JPS58127707A - Method and apparatus for catalyst supply - Google Patents

Abstract

PURPOSE:To supply a high-concentration catalyst smoothly to a reaction vessel, by disposing a rotating body having two uncrossed passages in a carrier fluid flowing into the reaction vessel, and filling one passage with the high-concentration catalyst while allowing the carrier fluid to pass through the other passage. CONSTITUTION:A storage tank 6 holding a high-concentration slurry catalyst 7 is pressurized with inert gas to maintain the inside under a pressure somewhat higher than that in the polymerization vessel 3. The carrier supply line 9 is connected to the catalyst supply line 2 by putting, in position, a first passage 31A of the rotating body 12 of a catalyst supply apparatus 1 to supply the carrier fluid to the vessel 3 and, at the same time, the second passage 31B is connected to the catalyst inlet line 5 to fill the passage with the catalyst 7. The extra portion of the catalyst is returned to the storage tank 6 through a line 8. Then, the rotating body 12 is rotated to bring lines 9 and 2 and lines 5 and 8 into the state of disconnection to discharge the carrier fluid within the passage 31A into a discharge line 10. Then, the rotating body 12 is rotated and the lines 9 and 2 are connected to each other through the passage 31B. The catalyst 7 is pushed foward by the carrier fluid and supplied to the tank 3.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for feeding a catalyst total reactor and an apparatus for its implementation.

Conventionally, Ziegler catalysts used for producing polyolefins, for example, have generally been supplied by pumping. In this type of catalyst supply method using a pump, if the concentration of the catalyst slurry is high, the catalyst supply line will be clogged, and if the concentration is high, it will be difficult to supply the catalyst in a constant quantity, making it impossible to supply the catalyst smoothly. However, the catalyst had to be diluted with an inert solvent before being supplied. However, if the catalyst is diluted with an inert solvent, the catalytic activity will decrease due to impurities in the inert solvent, and it is necessary to completely separate and remove the inert solvent in the post-treatment process, which requires a lot of energy. However, it also had the disadvantage of going against the call for resource conservation.

The purpose of the present invention is to achieve a high total catalyst concentration. 1. To provide a method and a device for supplying a catalyst to a reaction tank smoothly. The supply method according to the present invention has two catalysts that do not intersect with each other during the flow of a carrier fluid flowing into a reaction tank. All rotating bodies having flow channels are arranged, and when the carrier fluid is flowing through one channel, the high concentration catalyst is filled in the other channel, and the rotating bodies are rotated fully to flow into the carrier fluid. In order to achieve the above object, the high concentration catalyst is appropriately supplied to the reactor, and the high concentration catalyst is transported by a carrier fluid and supplied to the reaction tank.

Further, the feeding device according to the present invention has a rotating body yca that has first and second flow paths that do not intersect with each other, and rotates the paper as needed, and when this rotating body is located at a predetermined rotation angle, the first A flow path connects a carrier fluid inlet into which a carrier fluid flows and a catalyst supply line that supplies a catalyst to a reaction tank to form a flow of the carrier fluid to the reaction tank, and a second flow path has a catalyst A catalyst inlet that communicates with the storage tank is communicated so that the catalyst is filled in this flow path, and when the rotating body is rotated by a predetermined rotation angle from this state, the first flow path removes the carrier fluid. The carrier fluid in the flow path is removed to the outside of the flow path by being communicated with the carrier fluid discharge port, and when the rotating body is further rotated by a predetermined rotation angle, the second flow path is connected to the carrier fluid inlet and the catalyst. The catalyst in the second flow path communicating with the outlet is supplied to be replaced by the carrier fluid in the flow of the carrier fluid flowing into the reaction tank, and the catalyst is carried by the carrier fluid and connected to the catalyst supply line. In order to achieve the above object, the catalyst is supplied to the reaction tank through the catalyst, and the first flow path is connected to a catalyst inlet to be filled with the catalyst.

Embodiments of the present invention will be described below with reference to all the drawings.

