Polymerization in suspensions with high solids content

 

The invention relates to a method of polymerization in a loop reaction zone olefin monomer in a liquid diluent with the use of the device for continuous sampling of the suspension product. According to the method of the monomer, diluent and catalyst are circulated in a loop reactor of a continuous action with obtaining a liquid suspension containing liquid diluent and solid particles of olefin polymer. Thus concentration of particulate olefin polymer in suspension support in the reaction zone above 40 wt.% by weight of polymer particles and the mass of liquid diluent. Continuously sampling the suspension of a product having an increased concentration of solid particles in comparison with the concentration in suspension in the reaction zone. The continuous process allows the reaction at a very high content of solids in the circulating suspension due to a higher rate of forced circulation. 3 S. and 26 C.p. f-crystals, 10 ill., table 1.

The present invention relates to the polymerization of olefinic monomers in a liquid diluent.

Polymerization attach often carried out in a liquid which is a solvent for poluchennogo and this method. It was soon discovered that such polymers would be obtained by suspension polymerization. Particularly preferred polymerization technology has become a continuous suspension polymerization in a tubular loop reactor with the selection of the final product through the apparatus for settling and working on the principle of periodic selection of the product. This technology has had international success, it made every year billions of pounds of polymers of ethylene. With this success came the desire to put less large reactors instead of a large number of small reactors of the same power setup.

Settling devices, however, creates two problems. First, they represent a combination of periodic technologies with the primary continuous process. Whenever settling apparatus is at a stage where he "unloads" or "throws" the accumulated suspension polymer are superimposed on the flow of slurry in a loop reactor upstream and in the selection of lower flow. In addition, valve mechanism associated with periodic softening settling apparatus in the reactor upstream and in the zone of selection downstream, requires Metra, necessary to seal the apparatus.

Secondly, since the size of the reactor increased, problems arose maintenance of the machines to protect. If the pipe diameter is doubled, the volume of the reactor was increased four times. However, due to the emergence of valve mechanisms having difficulty with further increase in size of the apparatus for sedimentation. Therefore, the number of required devices is beginning to exceed the available physical space.

Despite these limiting factors, continued to use the apparatus for settling where the olefinic polymers are formed in suspension in a liquid diluent. This is because in contrast to the way the periodic suspension polymerization (i.e., where the monomer is thinner), which typically achieved concentration exceeds 60 percent, the concentration of solid particles in suspension olefin polymer in the diluent usually do not go beyond from 37 to 40 mass percent. Therefore, the apparatus for settling felt it necessary to get ready suspension at the outlet of the apparatus settling with a concentration above 37-40 percent. This is because stoic in the final suspension, output as suspension product.

Another factor in determining the maximum actual amount of solid particles in the reactor, is the circulation rate, and a higher speed when the diameter of the reactor allows to increase the solids content, because the factors limiting the operation of the reactor, are clogging due to filling of the reactor with the polymer.

Summary of invention the present invention is to obtain olefin polymers in the form of a suspension in a liquid diluent with the use of the device for continuous sampling of the suspension product.

Further, the present invention is a process of suspension polymerization of olefin in the diluent at a sufficiently high concentration of solid particles in the reaction medium, enabling direct continuous selection of the product on an industrial scale.

Another objective of the present invention is a process for the suspension polymerization of olefin in the diluent at elevated speeds circulation.

In addition, the present invention is a process of suspension polymerization of olefin in the diluent in the reaction zone or, having capacity above 113,6 m3(30,000 gallons), provided with a device for continuous selection.

In accordance with one aspect of the present invention the polymerization of the olefin takes place with high concentration of solid particles in the reaction medium and using the device for continuous sampling of the suspension product.

In accordance with another aspect of the present invention looped reactor for the polymerization of olefin is designed to operate at high speed circulation at a certain diameter of the pipe reactor.

In accordance with another aspect of the present invention looped reactor for the polymerization of olefin has an oblong hollow device in the lower end of the flow loop of one of the longitudinal sectors; the hollow device is directly connected with the liquid stream with the heated line of the evaporator and, in addition, it is adapted for continuous sampling of the suspension product.

