CN107177017B - System and method for removing volatile components in high-viscosity polymer - Google Patents
System and method for removing volatile components in high-viscosity polymer Download PDFInfo
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- CN107177017B CN107177017B CN201610135706.8A CN201610135706A CN107177017B CN 107177017 B CN107177017 B CN 107177017B CN 201610135706 A CN201610135706 A CN 201610135706A CN 107177017 B CN107177017 B CN 107177017B
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Abstract
The embodiment of the invention provides a system and a method for removing volatile components in a high-viscosity polymer, wherein the system comprises: first volatilizer, second volatilizer and the heat exchanger that corresponds every volatilizer, first volatilizer includes: first separation chamber, first solution import, first solution export and first gas outlet, first volatilizer still includes: the separating surface of the distributor is provided with a plurality of first distribution holes; the distributor is located in the first separation chamber and connected to a lower end of the first solution inlet so that the high-viscosity polymer solution introduced from the first solution inlet is brought into contact with the separation surface of the distributor. The first evaporator is internally provided with the distributor which is simple in structure and provided with the first distribution holes, so that the system provided by the invention is easy to install and maintain; by applying the system and/or the method provided by the invention, the content of volatile components in the high-viscosity polymer can be effectively reduced, and the polymer with higher purity can be obtained.
Description
Technical Field
The invention relates to the technical field of removing volatile components in polymers, in particular to a system and a method for removing volatile components in high-viscosity polymers.
Background
The removal of volatiles (also called devolatilization) from polymers is an important process in the polymer production process, mainly the separation of unreacted monomers and low boiling solvents.
The existing method for removing volatile components from polybutene can reduce the amount of residual monomers and solvent in polybutene to 100PPM, for example, patent CN1662561A of Italian company, Barcel polyolefin, FIG. 1 is a system structure diagram of the method for removing volatile components from polybutene disclosed in the patent, and monomer butene is prepared into polybutene in the polymerization zone as shown in FIG. 1; removing residual catalyst from the solution in a deactivation tank 20; heating and pressurizing the butylene to a supercritical state through a first heat exchanger 40; and the gaseous butene-1 monomer is conveyed into a first volatilizer 50 to be separated by gravity and recovered through a pipeline 4, and the polybutene melt falls to realize the volatile removal, so that the content of the gaseous butene-1 monomer in the polybutene solution is less than 10-6 percent; then heated by a second heat exchanger 70 and conveyed to a second volatilizer 80 in a vacuum state for secondary volatilization, a gaseous butene-1 monomer is recovered through a channel 7, and a polybutene melt falls down to realize secondary volatilization; finally, the polybutene is underwater granulated to obtain a high purity product.
However, in the solution for removing gaseous butene-1 monomer from polybutene disclosed in patent CN1662561A, the viscosity of the polymer solution is very high when the polybutene is subjected to devolatilization in the first volatilizer 50 and the second volatilizer 80, especially when the polybutene is subjected to the second volatilizer 80, which is not favorable for separating gaseous butene-1 monomer from the polymer, and the content of butene-1 monomer in the polymer discharged from the second volatilizer 80 is 100 PPM. Therefore, the effect of removing gaseous butene-1 monomer from polybutene disclosed in patent CN1662561A is not ideal.
In order to further reduce the content of volatile components in the polymer, there is also a prior art in which a distributor is installed in the first volatilizer 50 or the second volatilizer 80 to improve the effect of removing volatile components in the polymer, for example, patent CN1986619A of the soxhlet chemical technology ltd, but the distributor is too complicated in structure, high in installation and maintenance costs, and the effect of removing volatile components when the distributor is statically distributed for a solution with high viscosity is not desirable.
Disclosure of Invention
An object of the embodiments of the present invention is to provide a system and a method for removing volatile components from a high viscosity polymer, so as to simplify the structure of a volatilizer, effectively reduce the content of volatile components in the polymer, and improve the purity of the polymer product.
In order to achieve the above object, an embodiment of the present invention provides a system for removing volatile components from a high viscosity polymer, including: a first volatilizer 50, a second volatilizer 80 and a heat exchanger corresponding to each volatilizer, said first volatilizer 50 comprises: a first separation chamber 501, a first solution inlet 502, a first solution outlet 503 and a first gas outlet 504, and the second volatilizer 80 comprises: a second separation chamber 801, a second solution inlet 802, a second solution outlet 803 and a second gas outlet 804,
the first volatilizer 50 further comprises: a distributor 505, wherein a plurality of first distribution holes 506 are arranged on a separating surface of the distributor 505;
the distributor 505 is located in the first separation chamber 501 and connected to the lower end of the first solution inlet 502 so that the high-viscosity polymer solution introduced from the first solution inlet 502 is brought into contact with the separation surface of the distributor 505.
Preferably, the diameter of the distribution hole in the plurality of first distribution holes 506 opened in the separation surface of the distributor 505, which is closer to the first solution inlet 502, is smaller than the diameter of the distribution hole which is farther from the first solution inlet 502.