FIG. 1 shows process steps when an embodiment of the catalyst supply device according to the present invention is applied to a polymerization reaction process. In this figure, a catalyst supply device 1 is connected to a polymerization reaction tank 3 as a reaction tank via a catalyst supply line 2, and a co-catalyst is appropriately supplied to a predetermined position of the catalyst supply line 2 from a co-catalyst supply line 4. It has become so.

Further, a catalyst storage tank 6 is connected to the catalyst supply device 1 via a catalyst inflow line 5, and the catalyst 7 in the catalyst storage tank 6 is supplied to the catalyst supply device 1.
The catalyst is then returned to the catalyst storage tank 6. Further, a carrier fluid supply line 9 and a carrier fluid removal line 10 are connected to the catalyst supply device 1 .

FIG. 2 shows the external appearance of the catalyst supply device 1, and FIGS. 3 and 4 show a partially cutaway front view and a partially cutaway right side view of the main parts, respectively. . In these figures, a truncated cone-shaped valve body 12 as a rotating body is fitted into a substantially thick-walled cylindrical main body 11 so as to be rotatable in the axial direction, and the catalyst supply device 1 is configured in a so-called rotary pulp type. .

The main body 11 has a carrier fluid inlet 13 and a catalyst outlet 1.
4 indicates all the valve bodies 1 on the same virtual straight line along the horizontal direction in the figure.
A round catalyst inlet 15 and a catalyst return port 16 are provided facing in opposite directions centering on the valve body 12 and facing in mutually opposite directions centering on the valve body 12, and the carrier fluid inlet 13 and catalyst outlet 14 It is provided on the same virtual horizontal plane as the carrier fluid inlet 13 and the catalyst outlet 14 in the angular direction. Here, the carrier fluid inlet 13 is provided with a carrier fluid supply line 97jX.

A catalyst supply line 2 is connected to the catalyst outlet 14 and a catalyst inlet 1 is connected to the catalyst supply line 2.
A catalyst inflow line 5 is connected to the catalyst inlet 5, and a catalyst return line 8 is connected to the catalyst return port 16.

The valve body 12 is housed in a cylindrical hollow part 21 provided at the center of the main body 11, and four conical parts 22 are formed at the center of the bottom surface of the valve body 12. The valve body 12 is rotatably supported by the carbide pole 23 inserted by a predetermined amount. The carbide ball 23 is inserted by a predetermined amount into the four conical portions 25 formed in the upper end surface of the disk-shaped bearing material 24 located below the valve body 12, and the bearing material 24 which has been twisted is A compression coil spring 27 interposed between the lid 26 attached to the lower part of the main body 11 and the bearing material 24 urges the valve element 12 upward in the figure. It is strongly supported.

A short cylindrical guide ring 28 is fitted and fixed on the outer periphery of the valve body 12, and this guide ring 28 guides the rotation of the valve body 12 in the hollow portion 21, and also guides the rotation of the valve body 12 within the hollow portion 21.
The vertical movement amount of 2 is regulated. Further, a communication hole 29 is bored at a predetermined position of the guide ring 28 .

The valve body 12 has a first flow path 31A and a second flow path 31B.
are bored inside the valve body 12 so that they do not intersect with each other. These two channels 31A and 31B are arranged to face each other in a vertical direction when viewed from above in the figure, and the openings at both ends of the channels 31A and 31B are located at approximately the same height on the outer periphery of the valve body 12. They are arranged at intervals of 90 degrees from each other along the circumferential direction. These channels 31A, 3
When the valve body 12 is positioned at the rotation angle shown in FIG.
The catalyst inflow port 15 and the catalyst return port 1 are
When the valve body 12 is rotated by 90 degrees from this rotation angle, the catalyst inlet 15 is opened by the first flow path 31A.
and the catalyst return port 16 are communicated with each other, and the carrier fluid inlet 13 and the catalyst outlet 1 are communicated with each other by the second flow path 31B.
4 are communicated. The communication holes 29 of the guide ring 28 are provided at the openings at both ends of the flow paths 31A and 31B.
The flow of the catalyst 7 and the carrier fluid is not obstructed by this.