A brief description of the drawings In the drawings annexed to the description of the present invention, is presented on the figure 1 - schematic representation of a loop reactor and the selection of the polymer; figure 2 is a transverse section along the line 2-2 of figure 1,gerny mechanism in the device for continuous sampling; figure 4 is a cross sectional view of a device for continuous sampling, placed tangentially; figure 5 shows a side view of the knee hinge of the reactor, on which you can see the device for sedimentation and nodes continuous selection; the figure 6 presents a cross-section along the line 6-6 of figure 5 showing the location of two nodes of a continuous selection; figure 7 shows a side view depicting another node orientation is a continuous selection; figure 8 is a cross sectional view of the centrifugal pump; figure 9 shows a diagram with a different image loops, which the upper sections 14a is made in the form of a semicircle is 180o, in which the vertical sector of at least two times longer than the horizontal; and figure 10 is given a schematic representation, showing that the longer axis is located horizontally.

Detailed description of the invention surprisingly, it was found that continuous selection of suspension of the product in the polymerization reaction of the olefin, passing in a loop reactor in the presence of an inert diluent, allows the reactor to operate at elevated significantly the content of solid particles. Industrial production mainly of polymers of ethylene in from the however, the continuous selection, as it was discovered, allows to increase significantly the concentration of solid particles. Furthermore, even continuous selection contributes to some additional increase solids content compared to their contents in the reactor, from which is selected a product that is explained by the location of the device for continuous sampling, which selectively takes a suspension of the settled layer, in which the concentration of solid particles above. Therefore, in accordance with the present invention are possible concentrations higher than 40 mass percent.

According to the present application is the mass of the catalyst does not matter, in particular with chromium oxide on silica, because the performance is extremely high.

Surprisingly it was also found that can be applied more forced circulation (with accompanying high concentration of solid particles). Indeed, more forced circulation in combination with a device for continuous sampling may allow continuous sampling from the reactor product with a solids concentration greater than 50 mass percent with a device for continuous sampling. For example, a device for continuous sampling is regulated so the concentration of solid particles will be higher by 10 percent; and more forced circulation can easily add another 7-9 percentage points, which will increase the solids content in the reactor to more than 50 percent. But as a device for continuous sampling is intended for selection of suspension of the settled layer flow, which has a solids concentration above the average, the selected product will have a concentration of about 3 percentage points higher than the average concentration of the suspension in the reactor. Thus, it can be achieved the actual concentration of the suspension equal to 55 mass percent and above, that is, when the average concentration in the reactor equal to 52 mass%, and finished the resulting suspension with a concentration of 55 mass%, (that is 3 points higher).

It should be emphasized that in industrial scale increase in the concentration of solid particles, even so little as one percentage point, is of great importance. Therefore, the transition from the concentration of solid particles in average 37-40 mass percent in the reactor even at 41 percent already of great importance, therefore, receive 50 percent concentration is truly an achievement.

Preferred diluents (unlike solvents or monomers) are well known to the expert and include hydrocarbons that are inert and liquid under the reaction conditions. The preferred hydrocarbon is isobutane, propane, n-pentane, I-pentane, neopentane and n-hexane; most preferred is isobutane.

Preferred catalysts are well known to the specialist. The most preferred catalyst is a chromium oxide with a carrier, such as silicon dioxide, the catalyst described the am. The figure 1 shows the loop reactor 10 having a vertical sector 12, upper horizontal sector 14 and lower horizontal sector 16. These upper and lower horizontal sector define the upper and lower zone of horizontal flow. The reactor is cooled by means of two tubular heat exchangers formed by the tube 12 and shirts 18. Each sector is associated with the following sector with the help of knee or elbow 20 which provides free continuous flow without internal driving. Circulation polymerization mixture occurs under the action of centrifugal pump 22 (shown in figure 8) working from the engine 24. The monomer, comonomer, if present, and the diluent serves on the lines 26 and 28, respectively, which can enter directly into the reactor in one or more places or they can be combined, as shown, with the return line of the condensed diluent 30. The catalyst is injected through the feeder catalyst 32, which has an area (a place) to enter the catalyst. An elongated hollow device for continuous sampling of the suspension of the intermediate product in the form of a suspension 34 is indicated in General by reference. The continuous about the first reactor or adjacent to the connecting elbow 20.