Preferably, the density of distribution holes in the plurality of first distribution holes 506 opened in the separation surface of the distributor 505, which are closer to the first solution inlet 502, is greater than the density of distribution holes which are farther from the first solution inlet 502.
Preferably, the separating surface of the distributor 505 is circular, and the outer diameter of the distributor 505 is smaller than the inner diameter of the first separating cavity 501.
Preferably, a plurality of first distribution holes 506 in the distributor 505 are arranged in parallel in each distribution row, the distribution rows being perpendicular to the axis of the first solution inlet 502, wherein the first distribution holes 506 in the distribution row that is closer to the first solution inlet 502 have a smaller pore size than the first distribution holes 506 in the distribution row that is farther from the first solution inlet 502; the density of the first distribution holes 506 in the distribution row that is closer to the first solution inlet 502 is greater than the density of the first distribution holes 506 in the distribution row that is farther from the first solution inlet 502.
Preferably, said first volatilizer 50 further comprises: a distribution screen 507;
the distribution screen 507 is located in the first separation cavity 501 and fixed below the distributor 505, and a plurality of second distribution holes 508 are formed in the distribution screen 507.
Preferably, the distribution screen 507 is circular, and the outer diameter of the distribution screen 507 is equal to the inner diameter of the first separation chamber 501.
Preferably, the second solution inlet 802 is located at the top of the second volatilizer 80 and is connected with the outlet of the heat exchanger corresponding to the second volatilizer 80.
The embodiment of the invention also provides a method for removing volatile components in the high-viscosity polymer, which comprises the following steps:
heating the high viscosity polymer solution in a heat exchanger corresponding to the first volatilizer 50 to obtain a first mixture comprising a polymer melt and volatiles in a supercritical state;
the first mixture enters the first separation chamber 501 of the first volatilizer 50 from the first solution inlet 502 and contacts the separation surface of the distributor 505 in the first separation chamber 501; a plurality of first distribution holes 506 are formed in the separation surface of the distributor 505, the distributor 505 is connected with the lower end of the first solution inlet 502, and the pressure of the first mixture entering the first separation cavity 501 from the first solution inlet 502 is higher than the pressure in the first separation cavity 501;
the supercritical volatile components in the first mixture on the separation surface of the distributor 505 are subjected to a first separation with the polymer melt to obtain a second mixture, wherein the supercritical volatile components in the first mixture are discharged through a first gas outlet 504 and recovered;
the second mixture is heated in a heat exchanger corresponding to the second volatilizer 80 and the heated second mixture is passed to the second volatilizer 80 for a second separation of the volatile components of the second mixture from the polymer melt.
Preferably, the temperature of the first mixture entering the first volatilizer 50 from the first solution inlet 502 is between 170 ℃ and 280 ℃.
Preferably, after the first separation of the supercritical volatile component from the polymer melt in the first mixture on the separation surface of the distributor 505 to obtain a second mixture, and before the second mixture is heated in the heat exchanger corresponding to the second volatilizer 80; the method further comprises the following steps:
the second mixture is contacted with the upper surface of a distribution screen 507 fixed below the distributor 505 in the first separation chamber 501, and a plurality of second distribution holes 508 are opened on the distribution screen 507.
Preferably, said passing the heated second mixture into the second volatilizer 80 comprises:
passing the heated second mixture from the second solution inlet 802 into the second volatilizer 80; wherein, the second solution inlet 802 is located at the top of the second volatilizer 80 and is connected with the outlet of the heat exchanger corresponding to the second volatilizer.
Preferably, the temperature of the second mixture entering the second volatilizer 80 through the second solution inlet 802 is between 170 ℃ and 280 ℃.
The embodiment of the invention provides a system and a method for removing volatile components in a high-viscosity polymer, wherein the system comprises: a first volatilizer 50, a second volatilizer 80 and a heat exchanger corresponding to each volatilizer, said first volatilizer 50 comprises: a first separation chamber 501, a first solution inlet 502, a first solution outlet 503 and a first gas outlet 504, and the second volatilizer 80 comprises: a second separation chamber 801, a second solution inlet 802, a second solution outlet 803 and a second gas outlet 804, wherein the first volatilizer 50 further comprises: a distributor 505, wherein a plurality of first distribution holes 506 are arranged on a separating surface of the distributor 505; the distributor 505 is located in the first separation chamber 501 and connected to the lower end of the first solution inlet 502 so that the high-viscosity polymer solution introduced from the first solution inlet 502 is brought into contact with the separation surface of the distributor 505. Because the first volatilizer 50 is provided with the distributor 505 which has a simple structure and is provided with the first distribution holes 506, the system for removing the volatile components in the high-viscosity polymer provided by the embodiment of the invention has a simple structure, is easy to install and maintain, and can effectively reduce the content of the volatile components in the polymer; the method for removing the volatile components in the high-viscosity polymer provided by the embodiment of the invention can effectively reduce the content of the volatile components in the high-viscosity polymer and obtain the polymer with higher purity. Of course, it is not necessary for any product or method of practicing the invention to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a system for removing volatile components from a high viscosity polymer provided in patent CN 1662561A;
fig. 2 is a cross-sectional structural view of a first evaporator according to an embodiment of the present invention;
fig. 3 is another sectional structural view of a first evaporator according to an embodiment of the present invention;
fig. 4 is a cross-sectional structural view of another first evaporator according to an embodiment of the present invention;
fig. 5 is a sectional structural view of another first evaporator according to an embodiment of the present invention;
FIG. 6 is a sectional view showing a structure of a second volatilizer provided in the embodiment of the present invention;
FIG. 7 is a flow chart of a method for removing volatiles from a high viscosity polymer according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiments of the present invention provide a system and a method for removing volatile components from a high viscosity polymer, which are described below separately, and first, a system for removing volatile components from a high viscosity polymer is described.
Referring to fig. 1, an embodiment of the present invention provides a system for removing volatile components from a high viscosity polymer, including: a first volatilizer 50, a second volatilizer 80 and a heat exchanger corresponding to each volatilizer,
as shown in fig. 2, the first volatilizer 50 comprises: a first separation chamber 501, a first solution inlet 502, a first solution outlet 503, and a first gas outlet 504;
as shown in fig. 6, the second volatilizer 80 comprises: a second separation chamber 801, a second solution inlet 802, a second solution outlet 803 and a second gas outlet 804;
in order to allow the supercritical state volatile components in the high viscosity polymer solution entering the first volatilizer 50 to be separated well, as shown in fig. 2, the first volatilizer 50 may further comprise: a distributor 505, wherein a plurality of first distribution holes 506 are arranged on a separating surface of the distributor 505; the distributor 505 is located in the first separation chamber 501 and connected to the lower end of the first solution inlet 502 so that the high-viscosity polymer solution introduced from the first solution inlet 502 is brought into contact with the separation surface of the distributor 505.
Specifically, the high-viscosity polymer solution entering the first volatilizer 50 includes a polymer melt and a supercritical state volatile component, which may be referred to as a mixture, and the volatile component in the mixture includes unreacted polymer monomer, solvent, catalyst, and the like.
Specifically, the distributor 505 may be connected to the lower end of the first solution inlet 502 by means of welding. Of course, the distributor 505 may be fixed in the first separation chamber 501 by other means and connected to the lower end of the first solution inlet 502 by welding. Preferably, after the distributor 505 is connected to the lower end of the first solution inlet 502, the separation plane of the distributor 505 may be perpendicular to the axis of the first separation chamber 501.
Specifically, the separation surface of the distributor 505 is a portion of the distributor 505, which is provided with first distribution holes 506 and is in contact with the high-viscosity polymer solution entering from the first solution inlet 502; the first distribution holes 506 may be circular in shape. The distributor 505 provided by the invention has a simple structure, is easy to install and maintain, and thus, the structure of the whole volatilization subsystem is also simple.
Specifically, in the process that the high-viscosity polymer solution entering the first volatilizer 50 contacts and stays at the separation surface of the distributor 505, the supercritical state volatile components in the high-viscosity polymer solution can be sufficiently volatilized and flow upward to be discharged out of the first volatilizer 50 from the first gas outlet 504 and be recovered by the recovery device; the polymer melt in the high viscosity polymer solution falls through the first distribution holes 506 of the distributor 505 and is precipitated at the bottom of the first volatilizer 50 and is passed through the first solution outlet 503 to the heat exchanger corresponding to the second volatilizer 80, thereby achieving the purpose of removing the volatile components in the high viscosity polymer solution.
Specifically, in order to ensure good fluidity of the high-viscosity polymer solution entering the first volatilizer 50 from the first solution inlet 502, the temperature of the high-viscosity polymer solution entering the first volatilizer 50 from the first solution inlet 502 is preferably between 170 ℃ and 280 ℃.
Since the high-viscosity polymer solution entering from the first solution inlet 502 is continuously decreased in temperature and pressure while flowing from the end near the first solution inlet 502 to the end far from the first solution inlet 502, the fluidity is gradually deteriorated. Thus, if the diameter of the first distribution holes 506 at the end of the distributor 505 close to the first solution inlet 502 is too large, on the one hand, the high-viscosity polymer solution is not favorably flowed toward the end far from the first solution inlet 502, thereby affecting the contact area of the high-viscosity polymer solution with the separation surface of the distributor 505 and affecting the effect of removing volatile components; on the other hand, the supercritical volatile components in the high-viscosity polymer solution on the separation surface at the position are not separated in time, and fall to the bottom of the first volatilizer 50, further affecting the effect of removing the volatile components; if the diameter of the first distribution holes 506 at the end of the distributor 505 remote from the first solution inlet 502 is too small, the polymer melt on the separation surface at this position, from which the volatile components have been removed, is not favorably settled toward the bottom of the first volatilizer 50, and in the serious case, the first distribution holes may be clogged, thereby affecting the effect of removing the volatile components. Therefore, preferably, as shown in fig. 3, the pore diameter of a distribution hole which is closer to the first solution inlet 502 among the plurality of first distribution holes 506 which are opened on the separation surface of the distributor 505 may be made smaller than the pore diameter of a distribution hole which is farther from the first solution inlet 502;
since, preferably, the first distribution holes 506 at the end of the distributor 505 near the first solution inlet 502 have a smaller pore size, therefore, in order to ensure the effect of the sedimentation of the polymer melt, from which the volatile components have been removed, on the separation surface at this position toward the bottom of the first volatilizer 50, it is further preferable that the density of the distribution holes, which are positioned closer to the first solution inlet 502 among the plurality of first distribution holes 506 opened on the separation surface of the distributor 505, is made greater than the density of the distribution holes which are positioned farther from the first solution inlet 502, thus, the densely distributed pores near the first solution inlet 502 can increase the contact area between the high-viscosity polymer solution and the separation surface of the distributor 505, and the pressure of the high-viscosity polymer solution near the first solution inlet 502 is not reduced, thereby ensuring that the high-viscosity polymer solution smoothly reaches the farthest end of the distributor 505; in addition, the relatively sparsely distributed macropores away from the first solution inlet 502 can prevent the high-viscosity polymer solution from flowing back from the end away from the first solution inlet 502 to the end close to the first solution inlet 502, which affects the distribution efficiency, thereby obtaining a better volatile component removal effect.
Specifically, the arrangement of the plurality of first distribution holes 506 in the distributor 505 may include the following two ways:
first, as shown in fig. 3, a plurality of first distribution holes 506 in the distributor 505 may be arranged in parallel in each distribution row, the distribution rows being perpendicular to the axis of the first solution inlet 502, the pitch of the distribution rows increasing with increasing distance from the first solution inlet 502, wherein the first distribution holes 506 in the distribution row that is closer to the first solution inlet 502 have a smaller hole diameter than the first distribution holes 506 in the distribution row that is farther from the first solution inlet 502; the density of the first distribution holes 506 in the distribution row located closer to the first solution inlet 502 is greater than the density of the first distribution holes 506 in the distribution row located farther from the first solution inlet 502.
Second, as shown in fig. 4, the plurality of first distribution holes 506 in the distributor 505 may be arranged in parallel in each distribution row, the distribution rows are parallel to the axis of the first solution inlet 502, and the distribution rows may be equal or different in pitch, wherein, in the same distribution row: the pore size of the first distribution holes 506 near the first solution inlet 502 is smaller than the pore size of the first distribution holes 506 far from the first solution inlet 502; the density of the first distribution holes 506, which are closer to the first solution inlet 502, is greater than the density of the first distribution holes 506, which are farther from the first solution inlet 502.
Preferably, the parting plane of the distributor 505 may be circular. Further, in order to prevent the high-viscosity polymer solution entering the first volatilizer 50 from the first solution inlet 502 from being accumulated on the separation surface of the distributor 505 when the flow rate is too large, the outer diameter of the distributor 505 may be smaller than the inner diameter of the first separation chamber 501, so that the high-viscosity polymer solution exceeding the separation capability of the separation surface of the distributor 505 is settled to the bottom of the first volatilizer 50 through the gap between the distributor 505 and the first separation chamber.
As shown in fig. 5, in order to further enhance the effect of the first volatilizer 50 in volatilizing, on the basis of fig. 2, the first volatilizer 50 may further comprise: the distribution sieve 507 is arranged on the top of the sieve,
specifically, the distribution screen 507 is also located in the first separation chamber 501 and fixed at any position below the distributor 505 and above the liquid level of the high-viscosity polymer solution, and a plurality of second distribution holes 508 are formed in the distribution screen 507.
Specifically, the second distribution holes 508 may be round holes, and preferably, may be tapered holes.
Preferably, the distribution screen 507 may be circular and the outer diameter of the distribution screen 507 is equal to the inner diameter of the first separation chamber 501.
In particular, the distribution screen 507 may be permanently fixed to the inner wall of the first separation chamber 501 by welding, or may be detachably fixed to the inner wall of the first separation chamber 501 by hinging or bolting.
Thus, the high-viscosity polymer solution separated by the distributor 505 can contact and stay on the distribution screen 507, and the residual supercritical volatile components in the high-viscosity polymer solution can be further separated in the stay process, so that the content of the volatile components in the high-viscosity polymer solution can be further effectively reduced.
Since the viscosity of the high-viscosity polymer solution obtained from the first solution outlet 503 of the first volatilizer 50 is very high, it is necessary to heat it again in a heat exchanger corresponding to the second volatilizer 80 in order to obtain a better fluidity when it is fed to the second volatilizer 80 for the second separation. This requires a heat exchanger corresponding to the second volatilizer 80 to have a high heating precision, which if the heating temperature is too high, may cause secondary reactions of the polymer, such as thermal degradation of the polymer chains; if the heating temperature is too low, the fluidity requirement cannot be met. And even if the high-viscosity polymer solution is heated in the heat exchanger corresponding to the second volatilizer 80 to obtain an appropriate temperature, the pipe from the heat exchanger corresponding to the second volatilizer 80 cannot be too long, otherwise, the temperature of the high-viscosity polymer solution is also reduced in the process of flowing into the second volatilizer 80 from the heat exchanger corresponding to the second volatilizer 80, which makes the fluidity of the high-viscosity polymer solution entering the second volatilizer 80 still not ideal, which is not favorable for the removal of the supercritical state volatile components in the high-viscosity polymer solution.
Therefore, it is preferable that another system for removing volatile components from a high viscosity polymer is provided in the embodiment of the present invention, as shown in fig. 6, wherein the second solution inlet 802 of the second volatilizer 80 is located at the top of the second volatilizer 80 and is connected to the outlet of the heat exchanger corresponding to the second volatilizer 80.
Specifically, the heat exchanger corresponding to the second volatilizer 80 may be a multi-tube heat exchanger which is connected to the second solution inlet 802. Therefore, on one hand, the high-viscosity polymer solution entering the second volatilizer 80 can have a proper temperature, so that the flowability of the high-viscosity polymer solution is ensured, and the multi-tube heat exchanger corresponding to the second volatilizer 80 can also play a role of a distributor, so that the supercritical state volatile component of the high-viscosity polymer solution entering the second volatilizer 80 can be smoothly separated from the polymer melt, and a good volatile component removing effect is achieved; on the other hand, the requirement for heating accuracy of the heat exchanger corresponding to the second volatilizer 80 and the limitation of the length of the piping are reduced.
Further, in order to ensure good fluidity of the high-viscosity polymer solution entering the second volatilizer 80 from the second solution inlet 802, the temperature of the high-viscosity polymer solution entering the second volatilizer 80 from the second solution inlet 802 is preferably between 170 ℃ and 280 ℃.
The system for removing the volatile components in the high-viscosity polymer provided by the embodiment of the invention comprises: a first volatilizer 50, a second volatilizer 80 and a heat exchanger corresponding to each volatilizer, said first volatilizer 50 comprises: a first separation chamber 501, a first solution inlet 502, a first solution outlet 503 and a first gas outlet 504, and the second volatilizer 80 comprises: a second separation chamber 801, a second solution inlet 802, a second solution outlet 803 and a second gas outlet 804, wherein the first volatilizer 50 further comprises: a distributor 505, wherein a plurality of first distribution holes 506 are arranged on a separating surface of the distributor 505; the distributor 505 is located in the first separation chamber 501 and connected to the lower end of the first solution inlet 502 so that the high-viscosity polymer solution introduced from the first solution inlet 502 is brought into contact with the separation surface of the distributor 505. Because the first volatilizer 50 is provided with the distributor 505 which has a simple structure and is provided with the first distribution holes 506, the system for removing the volatile components in the high-viscosity polymer provided by the embodiment of the invention has a simple structure, is easy to install and maintain, can effectively reduce the content of the volatile components in the high-viscosity polymer, and obtains a polymer finished product with higher purity.
As shown in fig. 7, the present invention also provides a method for removing volatile components from a polymer by using the system for removing volatile components from a high-viscosity polymer according to an embodiment of the present invention, which may include the following steps:
s101, heating a high-viscosity polymer solution in a heat exchanger corresponding to the first volatilizer 50 to obtain a first mixture comprising a polymer melt and a supercritical volatile component;
specifically, the high-viscosity polymer solution is heated in a heat exchanger corresponding to the first volatilizer 50, and the temperature of the obtained first mixture is between 170 ℃ and 280 ℃.
S102, making the first mixture enter the first separation cavity 501 of the first volatilizer 50 from the first solution inlet 502 and contact with the separation surface of the distributor 505 in the first separation cavity 501; a plurality of first distribution holes 506 are formed in the separation surface of the distributor 505, and the distributor 505 is connected with the lower end of the first solution inlet 502; the pressure of the first mixture entering the first separation chamber 501 from the first solution inlet 502 is greater than the pressure in the first separation chamber 501;
specifically, the distributor 505 may be connected to the lower end of the first solution inlet 502 by means of welding. Of course, the distributor 505 may be fixed in the first separation chamber by other means and connected to the lower end of the first solution inlet 502 by welding. Preferably, the separation plane connecting the rear distributor 505 may be perpendicular to the axis of the first separation chamber 501;
specifically, in order to ensure that the high-viscosity polymer solution entering the first volatilizer 50 from the first solution inlet 502 has a good fluidity, the temperature of the high-viscosity polymer solution entering the first volatilizer 50 from the first solution inlet 502 is preferably between 170 ℃ and 280 ℃;
specifically, the shape of the distributor 505, the shape and size of the first distribution holes 506, and the distribution of the first distribution holes 506 on the separation surface of the distributor 505 may be the same as those in the embodiments shown in fig. 3 and 4 of the present invention, and are not described herein again;
specifically, the pressure of the first mixture entering the first separation chamber 501 from the first solution inlet 502 may be 8 to 10Pa, and the pressure in the first separation chamber 501 may be 2 to 4 Pa.
S103, performing first separation on the supercritical volatile component in the first mixture and the polymer melt on the separation surface of the distributor 505 to obtain a second mixture, wherein the supercritical volatile component in the first mixture is discharged through a first gas outlet 504 and recovered;
specifically, the second mixture comprises a polymer melt and residual supercritical volatile components;
specifically, during the contact of the high-viscosity polymer solution entering the first volatilizer 50 with the separating surface of the distributor 505, the supercritical state volatile components in the high-viscosity polymer solution are flashed and flow upward to be discharged from the first volatilizer 50 through the first gas outlet 504 and recovered by the recovery device.
Specifically, since the pressure of the first mixture entering the first separation chamber 501 from the first solution inlet 502 is greater than the pressure in the first separation chamber 501; thus, the first mixture entering the first separation chamber 501 from the first solution inlet 502 is almost sprayed on the separation surface of the distributor 505, so that the first mixture is rapidly contacted with the separation surface of the distributor 505, thereby rapidly separating the volatile components in the first mixture from the polymer melt.
Preferably, after the first separation of the supercritical volatile component from the polymer melt in the first mixture on the separation surface of the distributor 505 to obtain a second mixture, and before the second mixture is heated in the heat exchanger corresponding to the second volatilizer 80; the method may further comprise:
the second mixture is contacted with the upper surface of a distribution screen 507 arranged below the distributor 505 in the first separation chamber 501, and a plurality of second distribution holes 508 are arranged on the distribution screen 507. During the contact of the second mixture with the upper surface of the distribution screen 507, the residual volatile components in the supercritical state in the second mixture can be further removed, so that the content of the volatile components in the second mixture obtained from the first solution outlet 503 of the first volatilizer 50 is further reduced.
Specifically, the distribution screen 507 is also located in the first separation chamber 501 and fixed at any position below the distributor 505 and above the liquid level of the high-viscosity polymer solution, and a plurality of second distribution holes 508 are formed in the distribution screen 507.
Specifically, the second distribution holes 508 may be circular or conical.
Preferably, the distribution screen 507 may be circular and the outer diameter of the distribution screen 507 is equal to the inner diameter of the first separation chamber 501.
In particular, the distribution screen 507 may be permanently fixed to the inner wall of the first separation chamber 501 by welding, or may be detachably fixed to the inner wall of the first separation chamber 501 by hinging or bolting.
And S104, heating the second mixture in a heat exchanger corresponding to the second volatilizer 80, and enabling the heated second mixture to enter the second volatilizer 80 to perform second separation on the volatile matter and the polymer melt in the second mixture.
Specifically, since the second mixture is cooled during the process of flowing into the second volatilizer 80 along the pipeline connecting the first volatilizer 50 and the second volatilizer 80, the second mixture is heated in the heat exchanger corresponding to the second volatilizer 80 before entering the second volatilizer 80, so as to obtain the second mixture consisting of the polymer melt and the supercritical state volatile component with better fluidity; if the heating temperature is too high, secondary reactions of the polymer, such as thermal degradation of the polymer chains, may result; if the heating temperature is too low, the fluidity requirement cannot be met. Therefore, it is preferable that the temperature of the second mixture entering the second volatilizer 80 through the second solution inlet 802 is between 170 ℃ and 280 ℃;
in addition, even if the second mixture is heated in the heat exchanger corresponding to the second volatilizer 80 to obtain an appropriate temperature, the piping from the heat exchanger corresponding to the second volatilizer 80 cannot be too long, otherwise, the second mixture is reduced in the process of flowing into the second volatilizer 80 from the heat exchanger corresponding to the second volatilizer 80, which makes the fluidity of the second mixture entering the second volatilizer 80 still not ideal, which is not favorable for the removal of the supercritical state volatile components in the second mixture.
Therefore, it is preferable that the passing of the heated second mixture into the second volatilizer 80 includes:
passing the heated second mixture from the second solution inlet 802 into the second volatilizer 80; wherein, the second solution inlet 802 is located at the top of the second volatilizer 80, and the heat exchanger corresponding to the second volatilizer is connected with the second solution inlet 802.
Specifically, the heat exchanger corresponding to the second volatilizer 80 may be a multi-tube heat exchanger which is connected to the second solution inlet 802. Therefore, on one hand, the second mixture entering the second volatilizer 80 can be ensured to have proper temperature so as to have better fluidity, and the multi-tube heat exchanger corresponding to the second volatilizer 80 can also play the role of a distributor so as to ensure that the supercritical state volatile component in the second mixture entering the second volatilizer 80 can be smoothly separated from the polymer melt, thereby achieving good volatile component removing effect; on the other hand, the requirement for heating accuracy of the heat exchanger corresponding to the second volatilizer 80 and the limitation of the length of the piping are reduced. In addition, because the connection of the multiple outlets of the multi-tube heat exchanger and the second solution inlet 802 can play the role of a distributor, the second volatilizer 80 provided by the application can save the cost of installing the distributor in the second volatilizer 80, and the production cost can be saved.