As shown in FIGS. 5 and 6, a carrier fluid discharge port 41 is provided at an intermediate position between the carrier fluid inlet 13 and the catalyst inlet 15 of the main body 11, and the valve body 12 is rotated at a predetermined rotation angle. When the flow path 31A or 31B is located at , the flow path 31A or 31B is communicated with the carrier fluid removal line 10 via the joint 80.

A stem 51 is provided on the valve body 12, and this stem 51 is rotatably supported by the main body 11 via an O-ring 52. As shown in FIGS. 2 and 3, the stem 51 is connected to a drive shaft 54 via a ratchet 53, and when the drive shaft 54 is rotated by an actuator 55 serving as a drive source, the stem 51 is also rotated. However, the ratchet 53 allows the stem 51 to always rotate in one direction only, and in this embodiment, the valve body 12 only rotates counterclockwise when viewed from above in the figure. There is.

The main body 1 is disposed above the ratchet 53 via a yoke 61.
A control section 56 supported on the upper part of 1 is provided. In addition to a limit switch 57 that detects the rotation speed of the drive shaft 54, the control unit 56 includes a solenoid valve 58, an actuator 55,
A speed controller 60 is provided, and the valve body 12 is rotated or stopped as appropriate by the action of the speed controller 60.

Note that, as shown in FIG. 3, the valve body 12 has a
A first adjustment hole 71 that communicates between the upper end surface side and the bottom surface side is formed, and a second adjustment hole 72 that communicates with the catalyst outlet 14 and the hollow portion 21 is formed in the main body 11.
The pressure around the valve body 12 is adjusted by these adjustment holes 71 and 72.

Next, regarding the effect of this embodiment, Fig. 7 (4) to (C) k
This will also be explained with reference to

The catalyst storage tank 6 is filled with a catalyst 7 in the form of a highly concentrated slurry and pressurized with an inert gas such as nitrogen to maintain the internal pressure in the tank slightly higher than that of the polymerization reaction tank 3.

When the rotating body 12 of the catalyst supply device 1 is stopped in the state shown in FIG. 7(4), the carrier fluid supply line 9 and the catalyst supply line 2 are communicated with each other by the first flow path 31A, and the carrier fluid is is supplied to the polymerization reaction tank 3. Most preferably, the carrier fluid is the monomer itself for the polymerization reaction.

On the other hand, a catalyst inflow line 5 is communicated with the second flow path 31B, and a catalyst 7 is filled in the second flow path 31B. At this time, the excess catalyst 7 is returned to the catalyst storage tank 6 via a catalyst return line 8.

From this, when the rotating body 12 is rotated counterclockwise in FIG. 7 to the state shown in FIG. 7 CB), the carrier fluid supply line 9, the catalyst supply line 2, the catalyst inflow line 5, and the catalyst return Each of the lines 8 is temporarily disconnected, and the first flow path 31A is connected to the carrier fluid removal line 1.
0, and the carrier fluid in the first flow path 31A is discharged to the carrier fluid removal line 10. On the other hand, the second flow path 31
Inside B is filled with a certain amount of catalyst 7.

Furthermore, the rotating body 12 is rotated counterclockwise, and as shown in FIG.
), that is, the state shown in FIG. 7(4), when the second flow path 3 is rotated exactly 90 degrees and stopped.
1B communicates the carrier fluid supply line 9 with the catalyst supply line 2, and the carrier fluid supply line 9 communicates with the catalyst supply device 1.
The catalyst 7 filling the second flow path 31B is pushed out to the catalyst supply line 2 by the carrier fluid flowing into the catalyst, and is supplied to the polymerization reaction tank 3 along with the flow of the carrier fluid. On the other hand, the catalyst inflow line 5 is in the empty first flow path 31A.
are in communication with each other, and the first flow path 31A is filled with the catalyst 7.

By repeatedly rotating and stopping the rotating body 12 as described above, a predetermined amount of the catalyst 7 is appropriately added to the flow of the carrier fluid flowing into the polymerization reaction tank 3 without being diluted. The catalyst 7 is supplied in a highly concentrated slurry state to replace the carrier fluid, and the catalyst 7 is carried by the carrier fluid and supplied to the polymerization reaction tank 3.