Device for continuous sampling is shown at the end of the lower thread lower horizontal sector loop reactor, such an arrangement is preferred. The location of this device may be in the area next to the last point in the loop where the flow turns up before the introduction of the catalyst that allows the fresh catalyst as long as possible to remain in the reactor before it is the first time point of selection. However, the device for continuous sampling can be placed on any sector or on any knee.

Also the sector that is attached to the device for continuous sampling, may have a larger diameter in order to slow the flow and, consequently, the subsequent stratification of the flow, helps to ensure that the output stream may have an even higher concentration of solid particles.

Continuously selected suspension intermediate product passes through the pipe 36 into the evaporation chamber with high pressure 38. The pipe 36 is covering the pipe 40, which is heated fluid, indirectly transferring heat to the suspension in the pipe 36 evaporative line. The evaporated diluent exits Espana using recirculation of condenser 50 and is returned to the system without compression on the return line diluent 30. Recirculation condenser 50 can run on any heat-exchange fluid, well-known specialist in any well-known specialist conditions. However, it is preferable to apply the liquid with a temperature that is optimal from an economic point of view. The preferred limit temperature of the liquid is enclosed between 4,4 and 54.4o(40 and 130 degrees F). The polymer particles are removed from the evaporation chamber with high pressure 38, line 44, after which they proceed to the next stage of the process, which use well-known technology expert. Preferably they are received in the evaporating chamber with low pressure 46, and then they are selected as the polymer product via line 48. The separated diluent passes through the compressor 47 in line 42. Such a scheme with high blood pressure are described in detail in U.S. patent 4424341 (January 3, 1984) Hanson and Sherk, the link provided here for reference. Surprisingly, it was found that continuous selection not only allows operation at higher concentrations of solid particles in the zone of the upper stream in the reactor, but also allows to improve the work at the stage of evaporation at high pressure, with the result that a large part addressed to the evaporation of the diluent Iran so. This is due to different reasons. First of all, because the flow is continuous and not interrupted, heaters line evaporation work better. After reducing the pressure after the valve which regulates the rate of a continuous stream exiting the reactor, the reactor pressure is reduced, this means that when there is evaporation, the temperature is reduced and this contributes to a more efficient use of space heaters line evaporation.

Now, referring to figure 2, we see a detailed image of the knee 20 with a device for continuous selection 34. Device for continuous selection includes a gripping cylinder 52, the line of discharge of the suspension 54, emergency overlying the valve 55, the valve with a motor drive 58 for flow control and line 60 evaporation. The reactor operates in full "liquid" state. Since the monomer is diluted, the fluid is slightly compressible, at least allowing you to control the pressure in the system is filled with liquid through the valve. The introduction of diluent support is usually constant; valve with motorized actuator 58 is applied to speed control of a continuous flow that is necessary for the maintenance of the 3, which shows a longitudinal section along the line 3-3 of figure 2, showing the pipe or elbow 20 with attached device for continuous selection 34 (shown in detail) of the knee 20, at least, is a device that carries the knee. As shown in the drawing, the device consists of a cylinder 52, in this case, attached at right angles to the tangent to the surface of the knee. Cylinder selection 52 represents the output line of the suspension 54. Located inside the cylinder 52 of the plunger mechanism 62 has a dual function. First, it is a simple and reliable cleaning mechanism for the cylinder, in case of driving the polymer. Secondly, it can play the role of a simple and reliable overlying valve for the whole site continuous selection.

The figure 4 shows the preferred direction of arrangement of the cylinder selection 52 tangent to the curvature of the knee 20 and at the point before turning the thread up. The hole at the connection point has the shape of an ellipse. In addition, this hole can be extended to improve the efficiency of selection.

