The method is carried out in the reactor bubble column with purge tube, and a regeneration process of the contained catalyst

 

(57) Abstract:

A continuous method of obtaining mainly heavy hydrocarbons from synthesis gas, in the presence of a gas phase, a liquid and a solid catalyst, and the above process is carried out using a bubble column. Bubble column includes at least one purge pipe; at least one device for the inlet of the synthesis gas; at least one device for intake regenerating gas; at least one device that generates/interrupts the flow of regenerating gas, and an optional device required to minimize mixing the synthesis gas from the regenerating gas. The technical result is a simplification of the process. 2 S. and 11 C.p. f-crystals, 5 tab., 1 Il.

The invention relates to a reactor bubble column equipped with a purge pipe that can be used in three-phase slurry processes, more specifically in the Fischer-Tropsch process.

The present invention also relates to a method of regeneration of catalysts, partially and reversibly deactivated carried out in the above reactor.

Suspension of catalytic processes, i.e. work in t is alistar, in particular the Fischer-Tropsch process, have the disadvantage of being more or less pronounced reversible deactivation of the initial catalytic activity of the catalyst. This deficiency usually eliminate by means of the regeneration of the exhausted catalyst.

European patent And 590882 describes a method for regenerating catalyst for synthesis of hydrocarbons containing cobalt or ruthenium, undergoing partial reversible deactivation during suspension of synthesis. This method ensures the recovery of at least 80% of the initial activity of the catalyst.

The above method involves performing the regeneration of the catalyst directly on the spot suspension reactor by periodically stopping the flow of process gas (synthesis gas) and enable the flow of gas containing hydrogen and other inert gases, excluding the presence of components such as carbon monoxide, capable of reaction with hydrogen.

The method described in European patent And 590882 has, however, a disadvantage in the periodic interruption of the synthesis of hydrocarbons to replace the process gas a gas containing hydrogen.

U.S. patent RA within one or more thin tubes, located inside the reactor bubble column, with the proportion of the column occupied purge pipes, was preferably less than 10%. Unlike what is described in the European patent And 590882, this solution does not include the cessation of synthesis gas.

It is also known that, in the case of reactions in three-phase systems the reactor bubble column equipped with a purge pipe is more preferable in comparison with a simple reactor bubble column with respect to the distribution of the solid phase in a three phase system.

Now found a specific configuration of the bubble column equipped with a purge pipe that does not have the above disadvantages.

The application of this specific configuration in bubble columns allows the regeneration of the partially deactivated catalyst in place (more specifically, between the reactor and purge pipe), thus eliminating the periodic interruptions in the supply of process gas.

In addition, the reactor according to the present invention achieve better homogenization of the phases in comparison with the reactor bubble column, which ispol get mostly heavy hydrocarbons, alternative fuel, means for increasing the octane number, chemicals and chemical intermediates of the synthesis gas in the presence of a gas phase, a liquid and a solid catalyst, and the above process is carried out using a reactor bubble column equipped with a cooling device, and includes periodic internal regeneration reversible partially deactivated catalyst and the regeneration is carried out in the presence of regenerating gas, when this bubble column contains:

(a) at least one purge pipe, consisting of essentially vertical cylinder, having a smaller size than the column, in which both the lower and upper ends are open, completely immersed in the liquid phase, containing solid matter in suspension;

(b) at least one device for the inlet of the synthesis gas, preferably gazoraspredelitel, preferably located in the lower part of the bubble column;

(c) at least one device for intake regenerating gas, preferably gazoraspredelitel, preferably located in the lower part of the gap between the purge tube and the inner wall of the reactor;

(d) on the s device, necessary to minimize mixing the synthesis gas with a regenerating gas, preferably air vents, preferably installed near the bottom of the hole purge pipe.

The term "regenerating gas" means a gas, usually hydrogen, possibly diluted with inert gases used for recovery - regeneration reversibly deactivated solid catalyst, preferably containing at least one metal of group VIII, preferably selected from cobalt and iron, preferably cobalt.

The configuration of the reactor bubble column according to the present invention provides a regeneration of the catalyst without interrupting the flow of the reacting gases.

The drawing represents a non-limiting example of an embodiment of the present invention.