While the rotating body 12 reaches the state shown in FIGS. 7(4) to 7(B), the carrier fluid supply line 9 and the catalyst supply line 2 are temporarily disconnected, but this period is usually within a few seconds. Since the time is extremely short, there is no possibility that the flow in the catalyst supply line 2 will stagnate and cause clogging. Note that the rotating body 12 does not necessarily need to be temporarily stopped in the states shown in FIGS. 7(4) to (C), and the rotating body 12 may be continuously rotated. The 120 rotation state is appropriately selected as necessary. That is, the flow path 31A,
Since the amount of catalyst 7 filled in 31B is constant, for example, when trying to supply more catalyst 7 to a carrier fluid with a constant flow rate, the control unit 56 can be operated to control the rotation body 12. You just need to speed up the rotation, or you can use reeds.
Even if the number of revolutions of the rotating body 12 is made to correspond to the changing flow rate of the carrier fluid by the function of the control unit 56, the catalyst 7 is always supplied at a constant rate even if the flow rate of the carrier fluid fluctuates. good.

However, when a monomer for a polymerization reaction is used as a carrier fluid, a co-catalyst may be supplied from the co-catalyst supply line 4 and preliminary polymerization may be carried out in the catalyst supply line 2.

This embodiment has the following effects.

Catalyst 7 is one of the highly concentrated slurries! It can be extremely smoothly supplied to the polymerization reaction tank 3 without being diluted.

For example, in the conventional method of supplying the catalyst by pump transfer, depending on the inert solvent such as heptane and the properties of the solid component, it is usually 10''' bodies/l-inert solvent to 0°1.
Previously, it was necessary to dilute the 2-solid with an inert solvent to a range of 0. However, according to this example, the amount of inert solvent required is at most 0.02% to 2-2% compared to the conventional method. lost. In other words, it can be supplied at a concentration 50 to 5000 times higher than conventional methods.

Therefore, it not only prevents the activity of the catalyst 7 from decreasing, but also eliminates the use of inert solvents that complicate the post-treatment process as much as possible, meeting the need for resource conservation and greatly contributing to lower manufacturing costs. can do. By freezing, the volatile content in the product caused by inert solvents in the drying process of the resulting polymer can be significantly reduced.

Furthermore, the supply amount of the catalyst T can be easily adjusted by controlling the rotation state of the rotor 120.

In addition, when using the monomer itself for the polymerization reaction as the carrier fluid, there is no need for a separation process for the carrier fluid, and since the monomer itself is a polymerization reaction product, it can be supplied in any amount in its entirety, resulting in a high concentration. Even if the catalyst slurry is supplied, the catalyst supply line 2 will not be clogged at all.

In addition, in the above-mentioned catalyst supply device 1, the flow path 31A,
31B are all oriented in a direction perpendicular to the rotational axis of the rotary body 12, but, for example, like a rotary ammunition for a handgun,
Each of the plurality of flow paths of the rotary body may be provided along a direction parallel to the rotation axis of the rotary body.

Further, in the above description, the case of polymerization reaction was explained, but the present invention is not limited to polymerization reaction, and the catalyst 'klP
It can be applied to all chemical reaction processes.

As described above, according to the present invention, it is possible to provide a catalyst supply method and a catalyst supply apparatus that smoothly supply a high concentration catalyst to a reaction tank.

Next, the present invention will be explained in more detail with reference to the following examples.

EXAMPLE Bulk polymerization was carried out in a polymerization reaction tank 3 using propylene, which is a polymerization reaction monomer, as a carrier fluid. At this time, the catalyst 7 is Tj supported on a catalyst slurry (M) in which the proportion of the solvent (heptane) in the solid component is 50ωf%.
catalyst), and its concentration is 7002 #1N = weight ratio). ,,buta・′oxidation−gune・tsu・
I used something that is. A fluidity improver may be used depending on the properties of the catalyst solid component, and in this example, magnesium oxide was used as the fluidity improver.

