg / h at approx. 1 MPa. In addition to the small flow of steamer steam, which is carried upwards through the steamer, no significant gas flow through the separator chamber.

In operation, the internal pressure in chamber 12 prevents a substantial flow of gases through the riser end aperture 13. The catalyst particles, which have a relatively high density and small volume, are introduced by their moving energy into the separator chamber 12, but the gases deflect at an angle with the cyclones through the openings 17. The absolute largest portion of the catalyst is excreted as the gases bend sideways and the particles are ejected from the riser and these particles pass mainly past the cyclone system. A small portion of the particles are not excreted or reintroduced into the gas and introduced into the cyclone system. They are excreted mainly in the first or second cyclone, which is much less loaded than in the prior art. Through the cyclones, a pressure drop of approx. 14 kPa.

A sudden change of direction of the gas flow is important to achieve a separation since the particles do not change direction as quickly as the gas. In this connection, it is further advantageous to increase the velocity of the flow of gas and particles just upstream of the side openings 17. For this purpose, according to the invention, suitable nozzle devices in the form of a tapered neck or constriction in the riser are used, as shown by a narrowed portion 32 of FIG. 2. This constriction reduces the cross-sectional area of the conduit so that the current is accelerated during passage.

Alternatively or further, when using an asymmetric or unbalanced cyclone system, it is convenient to use a deflection plate, preferably in the form of the one shown in FIG. 4 deflecting plate 33 extending at an angle inward from the side wall of the riser just upstream of the side opening 17 and at the height of 8 86032 so that particles of bend from the side wall opening. The plate 33 conveniently forms an angle A with the side wall 10 of approx.

30 ° and has a length of approx. 15% of the pipe diameter. This further improves efficiency as shown below.

The advantage of the invention is further apparent from the following examples for comparison with known particle separation devices.

The data for runs 1-10 shown in Table I below is obtained with a separation device of the prior art type, in which the entire outflow from the riser is discharged through a side opening therein and through a side pipe directly to the inlet in a first cyclone stage. There was no end aperture and the entire amount of catalyst was introduced into the cyclone system. The gas outflow from the first cyclone stage was also discharged to the separation chamber, and a second cyclone stage was connected at its inlet to the interior of the chamber. Evaporation vapor from an external source was fed to the separation chamber.

The data set out in Table II below is obtained after the apparatus with data values as given in Table I was changed to include the construction of the invention.

Catalyst A consisted of an equilibrium mixture of silica and alumina in microspherical particles having a density of 0.72 g / cm 2. Catalysts B and C were of the same common type as Catalyst A, but with a space density of approx.

0.82 g / cm 2.

The values in Tables I and II are taken from yield summaries. When a trial number is followed by the letter A, the values given represent the average for a week instead of a day. In the tables, "catalyst conversion" means the amount of catalyst circulating through the riser. By "fractionator bottom flow" is meant the total flow from the fractionator bottom and the catalyst content is given in percent by volume of the fractionator bottom flow. By "catalyst loss" is meant the amount of catalyst that is not recovered by the cyclones, which assumes that all the catalyst entering the fractionator leaves it in the bottom stream. The catalyst losses in kg / day are calculated by determining the bottom stream frame in liters / day and multiplying by the volume percentage of the catalyst in the stream. The catalyst losses in kg / barrel of feed oil are calculated by dividing the catalyst loss per day by the inflowing amount of feed oil, expressed in barrel / day.

By comparing Tables I and II, it is seen that the catalyst losses are substantially reduced by the invention, while the amounts of feed oil can simultaneously be increased. From a comparison of the tests 11, 12 and 13 of the invention with the experiments 6-10 of the prior art, where the same type of catalyst was used in all cases, it is seen that the average loss per incoming barrel was reduced by 52%, while the amount of oil added at the same time increased by 13%. Furthermore, the temperature of the separation chamber could be increased to 560 ° C relative to the previous upper limit of 510 ° C, so that a better quality product was obtained.

The data set out in Table III below was obtained for a laboratory scale separator where the cracking catalyst is suspended in air instead of cracking gases and the values do not represent real cracking processes. In experiments A and B of Table III, the simulated stirrer in the separation chamber flowed through a T-shaped head with its upper end above the catalyst base at the bottom of the separator. The T-shaped piece had side openings and a bottom opening through which the gases were diverted directly to the chamber. The inlet to a first cyclone stage opens into the chamber and a second cyclone stage is fed directly from the outlet of the first cyclone stage. In experiments C and D, the outflow from the stirrer occurred through a T-shaped head piece, which was provided at plates at an angle of 45 ° at the outermost open ends of the arms to deflect the discharged material downward.

In experiment E, the riser opened through an open upper end to the chamber and was connected directly to the cyclone inlet of the invention through a side opening located near the end opening.

In the experiments referenced in Table III, as for the experiments in the following Table iv, the catalyst used was an FCC equilibrium catalyst with the following typical particle size distribution: 0-20 µm ϊ 0 wt% 0-40 µm: 8 wt% 0-80 µm: 70% by weight

The bulk density of the catalyst was 0.8 g / cm 2. The separation efficiency is 1 minus the quotient at the division of the amount of catalyst flowing into the first stage with the amount of catalyst fed to the riser.