Reference numbering indicates the following:

1 - inlet line synthesis gas,

2 - supply line regenerating gas for regeneration of the catalyst,

3 - lateral line of the gaseous products (preferably, light hydrocarbons) and areagirls components,

4 - discharge line liquid products,

5 - lead line coolant,

6 - lateral face between the purge pipe and reactor

9 - cooling device located inside the blowdown pipe,

10 is a device for the inlet of the synthesis gas,

11 is a device for intake regenerating gas,

12 - the deflectors,

13 - valve for the formation/interrupting the flow of regenerating gas catalyst

14 - the level of dispersion (gas-liquid-solid).

In the drawing there are also arrows that indicate the direction of movement of the internal circulation of the liquid, which is set purge pipe, when interrupted, the gas stream containing hydrogen.

Shown in the drawing the reactor bubble column contains the purge pipe (7) located essentially vertically, which uses process gas as a carrier. This device consists essentially of a vertical cylinder with a smaller size than the reactor bubble column, which is placed inside the column vertically, open at both ends and completely immersed in a liquid containing solid matter in suspension. This allows the liquid and solid matter in suspension to circulate through the cylindrical device and the gap on the outside of the cylinder, if the driving force produced by under the should be such as to the lower end was located preferably directly above the lower part of the reactor, while the upper end was located directly beneath a free surface of the suspension, the solid-liquid containing gas.

Synthesis gas containing carbon monoxide and hydrogen, is passed into the lower part of the reactor through a device, preferably the dispenser (10). The geometry of the distributor and the distance between the purge pipe and the lower part of the column appropriately chosen to ensure the passage of the process gas inside the cylindrical device, thus exclude the selected path in the area of the gap. The reaction of the Fischer-Tropsch synthesis takes place inside a cylindrical device.

Regeneration of the catalyst takes place using the regenerating gas, preferably hydrogen, at high temperatures and pressures corresponding to the temperatures and pressures adopted for Fischer-Tropsch synthesis. The hydrogen is supplied in the form of a stream of gas; this stream may contain inert gases, such as methane or other light hydrocarbons (C2-C10). Preferably, they contain no carbon monoxide or other components that Moto above, the above configuration of the bubble column provides regeneration of the deactivated catalyst in place.

Another object of the present invention is a method of regeneration on the site of reversible partially deactivated solid catalyst mainly containing metals of group VIII, preferably selected from cobalt and iron, including the use of the reactor under item 1 providing a continuous supply of the synthesis gas during regeneration, which includes:

(i) the first stage of catalyst regeneration, in which the regenerating gas containing hydrogen, fills the gap between the reactor and purge pipe, in a period of time which is sufficient for the regeneration amount of the exhausted catalyst suspended in the liquid contained in the interval, and the velocity of the stream containing hydrogen gas is such that the balance of hydrostatic pressure between the purge zone of the pipe and the area of the gap;

(ii) a second stage in which the gas containing hydrogen, is discontinuous, and the circulation of liquid containing solid matter in suspension, again set using the purge pipe; in this way the regenerated catalyst, the floor is torenia stages (i) and (ii) is preferably as long until it reaches the full regeneration of the catalyst contained in the reactor column.

The term "regeneration of the catalyst" means a recovery of at least 80% of the initial catalytic activity of the catalyst.

At stage (i) it is preferable that was minimized circulation of the suspension liquid-solid and gas between the cylindrical device and the gap; this is achieved by influencing the flow rate of gas containing hydrogen that fills the gap to achieve the balance of hydrostatic pressure between the two areas.

Deflectors appropriate form set in the lower orifice of the purge pipe, in order to minimize the mixing of the two gas streams, the process gas stream and the stream containing hydrogen for regeneration.

At stage (ii) interrupt the flow of regenerating gas, again set the circulation of liquid containing solid matter in suspension, using the purge pipe and the process gas flow rate which remains basically the same, and it depends solely on the established operating conditions and process conditions.

The reg is the dominant gas, preferably passing through suitable control valves, preferably located at the bottom of the hole of the annular gap.

Establishing a forced circulation of a liquid containing solid matter in suspension, between the purge pipe and interval allows a new portion of the exhausted catalyst suspended in a liquid containing mainly hydrocarbons obtained in the synthesis process, enter the interval, replacing thus the suspension containing the regenerated catalyst.

"Regenerated catalyst" through the movements carried out by using the purge pipe, leaving a gap to enter into the reaction zone (inside the blowdown pipe) through the hole in the lower part, while the portion of the exhausted catalyst passes from the reaction zone in the gap where regeneration occurs through the upper hole.

When the gap is fully updated, ends one cycle of regeneration, and the flow of regenerating gas in the gap opens again, starting a new cycle of regeneration.

During both stages (i) and stage (ii) continuously reaction occurs Fischer-Tropsch inside of cylindrial gas.

The regeneration cycle begins when the activity of the catalyst deteriorates to a certain level, for example 50%, and stops when the catalyst restores the desired catalytic activity, preferably after regeneration, at least 80%, even more preferably at least 90% of its original catalytic activity.

When the regeneration cycle and the recovery of the regenerated portion does not occur in the reactor according to the present invention, the reactor column operates with a constant internal circulation of liquid containing solid matter in suspension, due to the purge pipe, permanently installed inside the reactor.

As is well known to specialists in this area, internal circulation contributes to the distribution of solids in the suspension fluid, which otherwise can only be achieved by means of gas bubbles coming near the bottom of the column, thus making a concentrated catalyst composition more homogeneous.

Thanks ekzotermicheskie as the reaction of the Fischer-Tropsch synthesis and regeneration, in order to set the temperature control and almost izotermicheskie, out of tube bundles, coils or other types of heat exchange surfaces immersed in the slurry (suspension). In the reaction of the Fischer-Tropsch synthesis is essential temperature control, because temperature directly affects the selectivity of the reaction; in addition, it is important to protect the catalyst from unwanted overheating, which may damage it.

Internal regeneration of the catalyst is preferably occurs under the same conditions of temperature and pressure, and the reaction of the Fischer-Tropsch synthesis. In any case, it is possible independent control of the temperature within the reaction zone and the regeneration zone.

Conditions, in particular temperature and pressure, to processes for the synthesis of hydrocarbons generally well known. The temperature may be between 150 and 380oC, preferably from 180 to 350oS, even more preferably from 190 to 300oC. the Pressure is generally higher than about 0.5 MPa, preferably from 0.6 to 5 MPa, more preferably from 1 to 4 MPa.

In the preferred embodiment of the present invention, i.e. in the synthesis of hydrocarbons by reduction WITH, the solid particles are at least partially composed of catalyst particles, wybraniec. Any catalyst for Fischer-Tropsch synthesis, especially based on iron or cobalt, may be used in the method of the present invention. Preferably used catalysts based on cobalt, in which the cobalt is present in an amount that is sufficient in order to be catalytically active in the reaction of the Fischer-Tropsch process. The cobalt concentration can usually be at least about 3%, preferably from 5 to 45% by weight, more preferably from 10 to 30% by weight, relative to total weight of catalyst. Cobalt and possible promoters dispersed in a carrier, such as silicon oxide, aluminum oxide or titanium oxide. The catalyst may contain other oxides, such as oxides of alkali, alkaline earth and rare earth metals. The catalyst may also contain other metal, which can be active as a catalyst for the Fischer-Tropsch process, for example a metal of group 6 or 8 of the periodic table of elements, such as ruthenium, or may be a promoter, such as molybdenum, rhenium, hafnium, zirconium, cerium, or uranium. The promoter metal(s) is typically present in amount in relation to the cobalt, at least to 0.05: 1, preferably, the thin honey powder, usually having an average diameter between 10 and 700 μm, preferably from 10 to 200 μm, even more preferably from 20 to 100 μm. The above catalysts are used in the presence of a liquid phase and a gas phase. In the case of the Fischer-Tropsch synthesis of liquid phase can be composed of any inert liquid such as one or more hydrocarbons having at least 5 carbon atoms in the molecule. Preferably the liquid phase consists mainly of saturated paraffin or olefin polymers having a boiling point above about 140oWith, preferably above approximately 280oC. in Addition, the corresponding liquid medium may consist of paraffins obtained in the reaction of the Fischer-Tropsch process in the presence of any catalyst, preferably having a boiling point above about 350oC, preferably from 370 to 560oC.

Download solid substance or the amount of catalyst in relation to the volume of suspension or solvent can reach up to 50%, preferably from 5 to 40%.

