CN115572337A - Polymer solution devolatilization method and equipment - Google Patents
Polymer solution devolatilization method and equipment Download PDFInfo
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- CN115572337A CN115572337A CN202211045837.9A CN202211045837A CN115572337A CN 115572337 A CN115572337 A CN 115572337A CN 202211045837 A CN202211045837 A CN 202211045837A CN 115572337 A CN115572337 A CN 115572337A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/06—Treatment of polymer solutions
- C08F6/10—Removal of volatile materials, e.g. solvents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/008—Liquid distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/343—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances the substance being a gas
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- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a polymer solution devolatilization method and equipment. Adding a polymer solution containing volatile components from the upper part of the container, flowing downwards along the outer surface of the hollow inner member to form a liquid film, collecting at the bottom of the container to form a solution pool, and discharging through a liquid discharge port at the bottom of the container; and (3) discharging volatile components in the polymer solution after escaping from a vent port in the upper part of the container, introducing a first airflow into a closed space formed by the outer surface of the hollow inner member and the inner surface of the container, introducing a second flow strand into the hollow inner member, and discharging the first airflow from the vent port in the upper part of the container after the first airflow is in countercurrent contact with the polymer solution. The invention can be used for the production process of materials such as rubber, polyolefin elastomer and the like, and has the advantages of simple equipment structure, large treatment capacity, good devolatilization effect, low energy consumption and the like.
Description
Technical Field
The invention relates to a method and equipment for devolatilizing a polymer solution, in particular to a method and equipment for devolatilizing a polymer solution.
Background
Devolatilization is a link in chemical production, is only secondary to the reaction process, and mainly has the function of transferring volatile substances in the polymer from a liquid phase to a gas phase or removing a solvent. The energy consumption of the devolatilization process often accounts for more than 60% of the overall energy consumption of the production process. With the continuous improvement of safety, environmental protection and health level, the requirements of different application fields on the content of volatile substances in polymer materials are higher and higher, and the content of specific volatile components in polymer products in certain special fields is required to be lower than 1mg/kg, so that the research and optimization of polymer devolatilization processes and equipment and the realization of low-energy-consumption and high-efficiency polymer devolatilization processes are of great significance.
The devolatilization process is generally divided into three stages: the first stage is a flash evaporation process, and 60 to 80 percent of volatile components can be removed; the second stage is bubbling devolatilization, which requires operating pressure to be reduced below the equilibrium partial pressure of solute and introducing inert gas or water vapor, and the first stage can remove 10-20% of volatile components; the third stage is diffusion devolatilization, which can reduce the volatile components in the polymer to the required ppm level.
The reason for the separation between the polymer and the volatile components during degassing or devolatilization is the difference in volatility between these species. The difference in chemical potentials in the polymer and gas phases is the driving force for devolatilization. This difference in chemical potential causes a concentration gradient at the polymer interface, resulting in diffusion from the polymer into the gas phase.
Devolatilization equipment is diversified, but can be roughly divided into static devolatilization equipment and dynamic devolatilization equipment, and the aim of the devolatilization equipment is to remove volatile components in the polymer more quickly and completely. The static devolatilization equipment mainly utilizes the geometrical configuration of internal members to increase the surface area of the polymer, and the high specific surface area is more favorable for removing volatile components. In addition, the static devolatilization apparatus is advantageous in that it has no moving parts, and its wear and maintenance costs are low. Dynamic devolatilization equipment, such as an extruder, whose rotating parts are used to provide surface renewal, evaporative cooling, and efficient mixing to allow for optimal heat and mass transfer, can significantly increase the surface renewal rate of the polymer by virtue of its moving parts. However, it has the disadvantages of high cost, complex mechanical structure, high energy consumption, high leakage rate, high maintenance cost, etc.
For static devolatilization equipment, the residence time of the polymer in the equipment may be increased in order to obtain a high quality product with lower residual volatile content. However, an increase in residence time may lead to degradation of some heat-sensitive polymer solutions, which is clearly disadvantageous, and the polymer in some static devolatilization devices has a residence time that is mostly in the liquid distributor, where only a small portion of the surface of the polymer solution is exposed to a vacuum or reduced pressure environment, and efficient devolatilization cannot be performed.
In static devolatilization equipment, the devolatilization environment is typically an inert gas or steam. In the devolatilization process, the polymer and the purge gas continuously carry out mass transfer and heat transfer, wherein, high-temperature decompression is favorable for the devolatilization process, but the gasification of volatile components or solvents in the polymer can absorb a large amount of heat, so that the temperature of the purge gas is reduced, and the devolatilization effect is further weakened, thus the problem to be solved is how to carry out effective devolatilization in the environment of keeping higher temperature.