The catalyst storage tank 6 used has an internal capacity of 1 ton, and the internal pressure is reduced to 'i 36 k, /! by nitrogen gas. I tried to maintain it.

Further, liquid propylene was flowed through the carrier fluid supply line 9 at a flow rate of 0.3 electric/second.

The volumes of the flow paths 31A and 31B are both 5-1, and the rotating body 12 is stopped for about 5 minutes in the state shown in FIGS. It was designed to be quick, rotating 12 times in an hour. Therefore, although the rotating body 12 is not particularly stopped in the state shown in ) in FIG. 7, the liquid propylene is quickly purged under reduced pressure through the carrier fluid removal line 10. Furthermore, while the rotating body 12 is rotating, the carrier fluid supply line 9 and the catalyst supply line 2 are disconnected, but the time during this period is extremely short, within a few seconds, and the flow rate of the catalyst supply line 2 is stagnant. The catalyst supply line 2 will not be blocked.

According to this example, the volatile component in the product polymer is 0.5%.
It was below. In contrast, conventional pumping resulted in a volatile content of 2% in the product polymer. Furthermore, in this example, it is possible to supply a catalyst with a slurry concentration 70 times higher than in the case of pump transfer, and the catalytic activity is 4.9 times higher in terms of the amount of polypropylene produced per unit titanium. did.

[Brief explanation of the drawing]

FIG. 1 is a schematic configuration diagram showing one embodiment of the catalyst supply device according to the present invention applied to a polymerization reaction process, FIG. 2 is a perspective view showing the external appearance of one embodiment of the catalyst supply device, and FIG. The figure is a partially cutaway front view of the embodiment, FIG. 4 is a right side view of the main part of FIG. 3 with a partially cutout, and FIG. 5 is a bottom view of FIG. Figure 6 is a sectional view taken along the line Vt-■ in Figure 5, and Figure 7 (4) to ((1)
) are schematic configuration diagrams showing the operating states of the embodiments. 1... Catalyst supply device, 2... Catalyst supply line, 3.
... Polymerization reaction tank as a reaction tank, 5... Catalyst inflow line, 6... Catalyst storage tank, 7... Catalyst, 9... Carrier fluid supply line, 10... Carrier fluid removal line, 11・
... Main body, 12... Valve body as a rotating body, 13...
Carrier fluid inlet, 14...Catalyst outlet, 15...Catalyst inlet, 31A, 31B--1st. second flow path, 4
1... Carrier fluid discharge port, 56... Control unit. Agent Patent Attorney Minoru Kinoshita Figure 1 Figure 2 Figure 4 Figure 6 Figure 11, X, A, 7f-752 Figure 5 Figure 7 (A) (B) 43- (C) 31A.

Claims (1)

[Claims] (1) A rotating body having two channels that do not intersect with each other is placed in the flow of the carrier fluid flowing into the reaction tank, and when the carrier fluid is flowing through one channel, the other flow The high-concentration catalyst is filled in the channel, and the rotating body is rotated to introduce the high-concentration catalyst into the conveying fluid. A method for supplying a catalyst, characterized in that the high concentration catalyst is appropriately supplied, and the high concentration catalyst is carried by a carrier fluid and supplied to the reaction tank. (Z) A rotating body having first and second flow paths that intersect with each other, a catalyst inlet communicating with a catalyst storage tank, and an outlet to a catalyst supply line that supplies all of the catalyst to the reaction tank. , a carrier fluid inlet into which the carrier fluid flows, and a carrier fluid outlet for discharging the carrier fluid in the flow path, and when the rotating body is located at a predetermined rotation angle, the first flow path The carrier fluid inlet and the catalyst outlet are communicated with each other, and the catalyst inlet is communicated with the second channel, and when the rotating body is rotated by a predetermined angle, the tenth channel is connected to the carrier fluid outlet. When the rotating body is further rotated by a predetermined angle, the first flow path is communicated with the catalyst inlet, and the second flow path is configured to be communicated with the carrier fluid inlet and the catalyst outlet. A catalyst supply device characterized by: