JP5486442B2 - Apparatus for removing volatile components from polymerization solution, method thereof, and polymerization apparatus - Google Patents

Description

  The present invention relates to an apparatus for removing volatile components from a polymerization solution that removes volatile components such as unreacted monomers and solvents mixed in a polyolefin polymerization solution, a method thereof, and a polymerization apparatus.

For example, when the olefin monomer is polymerized by solution polymerization or bulk polymerization, volatile components such as unreacted monomer and solvent in the case of solution polymerization remain in the polymerization solution. These volatile components cause deterioration of product quality as odors and the like, so it is necessary to remove them to such an extent that they do not affect the quality.
And the method of removing continuously volatile components, such as an unreacted monomer and a solvent, from a polymerization solution in the last process of the manufacturing equipment of a thermoplastic resin of a polymer is known (for example, refer to patent documents 1). ).
The thing of this patent document 1 has connected the devolatilization tank connected to the vacuum apparatus under the heat exchanger for heating a polymerization solution. Furthermore, a divider having a plurality of circular openings with a diameter of 3 to 5 mm is provided between the heat exchanger and the devolatilization tank. And in this patent document 1, when the polymerization solution heated with the heat exchanger flows in into a devolatilization tank through a divider | distributor, the volatile component in a polymerization solution foams, and a polymerization solution and foam in a devolatilization tank. The structure which isolate | separates from the vapor phase component which was made is taken.

Further, as a method for removing volatile substances, a method is known in which a polymerization solution containing a volatile substance is treated in a heating step and a gas-liquid separation step under reduced pressure following the heating step (for example, Patent Documents). 2).
The thing of this patent document 2 is divided | segmented into the some heating zone as a heating process. Then, a temperature gradient from the inlet side to the outlet side of the polymerization solution is set, the volatile substances are heated to a temperature at which the volatile substances are not substantially vaporized in the inlet heating zone, and the volatile substances are vaporized after the second heating zone. Is heated. And in this patent document 2, the structure which is made to flush by the gas-liquid separation process after a heating process and carries out gas-liquid separation is taken.

JP-A-2-209902 JP-A-2-232205

However, in Patent Document 1, due to the solution properties such as the viscosity in the polymerization solution and the residual amount of the volatile component, a part of the volatile component is foamed in the heat exchanger on the upstream side of the divider, and the overall heat transfer coefficient in the heat exchanger is May decrease, and the polymerization solution may not be sufficiently heated. As a result, the volatile component cannot be sufficiently foamed and removed, and the produced polymer has a volatile component odor.
For this reason, there exists a possibility of producing the problem that an apparatus enlarges by enlarging a heat-transfer area in order to fully heat a polymerization solution. Furthermore, the amount of energy required for heating increases, which may cause a disadvantage that energy efficiency is lowered.

  On the other hand, in Patent Document 2, since the heating zone is divided into a plurality of parts and controlled at different temperatures, the configuration may be complicated. Further, when properties such as the viscosity of the polymerization solution and the residual volatile content fluctuate, it is necessary to adjust the temperature of each heating zone, and the control may be complicated. And a volatile substance will vaporize gradually in the downstream in each heating zone, and an overall heat transfer coefficient will fall gradually. For this reason, in order to fully heat a polymerization solution, it is necessary to enlarge a heat-transfer area, and there exists a possibility of producing the problem that an apparatus enlarges. Furthermore, the amount of energy required for heating increases, which may cause a disadvantage that energy efficiency is lowered.

  In view of the above, an object of the present invention is to provide an apparatus for removing a volatile component from a polymerization solution, a method thereof, and a polymerization apparatus that can efficiently and well remove a volatile component.

The apparatus for removing a volatile component of a polymerization solution according to the present invention includes a pressurizing unit that pressurizes a polymerization solution obtained by polymerizing an olefin using a solvent, and heats the polymerization solution pressurized by the pressurizing unit under pressure. Heating means, a pressure reducing means having a reduced pressure reducing space into which the pressurized and heated polymerization solution flows, a plurality of flow paths through which the polymerization solution can flow, and the pressure reducing means of the pressure reducing means A porous member disposed in the decompression space in a state in which the polymerization solution flowing into the space is circulated through the flow path, and the decompression means constitutes the decompression means, The desolvation tank includes a polymerization solution inflow path through which the pressurized and heated polymerization solution flows, and an outflow path through which the polymerization solution in the decompression space flows out. Connected, and the porous member is Between the solution inflow path and the outflow path, the polymerization solution inflow path side and the outflow path side are arranged in the decompression space so as to be able to circulate through the flow path, and the pressurizing means is the heating means. The polymerization solution is pressurized to a pressure that does not foam when heated .

Also, in the present invention, the porous member is preferably proportion of pore size of the flow path to the pitch dimension of the channel (L) (D) (D / L) is configured not more than 0.4 .
In the present invention, the polymerization solution heated by the heating means preferably has a polyolefin concentration of 90% by mass or more.
Further, in the present invention, the heating means is preferably configured to heat to 230 ° C. or higher and 250 ° C. or lower.
Moreover, in this invention, it is preferable that the said pressure reduction means is set as the structure which pressure-reduces to 0.5 kPa or less.
And in this invention, it is preferable that the said pressurization means is set as the structure provided with the pressure control valve arrange | positioned between the said heating means and the said pressure reduction means.
In the present invention, it is preferable that the pressurizing unit is disposed upstream of a position in the polymerization solution inflow passage where the polymerization solution flows from a position connected to the solvent removal tank .
In the present invention, it is preferable that the polymerization solution has a limiting viscosity of 0.5 dL / g or more and 15.0 dL / g or less.
In the present invention, the polyolefin preferably has a isotactic pentad fraction of 20 mol% to 60 mol%.
In particular, in the present invention, the polyolefin is preferably a polypropylene having a weight average molecular weight (Mw) of 2 or more and 400,000 or less .
In the present invention, a pre-stage pressurizing unit that pressurizes the polymerization solution, a pre-stage heating unit that heats the polymerization solution pressurized by the pre-stage pressurization unit under pressure, and the pressurized and heated polymerization. A pre-stage depressurization means having a depressurized vacuum space into which the solution is introduced, and a pre-stage treatment means for supplying the polymerization solution depressurized by the pre-stage depressurization means to the pressurization means. preferable.

The method for removing a volatile component from a polymerization solution according to the present invention is a method for removing a volatile component from a polymerization solution obtained by polymerizing an olefin using a solvent, and heating the polymerization solution under pressure. A pressurizing / heating step and a foaming / foaming step of circulating the polymer solution pressurized and heated in the pressurizing / heating step through a plurality of channels provided in the porous member under reduced pressure are performed. In this case, the pressurizing / heating step is characterized in that pressurization is performed at a pressure at which the heated polymerization solution does not foam .