A static devolatilization apparatus is disclosed in US 2007/0137488 A1. A disadvantage of this known static devolatilization apparatus is that a large part of the residence time of the polymer takes place in the distributor, after moving through the perforated plate and dispersing there, the polymer then flows directly into the discharge pump and is directly evacuated. Thus, the residence time of the dispersed polymer in the devolatilization vessel is generally very limited, typically in the range of seconds for less viscous liquids, poor heat transfer during devolatilization, and small specific surface area, limited mass transfer effects. As a result, the devolatilization is often insufficient to provide a high quality product with a low volatile concentration.
A static devolatilization apparatus is disclosed in CN 110746524A. The multiple liquid distribution subunits arranged in the devolatilization environment of the equipment optimize the residence time distribution problem of the scheme, so that the liquid has longer devolatilization time in the equipment, but the heat transfer problem is still not solved.
A static devolatilization apparatus is disclosed in US 005453158A. The polymer solution is heated in a heating flat plate before entering a decompression area for devolatilization. The heating is still preheating, and no heat source is supplied in the devolatilization process.
When the volatilization is removed, the polymer solution is heated by evaporation, so that the temperature of the polymer solution is reduced, and the volatilization effect is reduced. In the above-mentioned patent equipment, the heat transfer effect is limited when the polymer devolatilization process is carried out, firstly, no extra heat source is provided for supplying heat in the devolatilization process, and secondly, no surface capable of exchanging heat in the devolatilization process is provided for the equipment.
In view of the foregoing, there is a need for a static devolatilization apparatus that allows for a larger specific surface area and longer residence time for devolatilization of dispersed polymer solutions, and that ensures both good mass transfer and heat transfer during the devolatilization process.
Disclosure of Invention
The object of the present invention is to provide a method and an apparatus for devolatilizing a polymer solution comprising volatile components, which method do not have the drawbacks of the prior art, in particular the reduced heat transfer effect caused by the reduced temperature during devolatilization. Further objects of the invention include providing a method for using the apparatus in devolatilization of viscous liquids comprising volatile components, and the use of the apparatus in devolatilization of polymer solutions comprising volatile components, preferably polymer melts or solutions.
The polymer solution devolatilization method comprises the following steps: in a container with a hollow inner member, adding a polymer solution containing volatile components from the upper part of the container, flowing downwards along the outer surface of the hollow inner member to form a liquid film, converging at the bottom of the container to form a solution pool, and discharging through a liquid outlet at the bottom of the container; volatile components in the polymer solution are discharged from an air outlet at the upper part of the container after escaping, a first air flow is introduced into a closed space formed by the outer surface of the hollow inner member and the inner surface of the container, and the devolatilization effect of the polymer solution is enhanced by strengthening mass transfer; introducing a second stream into the hollow inner member for heating the formed liquid film; the first gas stream is discharged from a vent in the upper portion of the vessel after counter-current contact with the polymer solution.
According to a preferred embodiment of the invention, the first gas stream is one or a mixture of several of the aforementioned gases nitrogen, carbon dioxide, water vapour.
According to a preferred embodiment of the present invention, the second stream is water vapor, water, silicone oil or heat conducting oil, and the high temperature oil heat transfer includes but is not limited to glycerin, paraffin oil, methyl silicone oil or some vegetable oils; the second stream is preferably water vapor.
According to a preferred embodiment of the invention, neither the first stream nor the second stream has a temperature lower than the temperature of the polymer solution.
According to a preferred embodiment of the invention, the ratio of the flow rates of the first gas stream and the second stream is 1.
According to a preferred embodiment of the invention, the residence time of the polymer solution in the vessel does not exceed 20 minutes.
According to a preferred embodiment of the invention, there are at least 2 of said hollow internals in said vessel.
According to a preferred embodiment of the present invention, the hollow inner member may be a circular tube, a square tube, a polygonal tube, a corrugated tube, or a straight tube with a spiral groove.
According to a preferred embodiment of the present invention, the hollow inner member may be a corrugated tube or a combination of a straight tube with a spiral groove and a round tube, wherein the upper section is the corrugated tube or the straight tube with the spiral groove, the lower section is the round tube, and the ratio of the length of the upper section to the length of the lower section is 1.
According to a preferred embodiment of the present invention, the polymer solution flows in a membrane on the outer surface of the hollow inner member with a reynolds number of not higher than 2000. Preferably, the residence time of the polymer solution in the membrane flowing on the outer surface of the hollow inner member is not less than 1 minute.
According to a preferred embodiment of the invention, a polymer solution distributor is arranged in the upper part of the vessel and a second strand distributor is arranged in the lower part of the vessel.
According to a preferred embodiment of the invention, the second flow distributor is located in the solution tank.
The second stream enters from the bottom of the vessel, flows counter-currently to the polymer solution, and exits from the top of the vessel.
When the second stream is a gas stream (e.g., water vapor), the second stream is introduced from the bottom of the container, one part of the second stream is introduced into the interior of the hollow inner member as the second stream, and the other part of the second stream is introduced into the closed space formed by the outer surface of the hollow inner member and the inner surface of the container as the first gas stream alone or as part of the first gas stream.