The figure 5 shows the four positions. First, it shows the angle of the cylinder selection 52. Cylinder selection is shown at an angle alpha to pogorizontali sector 16. Angle with this plane is taken in the direction of the bottom stream from the plane. The vertex of this angle lies in the Central point of the radius of curvature, as shown in figure 5. The plane can be described as a cross section plane of the horizontal sector. In this case depicts an angle of approximately 24 degrees. Secondly, it shows several devices for selection, 34 and 34a. Thirdly, it shows that one device 34 is located on the vertical axis plane of the lower sector 16, 34a and the other is located at an angle to this plane, as it will be shown in more detail in figure 6. And finally, it shows the combination of the selection device 34 with traditional decanting apparatus 64 for periodic selection if necessary.

As is evident from the relative sizes of the cylinders of the selection is significantly less than conventional clarifiers. Even when 50,8 mm (2-inch) internal diameter of the device for continuous sampling is possible to select the same willing suspension as with the settling apparatus having an inner diameter equal 3759,2 mm (148 inches). It is of great importance, since the existing large industrial loop reactors with a capacity of 56,8-68,13(15000 is otopleniya reliable valves large diameter. As already noted, increasing the pipe diameter is twice associated with an increase in volume four times and there is simply no space for the free accommodation of large numbers, which increased four times, settling apparatus. Therefore, the present invention makes possible the use of larger, more powerful reactors. According to the present invention can be used reactors with a volume of 113,6 m3(30,000 gallons) and more. Usually cylinders for continuous selection will have a nominal internal diameter ranging from 25.4 mm (1 inch to less than 203 mm (8 inches). The preferred inner diameter is equal to or 50.8-76.2 mm (2-3 inches).

In figure 6 longitudinal section taken on the line 6-6 of figure 5, figure 6 shows the cylinder selection 34a located at an angle beta to the vertical plane relative to the axis of the reactor. This plane can be considered as the vertical axial plane of the reactor. This angle can be taken or from one side of the plane or from both sides of the plane, if it is not equal to zero. Angle vertex lies on the axis of the reactor. As seen in figure 6, the angle is in the plane perpendicular to the axis of the reactor.

It is noticed that there are three types of accommodations. First, there are situated the 7, or at an angle from 0 to 90 degrees. Secondly, there is the location relative to which the distance is the curvature of the knee, as shown by angle alpha (figure 5). It can be from 0 to 60 degrees, preferably from 0 to 40 degrees and more preferably from 0 to 20 degrees. Thirdly, there is an angle beta to the Central longitudinal plane of the sector (figure 6). This angle can be from 0 to 60 degrees, preferably from 0 to 45 degrees, more preferably from 0 to 20 degrees.

The figure 7 shows an embodiment of the present invention, according to which cylinder for continuous selection 52 has a perpendicular position, angle alpha is equal to 0 (because it is at the end, but still on the straight section of the sector), and the angle beta is equal to 0, i.e. it is right on the vertical axial plane of the lower horizontal sector 16.

Figure 8 provides a detailed picture of the centrifugal pump 22 necessary for the continuous promotion of the suspension in the direction of flow. According to this variant implementation of the present invention can be seen that the centrifugal pump is slightly expanded part of the tube, which is a push zone for circulating reagent is sustained fashion, at least in 137,9 kPa (20 psig) and more preferably, at least 151,68 kPa (22 psig) between the ends of the upper and lower threads in the push area when the nominal diameter of the reactor, equal 0,610 m (two feet), with a total length of flow equal to about 289,6 meters (950 feet), using isobutane mainly for polymers of ethylene. Such high pressure as 344,74 kPa (50 psig) and above may. This can be obtained by regulating the speed of rotation of the blades of the pump while reducing the gap between the blades and the inner wall of the pump housing or by using a more powerful pump, well-known specialist. This high pressure drop can be achieved when using at least one additional pump.