  The polymerization apparatus according to the present invention includes a polymerization means for polymerizing olefins in a solvent, and a volatile component removal apparatus for the polymerization solution according to the present invention for removing volatile components from a polymerization solution obtained by polymerizing the olefins with the polymerization means. And a granulating means for granulating the polymerization solution from which the volatile component has been removed by the volatile component removal apparatus for the polymerization solution.

  According to the present invention, the polymerization solution obtained by polymerizing the olefin using a solvent is heated under pressure, and is caused to flow into the reduced pressure space of the decompression means and foam and circulate through the plurality of flow paths of the porous member to break the bubbles. It can be heated efficiently by pressurizing to a pressure that does not foam during heating, and the appropriately heated polymerization solution is circulated through multiple channels of the porous member under reduced pressure to break bubbles, so that the volatile components foamed by reduced pressure are efficiently It can be well separated from the polymerization vessel and can easily and highly remove volatile components.

It is a block diagram which shows schematic structure of the olefin polymerization apparatus of one Embodiment which concerns on this invention. It is a block diagram which shows schematic structure of the deaeration means in this embodiment. It is a perspective view which shows the porous member in this embodiment. It is a graph which shows the relationship between the vapor pressure of the polymerization solution in this embodiment, temperature, and a density | concentration. It is a graph which shows the relationship between the vapor pressure for every polymer concentration of the polymerization solution in this embodiment, and temperature. It is a graph which shows the relationship between the vapor pressure for every temperature of the polymerization solution in this embodiment, and a polymer concentration.

The olefin polymerization apparatus according to the present invention will be described below with reference to the drawings.
FIG. 1 is a block diagram showing a schematic configuration of an olefin polymerization apparatus. FIG. 2 is a block diagram showing a schematic configuration of the deaeration means of the polymerization apparatus. FIG. 3 is a perspective view showing a porous member in the deaeration means.

[Configuration of olefin polymerization equipment]
In FIG. 1, 100 is an olefin polymerization apparatus, and this polymerization apparatus 100 is an apparatus for producing a polyolefin by homopolymerizing various olefins or copolymerizing different olefins.
Here, as the olefin, various olefins such as methylene, ethylene, propylene and butylene can be targeted. In particular, the present invention is suitable when producing a low molecular weight low regularity polypropylene.

In particular, the polymerization apparatus 100 is suitable for polymerization of a polymer having a weight average molecular weight (Mw) of 2 or more and 400,000 or less, preferably 4 or more and 100,000 or less.
That is, when producing a low molecular weight, it is necessary to increase the polymerization temperature. If the polymerization temperature is high, the catalytic activity may decrease, and the production efficiency may decrease. On the other hand, in the case of producing a high molecular weight, since the viscosity of the polymer becomes high, there is a concern about poor extraction from the polymerization tank for carrying out the polymerization reaction to be polymerized, so the concentration of the polymer is increased in order to avoid the defective extraction. This is because it is necessary and production efficiency may be reduced.

Furthermore, when the number average molecular weight is Mn, Mw / Mn is preferably 1.8 or more and 4 or less, more preferably 3 or less, and even more preferably 2.4 or less.
That is, when Mw / Mn is larger than 4, the molecular weight distribution is widened and the low molecular weight components are increased, so that the product surface may be so-called bleed and sticky.

And as polyolefin to manufacture, in DSC measurement, melting | fusing point (Tm (degreeC)) is not shown, or when showing Tm, Tm and fusion | melting endothermic quantity (DELTA) H (J / g) show the following relational expression (1). What satisfies is preferable.
(Relational formula 1)
ΔH ≧ 6 × (Tm−140) (1)
That is, in particular, when a low molecular weight low regularity polypropylene is produced using a catalyst described later, those having a melting point of 50 ° C. or higher and 110 ° C. or lower, preferably 60 ° C. or higher and 80 ° C. or lower are suitable.

Further, the intrinsic viscosity of the polymerization solution is 0.5 dL / g or more and 15.0 dL / g or less, preferably 0.3 dL / g or more and 1.2 dL / g or less, more preferably 0.4 dL / g or more and 0.95 dL / g. The following molecular weight is preferred.
When producing a polymer having an intrinsic viscosity of less than 0.5 dL / g, it is necessary to increase the polymerization temperature. By raising the polymerization temperature, there is a possibility that the catalyst activity is lowered and the production efficiency is lowered. On the other hand, in the case of producing a polymer having an intrinsic viscosity greater than 15.0 dL / g, the viscosity of the polymer becomes high, and thus there is a risk of poor extraction from the polymerization tank in which the polymerization reaction is carried out. For this reason, it is necessary to reduce the concentration of the polymer in the polymerization solution in order to avoid a defective blowing of the polymer, which may reduce the production efficiency. For these reasons, the limiting viscosity is set to the predetermined range described above.

Further, as the polyolefin to be produced, the isotactic pentad fraction is 20 mol% or more and 60 mol% or less, preferably 40 mol% or more and 55 mol% or less, more preferably 44 mol% or more and 51 mol% or less. Is particularly suitable for the production of low molecular weight, low order polypropylene.
When the isotactic pentad fraction is less than 20 mol%, the obtained polyolefin becomes sticky, and there is a possibility that particles are reattached during granulation in a subsequent process and productivity is lowered. On the other hand, if the isotactic pentad fraction is greater than 60 mol%, the catalyst performance will not be exceeded and production may not be possible.

Here, the measurement of the isotactic pentad fraction used as an index of stereoregularity is as follows. This was carried out in accordance with the ¹³ C-NMR method (Macromolecules, 6925, 1973) disclosed by Zambelli. Specifically, first, 220 mg of the i-PP sample was collected in a 10 mm diameter NMR sample tube, and 2.5 ml of a 1,2,4-trichlorobenzene / heavy benzene mixed solution (90/10 vol%) was added, and uniform at 140 ° C. After the mixture was dissolved, ¹³ C-NMR spectrum was measured using JNM-EX400 (trade name: manufactured by JEOL Ltd.). ^{The 13} C-NMR spectrum measurement conditions are shown below.
・ Pulse width: 7.5μs / 45 degrees ・ Observation frequency range: 25,000Hz
-Pulse repetition time: 4 seconds-Measurement temperature: 130 ° C
・ Total number of times: 10,000

The isotactic pentad fraction is a total of nine types of bond patterns of five propylene molecules (“mmmm”, “mmmr”, “rmmr”, “mmrr”, “rmrr + mrmm”, “rmrm”, “rrrr”, “Mrrr” and “mrrm”) are defined as relative ratios of the peak area corresponding to “mmmm” with respect to the area of all nine peaks observed as ¹³ C-NMR spectra corresponding to each of Specifically, it was calculated by the following equation (2). Here, when there was an overlap between the two peaks, a perpendicular line was drawn from the valley of the two peaks to the base line to divide both peaks (vertical division method).
(Formula 2)
Isotactic pentad fraction (mol%)
= {A (mmmm) / A (total)} × 100 (2)
Here, A (mmmm) is the area of the mmmm peak, and A (total) means the sum of the nine peak areas.
In addition, when there is an overlap between two peaks, in addition to the above vertical division method, there is also known a method of performing waveform separation using each peak as an aggregate of Lorentz-type peaks. Analysis software (ALICE 2 from JEOL Ltd.) is also known. ) May be used.