The present invention provides a devolatilization apparatus comprising:
a tank for receiving the polymer solution,
a polymer solution inlet for introducing a polymer solution into the tank;
a polymer solution outlet for leading the polymer solution with the volatile components removed out of the tank body;
a first gas flow inlet for introducing a first gas flow into the tank;
the first air flow outlet is used for leading the first air flow and the volatile component mixed gas out of the tank body;
the upper end socket comprises a second flow outlet for discharging a second flow, and the lower end socket comprises a second flow inlet for allowing the second flow to enter;
an upper baffle for separating the upper head from the tank, wherein the upper baffle is located in an upper region of the tank and above the polymer solution inlet;
a lower baffle for separating the lower head from the tank, wherein the lower baffle is located in a lower region of the tank and below the first gas inlet;
and the hollow internal components are uniformly and orderly arranged in the tank body, penetrate through the upper partition plate and the lower partition plate and extend into the upper end enclosure and the lower end enclosure.
Further, the apparatus is provided with a liquid distributor and a first gas flow distributor, the liquid distributor is positioned in the tank and is positioned below the polymer solution inlet and above the first gas flow outlet, the liquid distributor is a partition plate, wherein the liquid distributor is provided with openings with the same number as the tubes, and each opening is arranged in a concentric circle with the respective tube, and the diameter of the opening is larger than that of the tube, so that a gap is formed; the first air flow distributor is a partition plate, the tubes pass through the first air flow distributor without gaps, the first air flow distributor is provided with holes between the tubes and at the periphery of the tubes and is upwards connected with an air outlet pipe, and the height of the air outlet pipe exceeds the height of the liquid outlet pipeline.
The invention also provides a devolatilization apparatus, the second stream being a gas stream, the apparatus comprising:
a tank for receiving the polymer solution,
a polymer solution inlet for introducing a polymer solution into the tank;
a polymer solution outlet for leading the polymer solution with the volatile components removed out of the tank body;
the upper end socket and the lower end socket are used for being connected with the tank body, the upper end socket comprises a second flow outlet for discharging a second flow, and the lower end socket comprises an airflow inlet;
the first air flow outlet is used for leading the first air flow and the volatile component mixed gas out of the tank body;
an upper baffle for separating the upper head from the tank, wherein the upper baffle is located in an upper region of the tank and above the polymer solution inlet;
the first air flow distributor is used for separating the lower end socket from the tank body, an opening of the first air flow distributor is connected with an air outlet pipe, and the height of the air outlet pipe is at least higher than that of the liquid outlet pipeline;
the hollow internal components are used for enabling the polymer solution to flow in a membrane mode and a second stream in the pipe to flow, wherein the hollow internal components are uniformly and orderly arranged in the tank body, and the upper end and the lower end of each hollow internal component respectively penetrate through the upper partition plate and the first air flow distributor and extend into the upper end socket and the lower end socket; the part of the air flow entering from the air flow inlet of the lower end socket enters a closed space formed by the outer surface of the hollow inner member and the inner surface of the container from an air outlet pipe of the first air flow distributor to be used as first air flow; and the part of the air flow entering from the air flow inlet of the lower end socket enters the hollow inner component to be used as a second flow strand.
Further, the devolatilization apparatus may further comprise a supplemental inlet for the first gas stream; the first air flow supplement inlet is used for supplementing a first air flow to a closed space formed by the outer surface of the hollow inner member and the inner surface of the container, and the supplemented first air flow is used as a part of the first air flow in the container.
According to the invention, these further objects are firstly achieved by a process for devolatilizing a polymer solution comprising volatile components using the apparatus of the invention, wherein the process comprises:
the polymer solution enters the tank body through the polymer solution inlet and flows along the outer wall of the tube array in a film-shaped mode to form a film-shaped coating tube array outer wall, the specific surface area is increased, the first air flow enters the tank body through the first air flow and flows in the reverse direction of the film-forming liquid to perform mass and heat transfer processes, and finally volatile substances are carried out and discharged through the first air flow outlet; and the second flow strand enters the lower end head through the second flow strand inlet, then enters the tube array, transfers heat to the polymer liquid flowing in the membrane mode on the outer wall of the tube array through the tube wall, then is discharged to the upper end head, and finally is discharged through the second flow strand outlet.
The apparatus and process of the present invention can be used in the devolatilization of polymer liquids comprising volatile components, preferably polymer solutions having a relatively high viscosity.
The present invention achieves these objectives and provides a solution to this problem by virtue of the tubes being uniformly arranged in the tank and having dual drive operation only in the middle region of the upper and lower baffles. The tubes are preferably round tubes. The polymer solution in the middle area of the tube array flows in a film shape along the outer wall of the tube under the action of gravity, and the surface area and the surface renewal rate of the polymer solution are continuously increased in the flowing process. The first airflow flows in the tank body from bottom to top in a reverse direction with the film-forming liquid, and the reverse flow can stably carry away volatile components in the polymer solution while increasing the heat transfer efficiency; the second stream flows in the tubes, and gives higher temperature to the tubes, so that temperature difference is formed between the tubes and the outer walls of the tubes, heat conduction is further formed, the film-forming polymer solution at the outer walls of the tubes obtains heat, and volatile components are removed more efficiently; the second flow strand does not carry out mass transfer with the film polymer solution, so the second flow strand can be discharged and then heated and pressurized for recycling.