In the case of the reaction of the Fischer-Tropsch incoming gas containing carbon monoxide and hydrogen may be diluted with other gases, usually up to a maximum of 30% of the volume, preferably hydrogen and carbon monoxide, it can vary within wide limits. In the preferred embodiment it is between 1:1 and 3:1, even more preferably from 1.2:1 to 2.5:1.

Regenerating treatment increases the activity of the synthesis of the catalysts of hydrocarbons, reversible and partially deactivated, regardless of the process in which they were received.

The following examples provide a better understanding of the present invention.

EXAMPLES

Example 1 describes the conditions necessary for regeneration of the catalyst inside the bubble column with a purge pipe without interrupting the process of synthesis of hydrocarbons, with the known geometry of the reactor and the operating conditions under which the process takes place.

In example 1, used industrial reactor with a diameter of 10 meters, are equipped with a purge pipe with a diameter of 9.5 m, and the flow rate of gas containing hydrogen, which must be submitted at the base of the annular gap is calculated relative to the speed of the process gas stream. In example 1 investigated three cases: surface speed of the process gas 0,2, 0,3, 0,4 MS-1in relation to the entrance part of the purge pipe.

In example 2, are supported on the same conditions as ofany cases with diameters of 6.5, 8.5 and 9.5 m, while the surface speed of the process gas, in relation to the plot purge pipe remains constant and equal to 0.3 MS-1. As in example 1, the flow rate of gas containing hydrogen, which must be submitted at the base of the annular gap is calculated at this time relative to the diameter of the purge pipe.

Example 1. How to conduct internal regeneration of the catalyst in the reactor bubble column without interrupting the process gas stream in continuous synthesis of hydrocarbons.

I. the influence of the flow rate of process gas.

In order to ensure that the regeneration of the catalyst takes place without interruption of the Fischer-Tropsch synthesis inside the reactor bubble column equipped with a purge pipe, you need to avoid:

(a) a gas stream containing hydrogen, which is introduced into the hole of the annular gap and come into contact with the process gas containing CO, which reacts with hydrogen, as it is in the process of synthesis inside the blowdown pipe, which prevents the regeneration of the catalyst;

(b) a liquid containing solid matter in suspension is circulated through the purge pipe and prema suspension, in which regeneration occurs, even if the gas stream containing hydrogen, periodically interrupted in order to re-establish a forced circulation created by using the purge pipe, and to update the download (or volume) of sediment, which must be regenerated, inside the annular gap.

In order to satisfy the above requirements in addition to the above, the distribution of process gas and a gas containing hydrogen, it is necessary to minimize the circulation of liquid containing the catalyst in suspension; to achieve this, the difference of the hydrostatic pressure (which is the driving force in the circulation of the liquid between the gap and the purge pipe must be reduced to zero:

< / BR>
where Rn- the difference in hydrostatic pressure between the gap and the purge pipe, PA;

d- delay of gas in the purge pipe;

a- delay of the gas in the gap;

the density of the gas phase, KGM,-3;

the density of the suspension phase, KGM,-3;

g - free fall acceleration, MS-1;

H - the height of the free surface of the variance in relation to the bottom of the column, m

In the equality (I) the site is that the density of the process gas is comparable with the density of the gas, containing hydrogen for catalyst regeneration.

In order to minimize the difference of hydrostatic pressure, taking into account that the density of the suspension at least an order of magnitude exceeds the gas density, and that, therefore, their difference is always the final value must be the same delay gas as purge tube, and in between;

d=a. (II)

The above equation (II), when the reaction conditions, the geometry of the reactor bubble column, including purge pipe, and the flow rate of the process gas is installed, can be performed only at a certain velocity of the gas stream containing hydrogen that fills the gap.