The polymerization apparatus 100 includes a polymerization facility 200 and a control device 300 as a control unit that controls the operation of the polymerization facility 200.
The polymerization facility 200 is a plant facility that produces a polyolefin by polymerizing an olefin (solution polymerization) using a solvent. The polymerization facility 200 includes a polymerization means 210, a devolatilization means 220 as a volatile component removal device for the polymerization solution, and a granulation means 230.

The polymerization means 210 is an apparatus for performing a polymerization reaction, and includes a polymerization tank (not shown). For this polymerization tank, for example, the latent heat of vaporization heat removal method is preferably used. This latent heat removal method uses, for example, the latent heat of vaporization of the monomer and is economically superior because it can secure a large amount of heat removal per one heat removal system. Furthermore, the latent heat of vaporization heat removal method is preferable because it can be efficiently and satisfactorily cooled even if the viscosity of the polymerization solution in the polymerization tank increases due to polymerization.
If the production volume is relatively small enough to cool the whole, a jacket heat removal system that cools from the outside of the polymerization tank can be used to reduce the size of the polymerization tank, and polymerization is performed when the viscosity of the polymerization solution is not high. An external circulation method in which the solution is circulated and cooled, or a raw material sensible heat removal method in which the raw material and the solvent are supplied after cooling in advance when using a catalyst system whose molecular weight does not greatly depend on the polymerization temperature may be used.
The polymerization means 210 is connected to a raw material supply means 211 for supplying propylene, which is a raw material olefin, to the polymerization tank. The polymerization means 210 is connected to a solvent supply means 212 for supplying heptane to the polymerization tank in the case of solution polymerization of a solvent such as propylene. Further, a catalyst supply means 213 for supplying a catalyst is connected to the polymerization means 210. The polymerization means 210 is connected to a hydrogen gas supply means 214 that supplies hydrogen gas (H ₂ ) that activates the catalyst and starts propylene polymerization. Further, the polymerization means 210 is connected to a third component supply means 215 for supplying a cocatalyst and a third component.

In the polymerization tank, for example, when polymerizing low molecular weight and low-order polypropylene, the pressure during solution polymerization is preferably 0.5 MPa or more and 3 MPa or less.
That is, if the pressure is increased, the concentration of the polymer in the polymerization solution increases and the production efficiency is improved. However, at a pressure higher than 3 MPa, the concentration of the polymer in the polymerization solution hardly increases and improvement in production efficiency cannot be expected, and there is a possibility that inconveniences such as increase in equipment size and increase in energy consumption due to increased pressure may occur. On the other hand, when the pressure is lower than 0.5 MPa, stereoregularity does not appear and the intended polymer cannot be obtained.

  Here, as the catalyst, various catalysts used for olefin polymerization can be used. In particular, a metallocene-based catalyst having high temperature dependency, specifically (A) a transition metal compound, (B) a solid organoboron compound that forms an ion pair with the transition metal compound, and (C) an organoaluminum compound, (D) a catalyst obtained by contacting one or more compounds selected from α-olefin, internal olefin, and polyene (the catalyst described in Japanese Patent Application No. 2007-514550), or (A) a transition metal compound and (B) A catalyst obtained by contacting a solid organoboron compound that forms an ion pair with a transition metal compound and (C) an organoaluminum compound is preferable because a polyolefin can be obtained with high efficiency and stability. For example, (1,2'-dimethylsilylene) (2,1'dimethylsilylene) -bis (3-trimethylsilylmethylindenyl) zirconium dichloride can be suitably used.

The devolatilization means 220 is an apparatus that is connected to the polymerization means 210 and removes volatile components from the polymerization solution flowing out from the polymerization tank of the polymerization means 210. The devolatilization means 220 includes a demonomer tank (not shown) and a solvent removal tank 221 shown in FIG.
The demonomer tank is connected to the polymerization tank and the polymerization solution is flowed into it. Connected to the demonomer tank is a volatile component gas recovery means 222 for recovering unreacted raw material propylene that is volatilized from the polymerization solution and a volatile component that is a solvent.
Volatile component gas recovery means 222 includes a decompression device for decompressing the inside of the demonomer tank, a recovery device for collecting volatile components from the gas phase sucked by the decompression device, and a volatile component recovered by the recovery device. For example, a refining apparatus equipped with a distillation column for purifying the components is provided.
In this demonomer tank, the volatile components are removed until the concentration of the polymer in the polymerization solution is 90% by mass or more, preferably 95% by mass or more. That is, the amount of the volatile component remaining in the product is determined by the vapor-liquid equilibrium state between the polyolefin and the volatile component determined by the temperature and pressure conditions in the tank in which the volatile component is separated and removed. When the concentration of the polymer in the polymerization solution is low, the rate at which the temperature decreases due to the latent heat of vaporization of the volatile components in the solvent removal tank 221 in the subsequent stage increases. For this reason, the desired vapor-liquid equilibrium cannot be obtained in the solvent removal tank 221, and it is necessary to separately supplement the amount of heat corresponding to the temperature decrease due to latent heat of vaporization, which makes it difficult to sufficiently evaporate and separate the volatile components. The volatile components are separated and removed in advance so that the polymer concentration becomes 90% by mass or more.
The condition for separating and removing the polymer at a concentration of 90% by mass or more depends on the temperature and pressure, which are conditions for vapor-liquid equilibrium between the polyolefin and the volatile component, as described above. When the ability to reduce the pressure in the volatile component gas recovery means 222 is 0.02 MPa in the demonomer tank, the temperature of the polymerization solution is 188 ° C. or higher (when the polymerization solution flows into the demonomer tank) The temperature is set to about 200 to 220 ° C.
The demonomer tank is not limited to a single tank, but preferably has a multistage structure in which, for example, unreacted monomers are separated and removed in the former stage, and most of the solvent is separated and removed in the latter stage. That is, the volatile component gas recovery means 222, the tank, and the like can be further downsized, and the volatile component after the recovery can be easily purified.