The apparatus and method then achieve the result that no special elaborate equipment is required, including moving parts such as screw blades or arms; without causing adverse conditions to the polymer, such as causing substantial thermal degradation of the polymer solution or significantly increasing residence time. The first airflow and the second airflow solve the problem of heat supply of the polymer solution in the devolatilization process by using a dual-drive principle; the second flow can be recycled, and consumption is reduced.
In a preferred embodiment of the apparatus or the method, the apparatus is provided with a liquid distributor and a first gas flow distributor, the liquid distributor being located in the tank below the polymer solution inlet and above the first gas flow outlet, the liquid distributor being essentially a baffle, wherein there are as many openings as there are tubes and each opening is arranged concentrically to the respective tube, the diameter of the openings being slightly larger than the diameter of the tubes, so that a gap is formed, the width of which can be designed; the first air flow distributor is substantially a partition plate, the tubes penetrate through the first air flow distributor without gaps, the first air flow distributor is provided with holes between the tubes and at the periphery of the tubes and is connected with an air outlet pipe upwards, the height of the air outlet pipe preferably exceeds the height of the liquid outlet pipeline, and the whole air outlet pipe and the whole tubes are arranged in a staggered manner. The polymer solution enters the tank body through a liquid outlet pipeline, and due to the existence of the liquid distributor, the polymer solution can form a liquid level on the liquid distributor and has a certain liquid level height, wherein the liquid level height can be adjusted according to the liquid inlet rate. Liquid on the liquid distributor flows downwards continuously through a gap formed by the open holes and the tubes by taking the outer walls of the tubes as supports, the flow rate and the initial film thickness can be adjusted by the width of the gap, so that the liquid is uniformly distributed, and the specific surface area is increased. The first airflow enters the tank body through the first airflow inlet, rapidly fills the area between the first airflow distributor and the lower partition plate, and is discharged to the tank body through the upper air outlet pipe of the first airflow distributor to form uniform distribution of the gas. It is worth noting that, at this time, the liquid accumulation area at the lower part of the tank body is positioned on the first air flow distributor, so the height of the exhaust pipe must be at least higher than the height of the liquid discharge pipeline, and the liquid in the liquid accumulation area can not pour into the area between the first air flow distributor and the lower partition plate. The liquid and the first gas flow distributor are added in the device, so that the liquid and the gas are uniformly distributed, the mass and heat transfer are uniform, and the film thickness and the falling rate of the polymer solution flowing along the pipe wall in a film form can be controlled.
In another preferred embodiment of the apparatus or the method, the apparatus is provided with a liquid distributor and a first gas flow distributor replacing the lower baffle, and the first gas flow inlet is eliminated, wherein the liquid distributor is located in the tank below the polymer solution inlet and above the first gas flow outlet, the liquid distributor is essentially a baffle, wherein the liquid distributor has the same number of openings as the tubes, and each opening is arranged concentrically with the respective tube, the diameter of the opening is slightly larger than the diameter of the tube, thereby forming a gap, and the width of the gap is adjustable; the first air flow distributor is positioned at the original lower partition plate and replaces the lower partition plate to directly separate the tank body from the lower seal head, the tubes still pass through the first air flow distributor and extend into the lower seal head, the opening of the first air flow distributor is connected with an air outlet pipe, and the height of the air outlet pipe is at least higher than that of the liquid outlet pipeline and is staggered with the tubes; the first air flow inlet is deleted, the first air flow in the tank body and the second air flow in the pipe are all supplied by the air flow inlet, the air flow enters the lower end socket through the air flow inlet and is filled, and then the air flow enters the tank body and the pipe arrays through the air outlet pipe and the pipe arrays respectively, wherein the air entering proportion can be distributed through the number proportion or the sectional area of the air outlet pipe and the pipe arrays. It should be noted that, taking the example of selecting steam as the introduced gas flow, although the apparatus only introduces the same steam, there is still a temperature difference, because the steam in the tank performs heat transfer and also a mass transfer process exists, when the volatile substance is gasified, a large amount of heat is absorbed to cause the temperature of the steam in the tank to drop, and the temperature difference is formed with the steam in the tubes to perform heat transfer.
In another preferred embodiment of the apparatus or the process, the first gas stream is at a pressure of less than 1bar, and a vacuum is formed in the shell side to enhance devolatilization mass transfer and to transfer heat from the second stream in the tube side along the outer walls of the tubes.