One specific example of removing volatiles from polybutene using a method for removing volatiles from high viscosity polymer according to the present invention is described below with reference to fig. 1, in which a first volatilizer 50 comprises: the device comprises a distributor 505 and a distribution screen 507 positioned below the distributor, wherein the distributor 505 is provided with a plurality of first distribution holes 506, and the distribution screen 507 is provided with a plurality of conical second distribution holes 508; the second volatilizer 80 in the system comprises: a second solution inlet 802, the second solution inlet 802 being located at the top of the second volatilizer 80 and being connected to a plurality of outlets of the multi-tube heat exchanger corresponding to the second volatilizer 80, in particular,
obtaining a first mixture comprising a polybutene melt and butene-1 in a supercritical state at a temperature of 190 ℃ and a pressure of 9Pa at the outlet of a heat exchanger corresponding to the first volatilizer 50;
the first mixture enters the first separation chamber 501 of the first volatilizer 50 from the first solution inlet 502 of the first volatilizer 50; when the mixture enters, the temperature of the first mixture is 188 ℃, the pressure is 8Pa, and the pressure in the first separation cavity 501 is 4 Pa; upon entry, the first mixture is in substantial contact with the separation surface of the distributor 505;
under the action of gravity, the supercritical butene-1 in the first mixture on the separation surface of the distributor 505 is subjected to a first separation from the polymer melt to obtain a second mixture; after separation, gaseous butene-1 in supercritical state flows upward to be recovered through the first gas outlet 504; the second mixture is poured through the first distribution holes 506 and falls to the upper surface of the distribution screen 507; the residual gaseous butene-1 in the second mixture is further separated on the upper surface of the distribution screen 507, and likewise, the gaseous butene-1 in a supercritical state obtained after the further separation flows upward to be recovered through the first gas outlet 504, and the second mixture obtained after the further separation falls through the second distribution holes 508 and is precipitated to the bottom of the first volatilizer 50; the content of butene-1 in the second mixture obtained from the first solution outlet 503 was 5%;
the second mixture is conveyed to a multi-tube heat exchanger corresponding to the second volatilizer 80 to be heated, when the second mixture is heated to 205 ℃, the second mixture is poured into the second volatilizer 80 through a plurality of second solution inlets 802 to carry out second separation on the butene-1 and the polybutene in the second mixture, and finally, a polybutene melt with the butene-1 content of less than 50PPM is obtained from a second solution outlet 803 of the second volatilizer 80.
Therefore, the method for removing the volatile components in the high-viscosity polymer can effectively reduce the content of the butene-1 in the finished polybutene and ensure the use safety of the polybutene product.
According to the method for removing volatile components from a high-viscosity polymer provided by the embodiment of the invention, a first mixture can be in contact with a separation surface of a distributor 505 in a first separation chamber 501 in a first volatilizer 50, wherein the distributor 505 is connected with the lower end of a first solution inlet 502, a plurality of first distribution holes 506 are formed in the separation surface of the distributor 505, and the pressure of the first mixture entering the first separation chamber 501 from the first solution inlet 502 is greater than the pressure in the first separation chamber 501; subjecting the supercritical volatile component in the first mixture on the separation surface of the distributor 505 to a first separation with the polymer melt to obtain a second mixture, wherein the supercritical volatile component in the first mixture is discharged through a first gas outlet 504 and recovered; the second mixture is heated in a heat exchanger corresponding to the second volatilizer 80 and the heated second mixture is passed to the second volatilizer 80 for a second separation of the volatile components of the second mixture from the polymer melt. Because the first volatilizer 50 is provided with the distributor 505 with the first distribution holes 506 and the good separation effect, the method for removing the volatile components in the high-viscosity polymer provided by the embodiment of the invention can effectively reduce the content of the volatile components in the high-viscosity polymer and obtain the polymer with high purity.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
All the embodiments in the present specification are described in a related manner, and the same and similar parts among the embodiments may be referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, as for the apparatus embodiment, since it is substantially similar to the method embodiment, the description is relatively simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A system for devolatilizing a high viscosity polymer comprising: a first volatilizer (50), a second volatilizer (80) and a heat exchanger corresponding to each volatilizer, the first volatilizer (50) comprising: a first separation chamber (501), a first solution inlet (502), a first solution outlet (503), and a first gas outlet (504), the second volatilizer (80) comprising: a second separation chamber (801), a second solution inlet (802), a second solution outlet (803), and a second gas outlet (804), characterized in that:
the first evaporator (50) further comprises: the distributor (505) is provided with a plurality of first distribution holes (506) on a separating surface of the distributor (505); the aperture of a distribution hole which is close to the first solution inlet (502) in a plurality of first distribution holes (506) which are opened on the separation surface of the distributor (505) is smaller than the aperture of a distribution hole which is far from the first solution inlet (502); the density of distribution holes in the plurality of first distribution holes (506) opened on the separation surface of the distributor (505) which are close to the first solution inlet (502) is greater than the density of distribution holes which are far from the first solution inlet (502);
the distributor (505) is located in the first separation chamber (501) and connected to the lower end of the first solution inlet (502) so that the high-viscosity polymer solution entering from the first solution inlet (502) is brought into contact with the separation surface of the distributor (505);
the separating surface of the distributor (505) is vertical to the axis of the first separating cavity (501);
the second solution inlet (802) is positioned at the top of the second volatilizer (80) and is directly connected with the outlet of the heat exchanger corresponding to the second volatilizer (80).