As shown in FIG. 2, the solvent removal tank 221 is connected to the monomer removal tank via a polymerization solution inflow path 223, and a polymerization solution from which some volatile components have been removed in the monomer removal tank flows. The desolvation tank 221 is provided with a decompression device (not shown) that depressurizes the internal decompression space 221A into which the polymerization solution is introduced, and the desolvation tank 221 is constructed in a depressurization resistant structure. The decompression device and the solvent removal tank 221 constitute the decompression means of the present invention. This decompression device is preferably used in common with the decompression device of the volatile component gas recovery means 222 to simplify the plant equipment.
The decompression device is preferably configured to be able to fully vacuum the inside of the solvent removal tank 221 at 0.5 kPa or less (4 torr or less). That is, the amount of the remaining volatile component is required to be 200 ppm by mass or less, preferably 100 ppm by mass or less, in order to prevent deterioration of product quality due to the odor of the volatile component. Thus, based on the vapor-liquid equilibrium value between the polyolefin and the volatile component, when the temperature is set to 230 ° C., which is a temperature condition at which the polyolefin does not change, it is set to 0.5 kPa or less (4 torr or less).

In addition, the polymerization solution inflow passage 223 is a delivery pump (not shown) for sending the polymerization solution in the monomer removal tank to the solvent removal tank 221, a heat exchange means 224 as a heating means, and a downstream side of the heat exchange means 224. A pressure adjusting valve 225 as a pressurizing means is provided on the solvent removal tank 221 side.
The heat exchange means 224 heats the polymerization solution by using heat exchange with the polymerization means 210 of the latent heat of vaporization heat removal method, that is, heat removed during the polymerization reaction, for example. Specifically, when propylene is homopolymerized, it may be heated to about 230 ° C to 250 ° C. That is, the polymer may be heated to a high temperature at which a vapor pressure that does not change the quality and can sufficiently foam the volatile component at the time of decompression at a later stage is obtained. Specifically, since the amount of remaining volatile components is determined by the vapor-liquid equilibrium between the polyolefin and the volatile components depending on the conditions of temperature and pressure, it is necessary to increase the degree of vacuum in the treatment tank as the temperature decreases. . For this reason, it is necessary to set a high degree of vacuum that is difficult to set industrially if the temperature is lower than 230 ° C., and if heated higher than 250 ° C., the polymer is decomposed to lower the molecular weight or the color. This is because the polymer may be deteriorated such as.
The pressure adjustment valve 225 adjusts the pressure so that the polymerization solution flowing through the polymerization solution inflow passage 223 flows at a pressure that does not foam when heated by the heat exchange means 224. That is, since the vapor pressure varies depending on the composition of the polymerization solution, the pressure at which the polymerization solution does not foam may be set according to the vapor pressure, and foaming can be prevented by adjusting the pressure higher than the vapor pressure.

In addition, a dome portion 221B is provided at an upper portion of the solvent removal tank 221 to which the polymerization solution inflow passage 223 is connected. A porous member 226 is provided on the bottom surface of the dome portion 221B facing the decompression space 221A. As shown in FIG. 3, the porous member 226 has a disk shape and a plurality of flow paths 226A having an axial direction along the thickness direction.
These flow paths 226A may be formed with a diameter of 2 mm or more and 15 mm or less, preferably 3 mm or more and 7 mm or less, for example, when the viscosity of the polymerization solution is about the same as that of polypropylene obtained by homopolymerizing propylene as a polymer. This is because if the diameter of the flow path 226A is smaller than 2 mm, the polymerization solution hardly flows, pressure loss increases, and it may be difficult to improve the production efficiency. On the other hand, when the diameter of the flow path 226A is larger than 15 mm, when the volatile component is foamed in the polymerization solution flowing through the flow path 226A, the foaming does not reach the outer surface side of the polymerization solution, and the polymerization solution cannot be broken. It is because there exists a possibility of melt | dissolving in again. That is, in order to break the bubbles efficiently, the surface area of the polymerization solution needs to be increased. However, if the diameter of the channel 226A is larger than 15 mm, it is difficult to obtain the bubble breaking effect due to the increased surface area.
Furthermore, the pitch of the flow paths 226A is preferably 7 mm or more and 16 mm or less. When the pitch of the flow path 226A is narrower than 7 mm, in the case of a polymerization solution having a relatively high viscosity, the bubbles swell at the downstream end of the flow path 226A and stick to the adjacent bubbles before they break up like a balloon. There is a risk that foam cannot be broken well. Furthermore, it is necessary to increase the thickness of the porous member 226 so that the strength does not decrease, which may cause inconveniences such as an increase in the size of the apparatus and an increase in the cost of the porous member 226. On the other hand, if the pitch of the flow paths 226A is larger than 16 mm, the surface area of the polymerization solution when passing through the porous member 226 decreases, and there is a possibility that bubbles cannot be broken sufficiently. Furthermore, it is necessary to provide a plurality of flow paths 226A so that the surface area of the polymerization solution does not decrease, and the diameter of the porous member 226 increases, which may cause inconveniences such as an increase in the size of the apparatus and an increase in the cost of the porous member 226. is there. From these facts, the pitch of the flow path 226A is designed to be 7 mm or more and 16 mm or less.
The ratio of the hole diameter of the flow path 226A to the pitch dimension of the flow path 226A, that is, the relationship (D / L) between the diameter (D) of the flow path 226A and the pitch (L) is 0.4 or less, particularly propylene homopolymerization. In this case, 0.3 is preferable. Here, if the value of L is too small with respect to D, it is difficult to obtain an effect of dispersing the polymer by adhering to the polymerization solution flowing through the adjacent flow path 226A, and if the value of L is too large with respect to D. This is because the porous member 226 becomes large, the equipment becomes large, and the equipment cost may increase. That is, the porous member 226 is not limited to the purpose of merely breaking bubbles but is also intended to disperse the polymer.
The bottom of the solvent removal tank 221 is provided with a transfer pump 227A for sending the polymer solution from which volatile components are highly removed to the granulating means 230 in the next step, and an outflow passage 227 is connected.

The granulating means 230 includes a cooler (not shown), a granulator, a cooling tank, and the like.
The cooler cools the polymerization solution transferred from the solvent removal tank 221 to a temperature having a certain degree of viscosity that enables granulation.
The granulator allows the polymer cooled by the cooler to flow out of the mold nozzle and spray water, and then cut into pellets with a rotary cutting blade spaced from the outlet of the mold nozzle by a predetermined gap. .
A cooling tank fully cools the pellet-shaped polymer granulated with the granulator, stirring with the water sprayed at the time of granulation. That is, since the cooling tank is not completely solidified at the time of granulation, in order to prevent inconvenience that the pellets adhere to each other after granulation, the cooling tank is sufficiently cooled to a temperature at which the pellets do not adhere to each other while stirring. A coalescence is produced.
The produced olefin polymer is appropriately stored in a storage hopper or the like.