In a preferred embodiment of the process, and in a preferred use of the apparatus, the viscous polymer solution is a polymer melt and comonomer mixture or polymer and solvent mixed solution, and the volatile component is a solvent or monomer. In the present invention, "polymer melt and comonomer mixture" refers to the following polymers, namely: at a sufficiently high temperature to be in a liquid state and to be capable of flowing without including a substantial amount of solvent (e.g., based on the total mass of polymer and solvent, while containing less than 50% by weight solvent). The "polymer solvent mixed solution" refers to a mixture of a polymer and a solvent, in which the solvent content is 50w% or more based on the total mass of the polymer and the solvent. The above-described polymer solutions of the present invention have proven to be particularly useful in the devolatilization of polymer solutions.
Those skilled in the art will understand that: in the present invention, combinations of the subject matter of the various claims and embodiments of the present invention are possible within the scope of technical feasibility, and are not limited. In this combination, the subject matter of any one of the claims can be combined with the subject matter of one or more of the other claims. In such a combination of subject matter, the subject matter of any one process claim may be combined with the subject matter of one or more other process claims or the subject matter of one or more apparatus claims or the subject matter of a mixture of one or more process claims and apparatus claims. By analogy, the subject matter of any one device claim may be combined with the subject matter of one or more other device claims or the subject matter of one or more process claims or the subject matter of a mixture of one or more process claims and device claims. By way of example, the subject matter of any claim may be combined with the subject matter of any number of other claims without limitation, so long as such combination is technically feasible.
Those skilled in the art will understand that: in the present invention, the subject matter of the various embodiments of the present invention can be combined without limitation. For example, the subject matter of one of the above-described preferred apparatus embodiments may be combined with the subject matter of one or more of the other above-described preferred process embodiments, or vice versa, without limitation.
Drawings
The invention is further explained below with reference to the drawings and the examples.
FIG. 1 is a schematic view of a devolatilization apparatus provided by the present invention;
FIG. 2 is a schematic view of a devolatilization apparatus having a liquid distributor and a first gas flow distributor, wherein a polymer solution forms a liquid-holding surface at a certain height on the liquid distributor after entering the apparatus, and then uniformly falls into a film under the action of gravity through an annular space formed by the liquid distributor and a tube array; after entering the equipment, the first air flow is limited in the area between the first air flow distributor and the lower end socket and is uniformly discharged upwards through an upper discharge pipe of the first air flow distributor;
FIG. 3 is a schematic view of a devolatilization apparatus with the first gas inlet line removed and the first gas distributor coupled to a lower end baffle plate, wherein the apparatus does not require the first gas inlet, and gas flows into a lower end head and is discharged to the shell side and tube side, respectively, via lines and tubes on the lower end baffle plate;
FIG. 4 is a schematic view of a combination of a liquid distributor and a tube array;
FIG. 5 is another schematic view of the combination of a liquid distributor and a tube array;
fig. 6 shows a schematic view of the first flow distributor in combination with the tubes.
In the figure, a-polymer solution inlet; a' -polymer solution outlet; b-a first gas stream inlet; b' -a first airflow outlet; c-a second stream inlet; a C' -second stream outlet; 1-sealing an upper end; 2-an upper end flange; 3-tank body; 4-a lower end flange; 5-sealing the lower end; 6-tubulation; 7-a liquid distributor; 8-a first air flow distributor; 9-first air distributor discharge pipe 1; 10-first air flow distributor discharge pipe 2; 11-a liquid distributor surface; 12-liquid distributor annulus; 13-gas distributor surface.
Detailed Description
The invention will be further illustrated and described with reference to specific embodiments. The described embodiments are merely exemplary of the disclosure and are not intended to limit the scope thereof. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
Fig. 1 is a schematic view showing an alternative structure of the polymer solution devolatilization apparatus of the present invention, which is composed of upper and lower end caps 1, 5, an intermediate tank 3 and an inner tube array 6. The upper end socket and the lower end socket are respectively provided with a second flow outlet C ' and a second flow inlet C, and the tank body is respectively provided with a pair of polymer solution inlets and outlets A and A ' and first airflow inlets and outlets B and B '.
As described in the method, the polymer solution 100 firstly enters the tank 3 through the polymer solution inlet a and flows down along the outer wall of the tube array 6 in a membrane manner, and finally forms a liquid accumulation area at the lower part of the tank 3 and is discharged as a devolatilization material stream 110 through the polymer solution outlet a'; the first gas flow 200 enters the tank 3 through the first gas flow inlet B, flows in a reverse direction and continuously contacts the material flow 100 from bottom to top in the tank 3, and finally is discharged as a mixture 210 of the first gas flow and volatile components through a pipe B'. Taking the example that the second flow strand selects steam and the hollow inner member selects a tube array (at this time, the polymer solution devolatilization device is actually a double-drive tube array devolatilizer), steam 300 enters the lower end socket 5 through the second flow strand inlet C, then enters the tube array 6, the steam 300 conducts heat to the polymer solution 100 flowing on the outer wall in a membrane manner through the tube wall, then is discharged to the upper end socket, and finally is discharged as steam 310 through the second flow strand outlet C'. If the second flow strand selects liquids such as heat transfer oil, the heat transfer oil (or other liquid media) enters the lower end head 5 through the second flow strand inlet C and then enters the tube array 6, and the heat transfer oil (or other liquid media) transfers heat to the polymer solution 100 flowing on the outer wall in a membrane manner through the tube wall, and then is discharged to the upper end head and discharged through the second flow strand outlet.
It should be noted that in the above apparatus, the sealing between the end sockets 1, 5 at the two ends and the intermediate tank 3 is required, so that upper and lower end partition plates (not shown in the figure) are disposed at the upper and lower end flanges 2, 4, and should be welded to the upper and lower end sockets or the upper and lower ends of the tank, so as to maintain the sealing, so that the first air flow 200 does not leak to the upper end socket through the upper end partition plate and contact with the second stream, and the polymer fluid, which is devolatilized in the liquid accumulation zone below the tank, does not leak to the lower end socket through the lower end partition plate and contact with the second stream. In addition, the tubes 6 should pass through the upper and lower end baffles and extend into the end enclosures, so that the second stream can flow between the upper and lower end enclosures through the tubes 6, and the joints of the tubes 6 and the upper and lower end baffles should be sealed to prevent steam leakage.
As shown in FIG. 2, which is a schematic diagram of a preferred structure of a polymer solution devolatilization device according to the present invention, the double-drive shell and tube devolatilizer shown in FIG. 2 can solve the problem of uneven gas-liquid distribution of the device shown in FIG. 1, by taking the second stream selected steam and the hollow inner member selected shell and tube as an example. The device is provided with a liquid distributor 7 and a first gas flow distributor 8, wherein the liquid distributor 7 is located at the lower end of the polymer solution inlet a and the upper end of the first gas flow outlet B ', and the first gas flow distributor 8 is located at the upper end of the first gas flow inlet B and the lower end of the polymer solution outlet a', and in one embodiment, the device and its components are constructed of metal. Suitable metals include, but are not limited to, carbon steel, stainless steel, nickel alloys, copper alloys, titanium, and zirconium.
The embodiment in fig. 2 shows a substantially vertical apparatus, but the person skilled in the art will understand that other orientations of the device are possible as long as technically feasible.
It is worth noting that after the polymer solution 100 enters the tank body 3, a liquid holding surface with a certain height is formed on the liquid distributor, and then the polymer solution uniformly falls under the action of gravity through an annular gap formed by the liquid distributor 7 and the tube array 6, so that the specific surface area is increased; after entering the tank body 3, the second flow is limited to the area between the first air flow distributor 8 and the lower end socket 5 and is uniformly discharged upwards through the first air flow distributor discharge pipes 9 and 10. Because the existence of liquid distributor and first air current distributor, the gas-liquid distribution is more even in whole device for the mass transfer heat transfer is more abundant, thereby takes off the effect better.
Referring to fig. 3, which is a schematic view of another preferred embodiment of the dual-drive shell and tube devolatilizer according to the present invention, the apparatus combines a first gas flow distributor 8 with a lower partition plate and removes a first gas flow inlet on the basis of fig. 2, wherein steam enters a lower end socket, a part of the steam is discharged to a shell side through first gas flow distributor discharge pipes 9 and 10 on the first gas flow distributor 8 as a first gas flow, and a part of the steam enters a tube side through a shell and tube 6 as a second flow. Besides steam, other gas media with higher hot melting can be selected as the working media of the dual-drive shell and tube devolatilizer, and the principle and the working method are the same as those of the steam.
It should be noted that, although a steam 300 is introduced instead in fig. 3, it still can perform the double (steam) driving function, because in addition to the heat exchange process, the steam in the shell side needs to supply heat for the gasification of volatile components, which results in temperature drop, and after the steam 300 enters the lower end socket, the steam amount entering the shell side and the tube side can be distributed by changing the number of the exhaust pipes 9 and 10 and the number and the cross-sectional area of the rows 6 of pipes of the first airflow distributor. Its advantages are: only one stream of steam enters; the first air distributor replaces the lower end baffle plate to enable the tank body to have longer space for the liquid film to flow.
Referring to fig. 4, which is a schematic top view of the liquid distributor 7, 11 is the surface of the liquid distributor 7, and it can be seen that the surface 11 has a plurality of openings, the number of which is the same as the number of the tubes 6, and each of which is arranged concentrically with a tube, the diameter of the opening is slightly larger than the outer diameter of the tube to form an annular space 12, and the width of the annular space can be adjusted by the diameter of the opening.
Fig. 5 shows a three-dimensional view of the liquid distributor 7, wherein the column 6 extends through the liquid distributor 7, and the upper part of the liquid distributor is a liquid accumulation area where the material stream 100 is collected and has a certain height, and the column located at the upper part of the liquid distributor 7 can be used for preheating the material stream 100, and then the material stream 100 flows down along the outer wall of the column 6 through the annular space 12 under the action of gravity. The flow velocity and the film thickness can be adjusted by parameters such as the number of openings, the height of the liquid holding surface, the width of the annular space and the like, and preferably, the retention time of the polymer solution in the film flowing on the outer surface of the hollow inner member is not less than 1 minute.