Typically, the system operates by receiving a pressure drop, expressed as pressure loss per unit length of the reactor, at least equal to 21.3 mm (0.07 ft), usually from 21.3-45.7 mm (0.07-0.15 m) pressure drop in mm of the length of the reactor with a nominal diameter 609,59 mm (24 inches). Preferably this pressure loss per unit length is 0,09-0,11 for a reactor with a diameter of 609,59 mm (24 inches). For reactors with large diameters required higher the Oia is expressed by the value of m in m (ft/ft). This allows the density of the suspension is approximately 0.5 to 0.6.

According to figure 9 the upper sector is shown as 180othe semicircle represents the preferred configuration. Vertical sector of at least twice as long, usually 7-8 times longer than the horizontal sectors. For example, the length of the vertical flow may be equal to 57.9-68,6 m (190-225 feet) in length and flows in a horizontal sectors of the 7.62 11,89 m (25-30 feet). You can use any number of loops in addition to the four described herein, and eight loops depicted in figure 1, but typically use four or six loops. Referring to dvuhvalkovyy diameter, means that the inner diameter of approximately 556,3 mm (21.9 inches). The stream length usually exceeds 152,4 m (500 ft), it is preferable 274,3 m (900 feet), more preferably, when it is equal to 286,5-411,5 m (940-1350 feet).

Industrial pumps, for example to ensure the circulation of the reaction medium in a closed loop reactor, usually experience their manufacturers, and the necessary suction pressure can be easily determined by conventional methods.

EXAMPLES of the polymerization Reactor with four vertical units to defend, which applied 660,4 mm (26-DUI Auntie this pump with 609,6 mm (24-inch) pump, giving less forced circulation (pressure drop of 0.20 to 0.30 m) (0,66 to 0,98 ft). This data is then compared with the data obtained by more forced circulation and when using the device for continuous sampling, for which details are shown in figure 5. The obtained data are given in the table.

Since the present invention has been described with illustrative purpose, one should not assume that the object of the present invention it is limited; it was made only intention is to cover all the options in the spirit and scope of the present invention.

Claims

1. The method of polymerization comprising polymerization in a loop reaction zone, at least one olefin monomer in a liquid diluent to form a liquid suspension containing liquid diluent and solid particles of olefin polymer, maintaining the concentration of particulate olefin polymer in suspension in the reaction zone above 40 wt.% by weight of polymer particles and the mass of liquid diluent, characterized in that ongoing selection of suspension with increased concentration of solid particles in comparison with the concentration in suspension in the reaction zone is selected from the certain solid particles of the polymer.

2. The method according to p. 1, characterized in that as the olefin monomer used ethylene or ethylene and 0.01-5 wt.% hexene of the total weight of ethylene and hexene, while the liquid diluent is an isobutane.

3. The method according to p. 1 or 2, characterized in that the concentration of solid particles of olefin polymer in suspension in the zone exceeds 50 wt.% by weight of polymer particles and the mass of liquid diluent.

4. The method according to one of paragraphs.1-3, characterized in that the support pressure drop at least equal 0,124 MPa in the push area to circulate the slurry in the reaction zone.

5. The method according to one of paragraphs.1-3, characterized in that the reactor support the magnitude of the pressure loss per unit length of the reactor above 21,3 mm on the length of the path, in particular in the range of 21.3-45,7 mm/mm / mm path length flow in the propulsion area.

6. The method according to one of the preceding paragraphs, characterized in that the reaction zone support in fluid-filled condition.

7. The method according to one of the preceding paragraphs, characterized in that the reaction zone has a volume of more 75,7 m3preferably more 113,6 m3.

8. The method according to one of the preceding paragraphs, characterized the second product, then the heated intermediate product is affected by the pressure drop in the zone of the evaporator high pressure, while in the process of heating a large part of the extracted liquid diluent evaporates and is separated from the withdrawn solid polymer particles, followed by condensation of the separated extracted liquid diluent to return to the cycle, without compression, by heat exchange with a fluid having a temperature in the range 4-54°C.

9. The method according to one of the preceding paragraphs, characterized in that the continuous selection of suspension is carried out at the site, located near the last point in the loop reaction zone before turning flow up and before the introduction of the catalyst.