In Table III, the amount of catalyst collected in the first cyclone downstream shows the completeness of the elimination process. According to the invention (experiment E), a much more complete recovery was obtained, providing a recovery of 1.05% in the first stage compared to recovery rates in other plants of 13.9 - 42%. Most notable was that the amount of catalyst remaining in the second cyclone recovery plant was very low, namely only 0.9 g.

Table IV shows the results obtained in the same simulated system by comparison between the invention (experiments F and G) and other known systems (experiments H - P). The structure used in Experiment F was the same as in Experiment E. In Experiment G, a similar structure was used where, however, in the riser a deflection plate was placed approx. 1/4 of the riser diameter below the side outlet opening, and as at an angle of approx. 45 ° with the riser axis extending beyond approx. 1/4 of the riser diameter. The purpose of this plate was to deflect particles away from the lateral gas discharge opening. The separator used in experiments H and I had the riser opening only at the inlet of the first cyclone step. The side tube did not open into the separation chamber and the gas outlet from the first cyclone stage opened into the separation chamber, while the second cyclone stage had its inlet directly open to the separation chamber. The length of the first stage downpipe was 2.5 cm, measured from the intersection H 146032 point between the cone-shaped piece and the downpipe. The separator used in Experiment J was similar to that used in Experiments H and I, however, the length of the downpipe was 60 cm. The separator in experiments K and L was the same, however the length of the downpipe was 45 cm. In experiments M and N, the stirrer in the chamber resulted in a T-shaped piece with downward opening openings. The two cyclone stages were connected in series with the inlet opening into the chamber above the tee. Experiments 0 and P were analogous to Experiments M and N except that a cruciform piece was used for the end of the stirrup instead of a T-shaped piece. The cross was provided with four short horizontal arms perpendicular to each other and with downward outflow openings, and the riser was connected to the center of the cross.

A comparison of the experiments F and G in Table IV shows that the use of a deflection plate significantly increases the separation efficiency of the first cyclone stage (from 80,690 to 93%). In both of these experiments, high excretion rates were obtained for the first cyclone stage compared to experiments Η, I, J, K and L, where nothing is excreted prior to the first cyclone step because the entire outflow from the stirrer was introduced directly into the first cyclone stage without any previous separation. .

The degree of excretion achieved before the first cyclone stage in Tests Μ, N, 0 and P was good, but the separation efficiency of the tested plants varied greatly when the surface of the catalyst base at the bottom of the separation chamber was less than 10 cm below the cruciform or T-shaped piece at the end of the riser. As a result of this instability, such plants will not exhibit uniformly good separations if used industrially, where the distance between the foundation and the cruciform portion is almost inevitably expected to vary substantially during normal operation. In comparison, by means of the invention good degrees of excretion are obtained regardless of the height of the base, as long as the downpipe is uncovered.

In the examples cited, the stirrer was introduced into the separation chamber through an opening in its bottom and the cyclones physically placed within the chamber. However, it is understood that the stirrer is not required to be introduced into the separator chamber through its bottom, but that it may be inserted through the side or even the top of the chamber and that the cyclones may be physically located outside the separation chamber, which may be advantageous for plants where no hydrocarbons are converted. It is not the physical placement of the cyclones in relation to the separation chamber that matters, but the fact that the riser opens through an end opening in the separation chamber and that it feeds the inlet of a cyclone through a side opening just upstream of the end opening, regardless of whether the cyclone is located inside or outside the separation chamber.

The invention is described above mainly for the purpose of hydrocarbon conversion processes. It is to be understood that the invention may also be used in conjunction with other gas phase catalytic chemical reactions, in which catalyst particles are contacted with chemical compounds suspended in a fluid stream through a reactor tube, and in other cases where either solid or liquid particles form must be separated from gases.

Examples of other applications in which the process and apparatus of the invention can be expected to be particularly useful include gasification of coal, desulfurization of solid fuels, and heat exchangers in which hot catalyst particles are mixed with inlet gases to heat them while cooling the catalyst.

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Claims (5)

17 146032 Patent claims: A method of separating catalyst particles from the cracked hydrocarbons by catalytic cracking of petroleum hydrocarbons which, together with the catalyst particles, in an upward flow, passes through an elongated tubular reaction zone, characterized in that the particles, by utilizing their motion energy alone, , is discharged to a separation chamber which, under stable operating conditions, is free of gas flow through an opening located opposite the downstream end of the reaction zone, while the flow of cracked hydrocarbons with residual amounts of catalyst particles upstream of this opening is fed into a cyclone separator. Process according to claim 1, characterized in that the hydrocarbon stream is fed into the cyclone separator with a flow direction which is substantially perpendicular to the flow direction of the discharged particles. Process according to claim 2, characterized in that the flow of hydrocarbons and particles is accelerated upstream of the point at which the hydrocarbons are discharged to the cyclone separator. Process according to claim 3, characterized in that catalyst particles with a maximum size of approx. 100 jim and the majority of which is in the 40-80 Jim range. Apparatus for separating catalyst particles from the cracked hydrocarbons by catalytic cracking of petroleum hydrocarbons, characterized in that it comprises partly a chamber (12) arranged for collecting the separated particles and during the continuous separation substantially free of gas flow and partly a gas stream. elongated tube (10) whose downstream end (13) flows freely into the chamber (12) and through which the hydrocarbons and particles