As the control device 300, for example, a computer is used to control the operating conditions of the polymerization equipment 200. Specifically, the supply amount of the raw material from the raw material supply means 211, the supply amount of the solvent from the solvent supply means 212, the supply amount of the catalyst from the catalyst supply means 213, the supply amount of hydrogen gas from the hydrogen gas supply means 214 The supply amount of the third component from the third component supply means 215, the temperature of the polymerization solution by circulating the gas phase in the polymerization tank, the pressure at which the devolatilization means 220 depressurizes, the heat exchange means 224 The heating temperature, the pressure applied by the pressure adjusting valve 225, the flow rate control by driving control of the transfer pump 227A, the cooling temperature in the granulating means 230, the rotational speed of the rotary cutting blade, and the like are controlled.
Here, the computer is not limited to a single personal computer, but a configuration in which a plurality of computers are combined in a network form, a circuit such as a CPU (Central Processing Unit) or a microcomputer, or a plurality of electronic components. It also includes a substrate.
Further, the control device 300 sets the volatile component content in the polymer solution after the decompression process to 200 mass ppm or less based on the concentration of the polyolefin, the temperature of the polymer solution, the vapor pressure of the polymer solution, and the time length of the decompression process. The preset conditions, that is, the pressure applied by the pressure adjusting valve 225, the temperature heated by the heat exchange means 224, the pressure reduced by the pressure reducing means, the flow rate of the polymerization solution, and the like are controlled.
Specifically, as shown in FIG. 4, since there is a predetermined relationship between the vapor pressure and temperature of the volatile component at the concentration of the polymer in the polymerization solution, based on the characteristics of the vapor pressure based on the composition of the polymerization solution. The pressure for depressurization, the temperature for heating in the heat exchange means 224, the flow rate for the size of the demonomer tank and the solvent removal tank 221 that will be the time length of the depressurization process are set, and the polymerization equipment 200 is controlled according to the set numerical values . FIG. 4 is a graph showing the relationship between the polymer concentration, the vapor pressure of the volatile component, and the temperature by heat exchange calculation at the position where the polymerization solution inflow passage 223 is connected in the solvent removal tank 221.

Here, the vapor-liquid equilibrium of the polymerization solution is an equilibrium state between the gas phase and the liquid phase of the mixture, and depends on gas-liquid equilibrium data which are factors of temperature, pressure, gas phase composition, and liquid phase composition. The liquid phase of the polymerization solution is a mixture of a polymer that is a polymer having no vapor pressure and a volatile solute.
When a non-volatile substance is dissolved in the solute, the vapor pressure P of the solution becomes lower than the vapor pressure P ₀ of the pure solvent. In the case of an ideal solution, the vapor pressure drop is proportional to the mole fraction and the vapor pressure according to the Laoult rule (P = P ₀ × (1−x); x is the mole fraction). However, when the non-volatile substance is a polymer, it deviates from Raoul's law and causes a very large vapor pressure drop.
Since the vapor-liquid equilibrium of the polymerization solution varies depending on the solute properties of the polymer and the volatile substance, as described later, vapor-liquid equilibrium data was calculated based on experiments. The Flory-Huggins equation is generally used to correlate and estimate the yield of solutes in the polymer, but the multi-component expandability and the entire process are expressed in one solution model. From the point that can be achieved, an NRTL (Non Random Two-Liquid) equation (see H. Renon, and JN Prausnitz, AIChE J. 14. (1), 135-144 (1968)) is used. In this case, since the polymer cannot be handled as it is, the polymer is substituted with n-C36. The substitute for n-C36 is only the molecular weight, and the specific volume uses the value of the polymer.

Specifically, as a correlation procedure, first, parameters are set to Flory-Huggins equation (PJFlory, J. Chem. Phys. 10, 51 (1942) and MLHuggins, J. Phys. Chem. 46, 151 (1942); Ann. NYAcad.Sci.41,1 (1942); J.Am.Chem.Soc.64, 1712 (1942)), and the relationship between solute partial pressure and solubility in a finite concentration range is obtained. After this, the NRTL parameters are optimized. In this optimization, it was expressed by a temperature-dependent type shown in the following formula (3) so that it can be used in a wide temperature range.
(Formula 3)
τ _ij = a _ij + b _ij / T
T: Temperature Then, the results of the correlated parameters are compared with the calculation based on the Flory-Huggins equation, and it can be confirmed that even the NRTL can express the vapor-liquid equilibrium of the polymer-solute system.

By such an estimation method, the relationship between the temperature and the vapor pressure in the composition of the polymerization solution during operation was estimated.
In addition, when estimating gas-liquid equilibrium by heat exchange of each process in this embodiment, it is necessary to calculate about the composition of the exit of the polymerization tank of the superposition | polymerization means 210, and the composition of the exit of the devolatilization tank of the devolatilization means 220. For this reason, since the concentration and composition of the polymer at each outlet differ depending on the polymerization conditions and the operating conditions of the demonomer tank, it is necessary to calculate for each different condition.

  In this embodiment, the results of gas-liquid equilibrium calculated by the above-described estimation method for the concentration of the polymer (polyolefin / (polyolefin + propylene + heptane)) in the polymerization solution (polyolefin, propylene, heptane) are shown in FIG. 5 and 6. These FIGS. 5 and 6 show the results of gas-liquid equilibrium in a polymerization solution obtained by polymerizing a polymerization solution at a temperature of 78 ° C. and a pressure of 1.6 MPa in a polymerization tank to a concentration of 30% by mass in a polymerization monomer. Is shown.

[Production of olefin polymer]
The control device 300 recognizes the necessary amount of raw materials based on the production plan data acquired in advance, and supplies the raw material supply means 211, the solvent supply means 212, the catalyst supply means 213, the hydrogen gas supply means 214, and the third component supply means 215. Are controlled to supply necessary amounts of raw material, solvent, catalyst, hydrogen gas, and third component to the polymerization tank of the polymerization means 210.
Then, the control device 300 circulates the gas phase component in the polymerization tank while appropriately cooling it with a cooler (not shown), and controls the temperature of the polymerization solution in the polymerization tank to advance the polymerization reaction.