10. The method according to one of paragraphs.1-8, characterized in that the continuous selection of the suspension is carried out, at least in one area, adjacent to the lower end of the zone of horizontal flow.

11. The method according to p. 10, characterized in that the continuous selection of suspension is carried out at the site, located along the vertical axial plane of the lower zone of horizontal flow before turning up.

12. The method according to p. 10, characterized in that at least one site is located along the vertical axis PLO is m, that at least one portion is located at an angle away from the vertical axial plane of the lower zone of horizontal flow and this angle is 0-45°.

14. The method according to p. 13, characterized in that at least one portion is located at a distance from the vertical axial plane at an angle equal to 0-20°.

15. The method according to p. 13, characterized in that at least one site is located before turning flow upwards.

16. The method according to p. 13, characterized in that at least one site is located after turning flow upwards at an angle equal to at least not less than 1, but less than 45° to the axis of the upper thread.

17. The method according to p. 10, characterized in that at least one plot for continuous selection is a single site or several sites.

18. The method according to one of paragraphs.1-17, characterized in that it further includes a step of settling slurries, at least one settling zone with the subsequent withdrawal of part of the settled slurry from the settling zone to form an intermediate product of the process, and then settling zone close.

19. The method according to p. 18, characterized in that during the start-up stage of settling suspension control conditions ol the howl of the reactor, includes many vertical sectors, many of the upper horizontal sectors, many of the lower horizontal sectors, in which each of the vertical sectors attached to the upper end through the top of the knee to one of the upper horizontal sectors, and the lower end through the bottom of the knee to one of the lower horizontal sectors to ensure a continuous flow of a liquid suspension, means for introducing a reactive monomer, polymerization catalyst and a liquid diluent in the reactor, means for continuously advancing the suspension in the direction of flow, at least one hollow branch, adjacent to one of the lower horizontal sectors, moreover, the specified branch is intended for screening a suspension of the product and is configured to open the message flow, and the longitudinal line of evaporation, which is connected by a thread with a branch for transmission to a suspension of the product from a branch in the host evaporation, and the line evaporation is covering the heat exchanger for heating a suspension of the product, while the reactor is substantially free from driving, characterized in that at least one hollow branch Ave is prevalent with the possibility of continuous selection suspension product.

21. Reactor according to p. 20, characterized in that at least one branch is connected to one of the lower horizontal sectors, with the formation of the lower horizontal sector, carrying a branch, and the branch is located along the vertical axial plane of the lower horizontal sector, carrying a branch, and is adjacent to smooth the lower knee in the lower end of the flow in the lower horizontal sector, the host branch.

22. Reactor according to p. 20, characterized in that the branch is connected to one of the lower horizontal sectors at an angle of 0-90°.

23. Reactor according to p. 20, characterized in that at least one branch connected with a smooth knee, attached to the lower end of the flow to the lower horizontal sector, carrying a fork, forming a smooth knee support branch.

24. The reactor under item 23, characterized in that the branch is connected with a smooth knee, bringing the branch at an angle of at least not less than 1° but less than 45° from the axis of the adjacent vertical sector.

25. Reactor according to p. 24, characterized in that at least one branch attached at right angles to the tangent to the knee, and carrying a branch.

26. Reactor according to p. 24, oenia.

27. The reactor under item 26, characterized in that at least one branch attached at a distance from the vertical axial plane at an angle of 20°-45°.

28. The reactor under item 26, characterized in that at least one branch represents exactly one branch or multiple branches.

29. The method of polymerization comprising polymerization in a loop reaction zone, at least one olefin monomer using a catalyst containing chromium oxide on the carrier in a liquid solvent to form a liquid suspension containing liquid diluent and solid particles of olefin polymer, maintaining the concentration of particulate olefin polymer in suspension in the zone above 40 wt.% by weight of polymer particles and the mass of liquid diluent, characterized in that ongoing selection of suspension with increased concentration of solid particles in comparison with the concentration in suspension in the reaction zone, while the selected suspension, representing promezhutochny product of the process contains the selected liquid diluent and separate solid particles of the polymer.

 

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