FIG. 6 shows a three-dimensional view of the first air flow distributor 8, wherein the tubes 6 extend through the first air flow distributor 8, and the upper part of the first air flow distributor is a liquid accumulation area where the devolatilization material stream 110 converges and has a certain height, and finally exits through the polymer solution outlet A'; the first flow distributor discharge pipe 9, 10 does not pass through the first flow distributor 8 but is only connected with the upper surface 13 of the first flow distributor 8.
It should be noted that the liquid level of the liquid accumulation region formed on the first air distributor 8 must be higher than the liquid outlet a 'to prevent the first air flow from being discharged through the liquid outlet a' to affect the final effect; but not higher than the height of the first gas flow distributor discharge pipes 9, 10, so as to prevent the devolatilized material stream 110 from entering the lower end enclosure through the first gas flow distributor discharge pipes 9, 10 to affect the normal operation of the device.
The method is described in further detail below with reference to specific examples, wherein the first and second streams used in examples 1, 3-4 are both water vapor, and the first stream used in example 2 is nitrogen; the examples 1 to 4 are all dual-drive shell and tube devolatilizers.
Example 1:
in the embodiment, the ethylene-1-octene elastic Polymer (POE) system is obtained by solution polymerization, the solvent is n-hexane, and after primary devolatilization, the content of the POE system solvent is 30w%, the temperature is 200 ℃, and the pressure is 3bar. The dual-drive tube array type devolatilizer is shown in figure 3, the tube diameter of the tube array is 16mm, the tube array comprises 16 tubes, the diameter of the round hole of the liquid distributor is 40mm, the number of the round holes is consistent with that of the tube array, and the width of the circular seam formed by the round holes and the outer wall shape of the tube array is 12mm. The liquid holding height above the liquid distributor is 30mm. Steam enters from the port C, the temperature is 240 ℃, the steam enters the tank body and the tubes through the gas distributor respectively, and the distribution ratio of the gas flow in the tank body to the gas flow in the tubes is 3. In the devolatilization process, the POE system flows down along the pipe wall in a membrane mode and continuously bubbles to perform devolatilization, flows to the upper part of the gas distributor to form a liquid holding surface, and is discharged. The solvent residual content in the POE system is 3000ppm.
The material consumption and the energy consumption in the whole process are as follows: steam consumption was 6 tons/ton POE.
Example 2:
in this example, a POE system was obtained by solution polymerization, the solvent was n-pentane, and after the initial devolatilization, the solvent content of the POE system was 10w%, the temperature was 220 ℃, and the pressure was 2.8bar. The dual-drive shell and tube devolatilizer is shown in FIG. 2, and nitrogen gas is introduced from port B at a temperature of 200 ℃. The diameter of the corrugated pipe is 20mm, the total number of the corrugated pipes is 16, the diameter of the round holes of the liquid distributor is 40mm, the number of the round holes is consistent with that of the corrugated pipes, and the width of a circular seam formed by the round holes and the shape of the outer wall of the corrugated pipe is 10mm. The liquid holding height above the liquid distributor is 30mm. The water vapor circulates in the tubes, and the temperature is 240 ℃. In the devolatilization process, the POE system flows down along the pipe wall in a membrane mode and continuously bubbles to perform devolatilization, flows to the upper part of the gas distributor to form a liquid holding surface, and is discharged. The solvent residual content in the POE system is 1300ppm finally.
The material consumption and the energy consumption in the whole process are as follows: the steam consumption is 3.25 tons/ton POE, and the nitrogen consumption is 2 tons/ton POE.
Example 3:
in this example, after the butadiene rubber-n-hexane system obtained by polymerization was subjected to preliminary devolatilization, the n-hexane content remained 10w%, the temperature was 120 ℃, and the pressure was 3bar. The dual drive shell and tube devolatilizer is shown in FIG. 2 at a pressure of 1bar and a first gas stream temperature of 120 ℃. The pipe diameter of each row pipe is 16mm, the number of the row pipes is 24, the diameter of the round hole of the liquid distributor is 12mm, the number of the round holes is consistent with that of the row pipes, and the width of the circular seam formed by the round holes and the outer wall shape of the row pipes is 7mm. The liquid holding height above the liquid distributor is 50mm. The water vapor circulates in the tube array at the temperature of 150 ℃. In the devolatilization process, the butadiene rubber-normal hexane system flows down along the pipe wall in a membrane mode and continuously foams to devolatilize, flows to the upper portion of the gas distributor to form a liquid holding surface, and then is discharged. Finally, the residual n-hexane content in the cis-butadiene rubber-n-hexane system is 900ppm.