Thereafter, the control device 300 transfers the polymerization solution in the polymerization tank to the devolatilization tank of the devolatilization unit 220 and removes volatile components from the polymerization solution by the volatile component gas recovery unit 222 that is separately driven and controlled. . As operation control of the volatile component gas recovery means 222, the volatile component gas recovery means 222 is retained in a demonomer tank depressurized to a predetermined pressure until the concentration of the polymer in the polymerization solution becomes 90% by mass or more. That is, based on the relationship between the vapor pressure and temperature of the volatile component in the concentration of the polymer in the polymerization solution, the pressure, flow rate, etc., to be reduced are controlled.
Then, the control device 300 causes the polymerization solution in which the volatile component is removed so that the concentration of the polymer in the polymerization solution is 90% by mass or more in the demonomer tank to flow into the desolvation tank 221 through the polymerization solution inflow path 223. When this polymerization solution flows through the polymerization solution inflow passage 223, it is pressurized to a predetermined pressure, that is, a pressure at which it does not foam during heating, by the pressure adjustment valve 225 of the polymerization solution inflow passage 223 controlled by the control device 300. It becomes. Further, the polymerization solution is heated by heat exchange to a predetermined temperature by the heat exchange means 224 controlled by the control device 300. Then, the polymer solution heated in the pressurized state flows through the pressure adjusting valve 225, and immediately flows while foaming into the dome portion 221B of the solvent removal tank 221 that has been depressurized to a predetermined pressure by the control device 300. .
The foamed polymerization solution is in a state where a large number of bubbles are mixed without breaking. Then, the polymerization solution in which the bubbles are mixed flows through the plurality of flow paths 226A of the porous member 226. During this distribution, the polymerization solution further foams and the bubble diameter increases, and bubbles mixed in the polymerization solution appear on the outer surface of the polymerization solution which is the inner surface of the flow path 226A, and the bubbles break. . That is, when the polymerization solution flows through the plurality of flow paths 226A, the surface area is increased. As a result, bubbles mixed in the inside appear on the outer surface of the polymerization solution and break the bubbles. The volatile components separated by the bubble breaking are recovered by the volatile component gas recovery means 222 from the top of the solvent removal tank 221 so as not to be redissolved in the polymerization solution.

The polymer, which is a polymerization solution in which the volatile components are sufficiently separated by the devolatilization means 220, for example, the residual volatile components are separated to 200 ppm or less, is provided with a transfer pump 227A to the granulation means 230 via the outflow passage 227. Be transported.
In this granulating means 230, the polymer transferred by the cooler controlled by the control device 300 is cooled and granulated into pellets by the granulator. The pelletized polymer after granulation is immediately cooled and solidified sufficiently in a cooling bath so as not to adhere to each other, and a pellet-shaped olefin polymer is produced.
The cooled and solidified polymer is appropriately removed after moisture, and then transferred to a storage hopper or the like and appropriately stored.

[Effects of Embodiment]
In the embodiment described above, after heating the polymerization solution in the heat exchange means 224 in a state of being pressurized by the pressure adjustment valve 225, the remaining volatile components are caused to flow by flowing into the desolvation tank 221 having a reduced pressure, A plurality of flow paths 226A of the porous member 226 disposed in the solvent removal tank 221 are circulated to break the bubbles.
For this reason, it is sufficient to sufficiently pressurize the pressure adjusting valve 225 appropriately adjusted according to the properties of the polymerization solution so that the remaining volatile components do not foam when heated by the heat exchanging means 224. With a simple process of adjusting the pressure at 225, the polymerization solution can be efficiently heated without loss. Therefore, the polymerization solution that has been efficiently heated to a temperature at which the vapor pressure necessary for sufficiently foaming the remaining volatile components is sufficiently foamed and broken by the porous member 226. Even if it flows out and returns to the atmospheric pressure state, it is possible to prevent the inconvenience that the volatile components are dissolved again and cannot be sufficiently separated, and the volatile components can be separated and removed to a high degree.

In the present embodiment, the pressure adjusting valve 225 adjusts the pressure so as not to foam when the polymerization solution is heated by the heat exchange means 224.
For this reason, it is possible to prevent the disadvantage that the heat transfer coefficient decreases due to foaming during heating, and the polymerization solution cannot be sufficiently heated and the remaining volatile components cannot be sufficiently foamed. Therefore, the polymerization solution can be efficiently heated to a temperature at which the vapor pressure is necessary to sufficiently foam the remaining volatile components, and the volatile components can be separated and removed to a high degree.

In this embodiment, the ratio (D / L) of the hole diameter (D) of the flow path 226A to the pitch dimension (L) of the flow path 226A of the porous member 226 is set to 0.4 or less.
For this reason, while suppressing an increase in flow resistance, it is possible to achieve a state in which the surface area where bubbles in the polymerization solution are located on the surface and easily breaks during flow increases, and the surface area is increased efficiently. Even if the bubbles can flow and flow out of the solvent removal tank 221 and return to the atmospheric pressure state, it is possible to prevent the disadvantage that the volatile components in the bubbles are dissolved again and cannot be sufficiently separated, and the volatile components can be highly separated and removed.

Furthermore, in the present embodiment, before the volatile component is foamed and separated by bubble breakage in the solvent removal tank 221 provided with the porous member 226 heated and depressurized by the heat exchange means 224 under pressure, Volatile components are removed until the polymer concentration reaches 90% by mass or more.
That is, when removing the volatile component in one operation, the equipment for sufficiently reducing the pressure in order to remove the volatile component highly becomes large while separating and collecting the volatile component that is volatilized in a large amount. For this reason, when there is a restriction on the enlargement of the equipment, as in this embodiment, the polymerization solution from which the volatile components have been removed to a polymer concentration of 90% by mass or higher in advance is heated under pressure to remove the solvent. By adopting a configuration in which the pressure is reduced at 221, volatile components can be separated and removed at a high level without increasing the size of the equipment.

Further, in order to remove volatile components in one operation, it is necessary to increase the temperature by the heat exchanging means 224, and it is necessary to maintain a high pressure at which the volatile components in the polymerization solution heated to a high temperature are not vaporized. There is a risk of increase in size and complexity. In addition, the high temperature may cause inconveniences such as decomposition of the polymer, decrease in molecular weight, and deterioration of color.
For this reason, a multi-stage configuration in which a part of the volatile components is removed in advance in a demonomer tank, and further, a desolvation tank after being processed by a pre-treatment unit that depressurizes and removes a part of the volatile components after pressurizing and heating the polymerization solution. A multi-stage configuration is used for processing at 221. With these structures, inconveniences such as simplification of the apparatus and alteration of the polymer can be prevented.
In particular, as the pretreatment, it is preferable to have a multistage configuration in which pretreatment means for removing volatile components by heating and pressurizing and then removing volatile components after the treatment of the monomer removal tank is provided. Specifically, a pre-stage pressurizing unit that pressurizes the polymerization solution, a pre-stage heating unit that heats the pressurized polymerization solution under pressure, and a pre-stage depressurization unit that depressurizes the pressurized and heated polymerization solution. The pretreatment means is provided between the demonomer tank and the heat exchange means 224 of the solvent removal tank. With this configuration, the configurations of the heat exchange means 224, the pressure adjustment valve 225, and the solvent removal tank 221 are connected in multiple stages. With this configuration, it is possible to highly remove volatile components without deteriorating the polymer while suppressing the increase in size and complexity of the apparatus as compared with the case of removing volatile components in one operation.