In order to describe the delay of gas in the purge pipe and between applied hydrodynamic model from the literature (Krishna and others, journal 43, 1997, S. 311-316), suitable for bubble columns in the presence of system gas-liquid-solid from the suspension phase in "periodic" conditions, which allows to estimate the delay of gas depending on the properties of the system, the diameter of the column and superficial gas velocity. As for the annular area between the two, he srawniwa model from the literature were applied to the reactor bubble column, working in the mode of heterogeneous flow, which is typical for industrial scale reactors, as is well known to specialists in this field. Heterogeneous mode can be represented using a generalized two-phase model, in which one phase, called "diluted", consists of part of the gas which passes through the reactor in the form of large bubbles. The second phase (dense phase) can be represented in the liquid phase, in which the suspended solid particles, and the remaining part of the gas in the form of small finely dispersed bubbles. Large bubbles have a higher rate of climb than small bubbles, can essentially be considered as being in the flow of the displacement. Dense phase consisting of liquid, suspended solids and small finely dispersed bubbles, has a certain level of back-mixing, which depends on the operating conditions of the process and diameter of the column. Hydrodynamic model from the literature, which is based on a large number of experimental results also suggests that the dependence of the delay of gas from the diameter of the column is valid when the diameter of the column of 1 m, for large diameters that impact mill is not exposed to the phenomenon, known as the "wall effect".

Considering the reactor industrial scale bubble column with a diameter of 10 m, in which the height of the suspension dispersion containing gas equal to 30 m, inside which there is a thin tube with a diameter of 9.5 m and a height of 29,8 m, located at a distance of 10 cm above the bottom part of the column coaxial, explore the flow rate of gas containing H2that satisfies the equalities (I) and (II), depending on the flow rate of the process gas used for the synthesis of hydrocarbons. The results for the three cases in which the surface speed of the process gas in relation to the plot purge pipe equal to 0.2, 0.3 and 0.4 m/s, are presented in table 1. In the above table also presents the delay of the gas, which is equal, by definition, in the purge pipe and in the interval, where the regeneration of the catalyst. Table 2 on the other hand shows the flow velocity of the liquid containing solid matter in suspension, which circulates through the gap and purge tube when the gas stream containing hydrogen, in between stops, for the same cases described in table 1. These flow rate of a fluid get determined, which satisfies the energy balance:

PN=PLOSS(III)

where Rnrepresents the difference in hydrostatic pressure between the gap and the purge pipe in PA, whereas PLOSSdenotes the full pressure drop in the reactor bubble column reactor with a purge pipe, which is obtained by summing the pressure drops due to friction in the gap in the purge pipe and the upper and lower parts of the purge pipe, where a sharp decrease and increase in size and the inversion of the flow direction of the mist.

Reaction conditions for all cases the following: 230oC and 3 MPa, the concentration of catalyst 35 % of the volume, the density of the suspension 906 KGM-3.

Example 2. How to conduct internal regeneration of the catalyst in the reactor bubble column without interrupting the process gas stream in continuous synthesis of hydrocarbons.

II. The influence of the diameter of the purge pipe.

In this example takes the same assumptions as in example 1, but instead of changing the surface speed of the process gas is changed, the diameter of the purge pipe. As in the previous example, the diameter of the column industrial scale is 10 m, the height of suspense is,8 m, the distance between the lower end of the purge tube and the lower part of the column is chosen constant and equal to 10 cm Superficial velocity of the gas relative to the free area inside the blowdown pipe is set to 0.3 MS-1while the working pressure and process temperature synthesis of hydrocarbons, as in the previous example, is 3 MPa and 230oC.

The flow rate of gas containing hydrogen, which satises the equalities (I) and (II) of example 1 is examined in relation to the diameter of the purge pipe, Dd. Results for three different values of the diameter of the purge pipe to 6.5, 8.5 and 9.5 m are presented in table 3, together with part of the area occupied by the gap in relation to the total area of the column (%).

As can be seen from the results shown in table 3, when the diameter of the purge pipe 6.5 and 8.5 m surface speed, which must have a gas containing hydrogen to satisfy the equalities (I) and (II) equal to the velocity of the process gas. The reason for this is that for both cases the hydraulic diameter, corresponding to a period of more than 1 m, therefore, the equality (II), for the assumptions specified in example 1, is independent of the diameter and the purge pipe is the same, the equality (II) is satisfied for the same system GAA-liquid-solid only when the surface speed of the two gases are the same.

When the gas stream containing hydrogen, stops and re-starts the internal circulation of liquid containing solid matter in suspension, the flow rate of the circulating suspension, obtained for the same cases as in table 3, are shown in table 4.

As you can see from the data presented in table 4, increasing the diameter of the purge pipe leads to an increase in the circulation of the suspension, similar to what happens when increasing the flow rate of synthesis gas while maintaining a constant diameter purge pipe (see table 5).