2. The system according to claim 1, wherein the separation surface of the distributor (505) is circular and the outer diameter of the distributor (505) is smaller than the inner diameter of the first separation chamber (501).
3. The system according to claim 2, wherein a plurality of first distribution holes (506) in the distributor (505) are arranged in parallel in each distribution row, the distribution rows being perpendicular to the axis of the first solution inlet (502), wherein the first distribution holes (506) in a distribution row that is closer to the first solution inlet (502) have a smaller aperture than the first distribution holes (506) in a distribution row that is further from the first solution inlet (502); the density of the first distribution holes (506) in the distribution row that is closer to the first solution inlet (502) is greater than the density of the first distribution holes (506) in the distribution row that is farther from the first solution inlet (502).
4. The system according to any one of claims 1 to 3, wherein the first volatilizer (50) further comprises: a distribution screen (507);
the distribution sieve (507) is positioned in the first separation cavity (501) and fixed below the distributor (505), and a plurality of second distribution holes (508) are formed in the distribution sieve (507).
5. A system according to claim 4, characterized in that the distribution screen (507) is circular, the outer diameter of the distribution screen (507) being equal to the inner diameter of the first separation chamber (501).
6. A method for removing volatile components from a high viscosity polymer, based on the system for removing volatile components from a high viscosity polymer according to any one of claims 1 to 5, comprising:
heating the high viscosity polymer solution in a heat exchanger corresponding to the first volatilizer (50) to obtain a first mixture comprising a polymer melt and volatiles in a supercritical state;
-passing said first mixture from the first solution inlet (502) into the first separation chamber (501) of the first volatilizer (50) and in contact with the separation surface of the distributor (505) in the first separation chamber (501); wherein, a plurality of first distribution holes (506) are arranged on the separation surface of the distributor (505), the distributor (505) is connected with the lower end of the first solution inlet (502), and the pressure of the first mixture entering the first separation cavity (501) from the first solution inlet (502) is higher than the pressure in the first separation cavity (501);
the supercritical volatile components in the first mixture on the separation surface of the distributor (505) are subjected to first separation with the polymer melt to obtain a second mixture, wherein the supercritical volatile components in the first mixture are discharged through a first gas outlet (504) and recovered;
heating the second mixture in a heat exchanger corresponding to a second volatilizer (80), and leading the heated second mixture to enter the second volatilizer (80) to carry out secondary separation on the volatile components in the second mixture and the polymer melt.
7. The method according to claim 6, wherein the temperature of the first mixture entering the first volatilizer (50) from the first solution inlet (502) is between 170 ℃ and 280 ℃.
8. The method according to claim 6, characterized in that after the first separation of the supercritical volatile substance from the polymer melt in the first mixture on the separation surface of the distributor (505) to obtain a second mixture, and before the heating of the second mixture in a heat exchanger corresponding to a second volatilizer (80); the method further comprises the following steps:
and enabling the second mixture to be in contact with the upper surface of a distribution sieve (507) fixed below the distributor (505) in the first separation cavity (501), wherein a plurality of second distribution holes (508) are formed in the distribution sieve (507).
9. The method according to any one of claims 6-8, wherein said passing the heated second mixture into a second volatilizer (80) comprises:
passing the heated second mixture from the second solution inlet (802) into a second volatilizer (80); wherein, the second solution inlet (802) is positioned at the top of the second volatilizer (80) and is directly connected with the outlet of the heat exchanger corresponding to the second volatilizer (80).
10. The method according to claim 9, wherein the temperature of the second mixture entering the second volatilizer (80) through the second solution inlet (802) is between 170 ℃ and 280 ℃.
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| CN1662561A (en) * | 2002-06-24 | 2005-08-31 | 巴塞尔聚烯烃意大利有限公司 | Method for removing volatile components from polymer compositions |
| CN101213247A (en) * | 2005-05-11 | 2008-07-02 | 巴塞尔聚烯烃意大利有限责任公司 | Polymerization process for preparing polyolefin blends |
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| CN1662561A (en) * | 2002-06-24 | 2005-08-31 | 巴塞尔聚烯烃意大利有限公司 | Method for removing volatile components from polymer compositions |
| CN101213247A (en) * | 2005-05-11 | 2008-07-02 | 巴塞尔聚烯烃意大利有限责任公司 | Polymerization process for preparing polyolefin blends |
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