And in this embodiment, it heats at 230 degreeC or more and 250 degrees C or less.
Therefore, the polymer is not denatured and heated at a high temperature at which the volatile components in the polymerization solution are sufficiently vaporized so that the volatile components in the polymerization solution can be sufficiently foamed during decompression in the solvent removal tank 221, so that the volatile components can be separated and removed to a high degree.

In the present embodiment, the pressure is reduced to 0.5 kPa or less in the solvent removal tank 221.
For this reason, it is possible to lower the temperature at which the vapor pressure of the volatile component in the polymerization solution is sufficiently foamed, and to efficiently separate and remove the volatile component efficiently.

In this embodiment, as a configuration for pressurizing the polymerization solution, a pressure adjustment valve 225 is disposed between the heat exchange means 224 and the solvent removal tank 221.
For this reason, even if the properties of the polymerization solution change, such as changes in viscosity and temperature, it can be easily adjusted to a pressurized state where the heat exchange means 224 does not foam, and the remaining volatile components are sufficiently foamed to a high degree. It can be easily removed with a simple configuration.

In the present embodiment, the pressure adjustment valve 225 is disposed in the vicinity of the solvent removal tank 221.
For this reason, since the path for allowing the pressurized polymerization solution to flow into the desolvation tank 221 that has been depressurized is short or almost absent, the foaming is performed before flowing into the desolvation tank 221 when the pressure is released. However, the transfer to the solvent removal tank 221 is not affected and the treatment can be performed stably.

And it is suitable for manufacture of a low molecular weight low regularity polypropylene.
Low molecular weight low regularity polypropylene foams and breaks the solvent in the polymer in a short time, so it is easy to reach the amount of solvent in the polymer in parallel while the polymer is devolatilized in the solvent removal tank. It is suitable because it can be easily devolatilized and the size of the apparatus can be easily reduced.

[Modification of Embodiment]
The aspect described above shows one aspect of the present invention, and the present invention is not limited to the above-described embodiment, and is within a range in which the object and effect of the present invention can be achieved. Needless to say, modifications and improvements are included in the content of the present invention. In addition, the specific structure and shape when implementing the present invention can be applied to other structures and shapes as long as the objects and effects of the present invention can be achieved.

That is, the configuration in which the operation condition of the polymerization equipment 200 is controlled by the control device 300 to automatically operate the polymerization device 100 is illustrated, but the configuration is not limited thereto. For example, it is good also as a structure set as the manual driving | operation which sets and sets driving | running conditions manually manually.
Further, the production is not limited to the continuous type, and may be a batch type.
Moreover, although it controlled based on Formula 1 mentioned above as conditions at the time of controlling with the control apparatus 300, it is not restricted to the conditions of Formula 1 as control conditions.

And as an olefin, various olefins, such as ethylene, propylene, butylene, can be made into object.
Furthermore, the polyolefin to be produced is not limited to a homopolymer such as polyethylene or polypropylene, but can also be applied to the case of producing a copolymer of ethylene and propylene.

As the devolatilizing means 220, a two-stage configuration of the demonomer tank and the desolvation tank 221 is illustrated, but it may be a single-stage configuration or a multi-stage configuration of three or more stages.
In particular, since a structure that does not foam when heated by the heat exchanging means 224 while applying pressure is preferable, it is preferable that the concentration of the polymer is, for example, 90% by mass or more when applying pressure and heating. Therefore, a volatile component can be separated and removed efficiently and easily by using a multi-stage configuration. In addition, the volatile component may not be removed until the polymer concentration is 90% by mass or more in the demonomer tank. That is, pressure may be applied so as not to foam during heating.
The pressurizing means is not limited to the pressure adjusting valve 225. For example, various pressurizing configurations such as press-fitting into the container using a pump or the like to pressurize the polymerization solution can be used.
Similarly, the heating configuration is not limited to the heat exchange means 224, and various heating methods such as heating the outside of the container for storing the polymerization solution with a heater or the like can be used. It is preferable that the heat exchange using the heat generated in the polymerization means 210 can effectively use energy and can be efficiently manufactured.

Further, in the configuration in which propylene is homopolymerized, for example, when the pressure to be reduced in the solvent removal tank 221 can be highly reduced to 0.5 kPa or less, the heat exchange means 224 may not be heated to 230 to 250 ° C. .
Furthermore, the pressure to be reduced is not limited to 0.5 kPa or less.

And as a porous member, it is not restricted to D / L <= 0.4, Any thing is applicable if a bubble-breaking and a dispersion effect are acquired.
Further, as the porous member, for example, a porous member such as a pumice or the like in which the flow path is not linear but bent or branched, or a mesh member may be used.

  In addition, the specific structure and procedure for carrying out the present invention may be changed to other configurations as long as the object of the present invention can be achieved.

  Next, the present invention will be described more specifically with reference to examples and comparative examples. In addition, this invention is not limited to the content of an Example etc. at all.

Example 1
Using the above-described polymerization apparatus, heptane 17 kg / h, triisobutylaluminum 28 mmol / h, hydrogen 37 NL / h, propylene 10 kg / h, catalyst ((1,2′-dimethylsilylene) (2,1′dimethylsilylene) -bis (3-Trimethylsilylmethylindenyl) zirconium dichloride) was continuously fed at 9 μmol / h and polymerized at a temperature of 70 ° C. and a pressure of 0.9 MPa.
The polymerization solution was added with ethanol to deactivate the catalyst, and after removing unreacted propylene in the demonomer tank, it was heated with a heat exchanger, and the polymer solution was heated at a temperature of 135 ° C. and a pressure of 20 kPaA in the solvent removal tank. It was previously devolatilized to a concentration of 96% by mass.
This pre-devolatilized polymerization solution was adjusted to 0.5 MPa with an outlet valve using a multi-tube ring heat exchanger equipped with 13 tubes with a tube inner diameter of 7 mm and a length of 1.2 m. Heated to 230 ° C. A porous member having a plurality of flow paths having a thickness of 3 mm, a hole diameter of 3 mm, and a pitch of 7 mm was provided, and was allowed to flow into a solvent removal tank having a pressure of 0.5 kPaA. The temperature of the polymer after devolatilization was 226 ° C., and the polymer was extracted with a gear pump installed at the bottom of the solvent removal tank, and the residual volatile substances were analyzed. The analysis method of this residual volatile substance is a gas chromatogram.
The residual volatile substance was 100 mass ppm.
(Example 2)
The devolatilization treatment was performed in the same manner as in Example 1 except that the pressure in the solvent removal tank in the pre-devolatilization in Example 1 was 140 kPaA and the polymer concentration was 87% by mass. The temperature of the polymer after devolatilization was 218 ° C.
Residual volatile material was 150 ppm by mass.
(Example 3)
The devolatilization treatment was performed in the same manner as in Example 1 except that the porous member having a pore diameter of 15 mm during the devolatilization treatment in Example 1 was used. The temperature of the polymer after devolatilization was 226 ° C.
The residual volatile material was 120 mass ppm.
(Comparative Example 1)
The devolatilization was carried out in the same manner as in Example 1 except that the porous solvent was not used in the solvent removal tank in Example 1 and the pre-devolatilized polymerization solution was treated by flowing into the solvent removal tank through a 11 / 2B pipe. Processed.
Residual volatile material was 200 ppm by weight. The temperature at the outlet of the multi-tube ring heat exchanger increased only to 190 ° C.