In order to maximize the reaction volume in relation to the regeneration zone, the interval should be reduced with the increase, with the same external diameter of the reactor, the diameter of the purge pipe.

However, if the diameter of the purge pipe is increased more than the allowable limit value, there is a sharp drop in the circulation flow rate of suspended solids (see table 5). This means that the effect of thrust caused by the presence of purge pipe decreases, whereas opredelennyuyu, that in order to obtain a sufficient circulation of the suspension should choose purge pipe diameter less 9,8 m

Conditions in table 5 are the same as in table 4.

1. A continuous method of obtaining mainly heavy hydrocarbons, alternative fuel, means for increasing the octane number, chemicals and chemical intermediates of the synthesis gas in the presence of a gas phase, a liquid and a solid catalyst, and the above process is carried out using a reactor bubble column equipped with a cooling device, and includes periodic internal regeneration reversible partially deactivated catalyst and the regeneration is carried out in the presence of regenerating gas, characterized in that the bubble column is within: (a) at least one purge pipe, consisting of essentially vertical cylinder, having a smaller size, than the column, in which both the lower and upper ends are open, completely immersed in the liquid phase, containing solid matter in suspension; (b) at least one device for the inlet of the synthesis gas; (c) at least one device for intake regenerating gas; (d) less is required to minimize mixing the synthesis gas from the regenerating gas.

2. The method according to p. 1, characterized in that the purge pipe fitted coaxially in relation to the bubble column.

3. The method according to p. 1, characterized in that the device (b) inlet synthesis gas is gazoraspredelitel.

4. The method according to p. 1, characterized in that the device (b) inlet synthesis gas is placed in the lower part of the bubble column.

5. The method according to p. 1, characterized in that the device for intake regenerating gas (C) is gazoraspredelitel.

6. The method according to p. 1, characterized in that the device for intake regenerating gas (C) is placed in the lower part of the gap between the purge tube and the inner wall of the reactor.

7. The method according to p. 1, characterized in that the device (s) required to minimize mixing the synthesis gas from the regenerating gas are deflectors.

8. The method according to p. 1, characterized in that the device (s) required to minimize mixing the synthesis gas with a regenerating gas, set near the bottom of the hole purge pipe.

9. The method according to p. 1, characterized in that the purge pipe (a) has the end come directly under the free surface of the suspension, the solid - the liquid containing solid matter.

10. The method according to p. 1, characterized in that the receiving mainly heavy hydrocarbons.

11. The method of regeneration on the site of reversible partially deactivated solid catalyst mainly containing metals of group VIII, preferably selected from cobalt and iron, including the use of the reactor under item 1 providing a continuous supply of the synthesis gas during regeneration, which includes: (i) the first stage of catalyst regeneration, in which the regenerating gas containing hydrogen, fills the gap between the reactor and purge pipe, in a period of time which is sufficient for the regeneration amount of the exhausted catalyst suspended in the liquid contained in the interval, and the velocity of the stream containing hydrogen gas, that is, that is, the balance of hydrostatic pressure between the purge zone of the pipe and the area of the gap; (ii) a second stage in which the gas containing hydrogen, is discontinuous, and the circulation of liquid containing solid matter in suspension, again set using the purge pipe; in this way the regenerated catalyst obtained in stage (i), replace the depleted catalysis fact, what's on stage (i) regenerating gas containing hydrogen, served with the bottom of the gap between the reactor and purge pipe.

13. The method according to p. 11, characterized in that stage (i) and (ii) repeat to achieve complete regeneration of the catalyst contained in the reactor column.

 

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SUBSTANCE: natural gas is brought into reaction with vapor and oxygen-containing gas in at least one reforming zone to produce syngas mainly containing hydrogen and carbon monoxide and some amount of carbon dioxide. Said gas is fed in Fisher-Tropsh synthesis reactor to obtain crude synthesis stream containing low hydrocarbons, high hydrocarbons, water, and unconverted syngas. Then said crude synthesis stream is separated in drawing zone onto crude product stream containing as main component high hydrocarbons, water stream, and exhaust gas stream, comprising mainly remained components. Further at least part of exhaust gas stream is vapor reformed in separated vapor reforming apparatus, and reformed exhaust gas is charged into gas stream before its introducing in Fisher-Tropsh synthesis reactor.

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7 cl, 3 dwg, 1 tbl, 5 ex

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