  From the results of the above examples, the residual volatile substances are efficiently removed by circulating the polymer solution through a porous member having a specified pore diameter with a polymer concentration of 90% by mass or more particularly at the inlet of the devolatilization treatment. did it.

  The present invention relates to an apparatus for removing a volatile component from a polymerization solution for removing a volatile component from a polymerization solution when a polyolefin is produced by homopolymerization or copolymerization of an olefin using a solvent, and further a polymerization equipped with this volatile component removal apparatus. Available for equipment.

DESCRIPTION OF SYMBOLS 100 ... Polymerization apparatus 210 ... Polymerization means 220 ... Volatilization means as a volatile component removal apparatus 221 ... Desolvation tank 221A ... Pressure reduction space 224 ... Heat exchange means 225 as heating means 225 ... Pressure regulating valve 300 as a pressurizing means 300... Control device as a controlling means

Claims (13)

A pressurizing means for pressurizing the polymerization solution obtained by polymerizing the olefin using a solvent;
Heating means for heating the polymer solution pressurized by the pressurizing means under pressure;
Decompression means having a decompressed decompression space into which the pressurized and heated polymerization solution is introduced;
A plurality of flow paths through which the polymerization solution can be circulated, and a porous member disposed in the reduced pressure space in a state in which the polymerization solution that has flowed into the reduced pressure space of the pressure reducing means flows through the flow path;
Equipped with,
The decompression means comprises a solvent removal tank that constitutes the decompression means and has the decompression space,
The desolvation tank is connected to a polymerization solution inflow passage through which the pressurized and heated polymerization solution is introduced, and is connected to an outflow passage through which the polymerization solution in the reduced pressure space flows out.
The porous member is disposed in the decompression space between the polymerization solution inflow path and the outflow path so that the polymerization solution inflow path side and the outflow path side can flow through the flow path,
The apparatus for removing a volatile component of a polymerization solution, wherein the pressurizing unit pressurizes the polymerization solution to a pressure that does not foam when the polymerization solution is heated by the heating unit. It is a volatile component removal apparatus of the polymerization solution of Claim 1 ,
The porous member has a ratio (D / L) of a pore diameter (D) of the flow path to a pitch dimension (L) of the flow path of 0.4 or less. A volatile component removal apparatus for a polymerization solution according to claim 1 or 2 ,
The polymerization solution heated by the heating means has a polyolefin concentration of 90% by mass or more. It is a volatile component removal apparatus of the polymerization solution as described in any one of Claim 1- Claim 3 , Comprising:
The said heating means heats to 230 degreeC or more and 250 degrees C or less. The volatile component removal apparatus of the polymerization solution characterized by the above-mentioned. It is a volatile component removal apparatus of the polymerization solution as described in any one of Claim 1- Claim 4 , Comprising:
The apparatus for removing a volatile component of a polymerization solution is characterized in that the pressure reducing means reduces the pressure to 0.5 kPa or less. It is a volatile component removal apparatus of the polymerization solution as described in any one of Claim 1- Claim 5 ,
The apparatus for removing a volatile component of a polymerization solution, wherein the pressurizing unit includes a pressure adjusting valve disposed between the heating unit and the depressurizing unit. It is a volatile component removal apparatus of the polymerization solution of Claim 6 , Comprising:
The apparatus for removing a volatile component of a polymerization solution is characterized in that the pressurizing means is disposed on the upstream side in the direction in which the polymerization solution flows from a position connected to the solvent removal tank in the polymerization solution inflow path . It is a volatile component removal apparatus of the polymerization solution as described in any one of Claim 1- Claim 7 ,
The polymerization solution has an intrinsic viscosity of 0.5 dL / g or more and 15.0 dL / g or less. It is a volatile component removal apparatus of the polymerization solution as described in any one of Claim 1- Claim 8 ,
The polyolefin has an isotactic pentad fraction of 20 mol% or more and 60 mol% or less. A volatile component removal apparatus for a polymerization solution according to any one of claims 1 to 9 ,
The polyolefin is a polypropylene having a weight average molecular weight (Mw) of 2 or more and 400,000 or less . A volatile component removal apparatus for a polymerization solution according to any one of claims 1 to 10 ,
Pre-pressurizing means for pressurizing the polymerization solution, pre-heating means for heating the polymerization solution pressurized by the pre-pressurizing means under pressure, and reduced pressure at which the pressurized and heated polymerization solution flows A pre-stage depressurization means having a reduced pressure space, and comprising a pre-stage treatment means for supplying the polymerization solution decompressed by the pre-stage depressurization means to the pressurization means. apparatus. A method for removing volatile components from a polymerization solution, wherein a volatile component is removed from a polymerization solution obtained by polymerizing olefin using a solvent,
A pressurizing / heating step of heating the polymerization solution under pressure;
When carrying out the foaming / bubble breaking step of circulating the polymer solution pressurized and heated in this pressurizing / heating step through a plurality of channels provided in the porous member under reduced pressure ,
In the pressurizing / heating step, the heated polymerization solution is pressurized at a pressure that does not cause foaming . A polymerization means for polymerizing olefin in a solvent;
The apparatus for removing a volatile component of a polymerization solution according to any one of claims 1 to 11 , wherein a volatile component is removed from a polymerization solution obtained by polymerizing the olefin by the polymerization means,
A granulating means for granulating the polymerization solution from which the volatile components have been removed by the polymerization solution volatile component removal apparatus;
A polymerization apparatus characterized by comprising:

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