The material consumption and the energy consumption in the whole process are as follows: the steam consumption was 3.25 tons per ton of butadiene rubber.
Example 4:
in this example, the chlorinated polyvinyl chloride-chlorobenzene solution after the chlorination reaction had a chlorobenzene content of 85w%, a temperature of 100 ℃ and a pressure of 2bar. The double-drive tube array type devolatilization device is shown in figure 2, the pressure is 1.3bar, the first airflow temperature is 140 ℃, the pipe diameters of the corrugated pipes are 30mm, 12 in total, the diameter of the circular holes of the liquid distributor is 40mm, the number of the circular holes is consistent with that of the corrugated pipes, and the circular seams are 5mm wide with the outer walls of the corrugated pipes. The liquid holding height above the liquid distributor is 35mm. The water vapor was circulated through the tubes at a temperature of 170 ℃. In the devolatilization process, the chlorinated polyvinyl chloride-chlorobenzene solution flows down in a film shape along the pipe wall and is subjected to flash devolatilization and bubble devolatilization, flows to the upper part of the gas distributor to form a liquid holding surface, and is discharged. The residual chlorobenzene content in the chlorinated polyvinyl chloride-chlorobenzene solution finally obtained was 5w%.
The material consumption and the energy consumption in the whole process are as follows: the steam consumption was 2.8 tons per ton of chlorinated polyvinyl chloride.
Example 5:
in this example, which is a comparative example of example 1, a solution polymerization was performed to obtain a POE system, in which n-hexane was used as a solvent, and 30w% of the solvent content of the POE system remained after the initial devolatilization, the temperature was 200 ℃, and the pressure was 3bar. The double-drive tube array type devolatilizer is shown in figure 3, the tube diameter of the tube array is 16mm, the tube array comprises 16 tubes, the diameter of the circular holes of the liquid distributor is 40mm, the number of the circular holes is consistent with that of the tube array, and the width of the circular seam formed by the circular holes and the outer wall of the tube array is 12mm. The liquid holding height above the liquid distributor is 30mm. No gas is introduced into the port B, and water vapor enters from the port C, the temperature is 240 ℃, and the water vapor only enters the tube array through the gas distributor. In the devolatilization process, the POE system flows down along the pipe wall in a film form and continuously foams to perform devolatilization, flows to the upper part of the gas distributor to form a liquid holding surface, and is discharged. The residual solvent content in the POE system is 13500ppm.
The material consumption and the energy consumption in the whole process are as follows: steam consumption was 6 tons/ton POE.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (11)
1. A polymer solution devolatilization method, in a container having a hollow inner member, a polymer solution containing volatile components is fed from the upper portion of said container, flows down along the outer surface of said hollow inner member to form a liquid film, converges at the bottom of said container to form a solution pool, and is discharged through a liquid discharge port located at the bottom of said container; the volatile components in the polymer solution are discharged from a vent at the upper part of the container after escaping, and the method is characterized in that: introducing a first gas flow into a closed space formed by the outer surface of the hollow inner member and the inner surface of the container, and enhancing the devolatilization effect of the polymer solution by enhancing mass transfer; introducing a second stream into the hollow inner member for heating the formed liquid film; the first gas stream is discharged from a vent in the upper portion of the vessel after counter-current contact with the polymer solution.
2. A method of devolatilization of polymer solutions as claimed in claim 1 wherein: the first gas stream is a mixture of one or more of nitrogen, carbon dioxide or water vapor.
3. A method of devolatilization of polymer solutions as claimed in claim 1 wherein: the second stream is water vapor, water, silicon oil or heat conducting oil; the temperature of the second stream is higher than the temperature of the polymer solution.
4. A method of devolatilizing polymer solutions as defined in claims 1-3 wherein: the ratio of the volume flow rates of the first and second streams is 1:5 to 5, the ratio of the volume flow of the first gas stream to the volume flow of the polymer solution being 1.
5. A method of devolatilization of polymer solutions as claimed in claim 3 wherein: the second air flow is water vapor, the water vapor is introduced from the bottom of the container, one part of the water vapor is introduced into the hollow inner member to serve as a second flow, and the other part of the water vapor enters a closed space formed by the outer surface of the hollow inner member and the inner surface of the container to serve as the first air flow alone or as one part of the first air flow.
6. A method of devolatilizing a polymer solution as defined in claim 1 wherein: there are at least 2 of said hollow internals in said vessel; the polymer solution flows on the outer surface of the hollow inner member in a membrane mode, the Reynolds number is not higher than 2000, and the retention time is not lower than 1 minute.
7. A method of devolatilization of polymer solutions as claimed in claim 1 or claim 6, wherein: the hollow inner component is one or a combination of a plurality of circular tubes, square tubes, polygonal tubes, corrugated tubes or straight tubes with spiral grooves.
8. A devolatilization apparatus for carrying out the process of claim 1 comprising:
a tank for receiving the polymer solution,
a polymer solution inlet for introducing a polymer solution into the tank;
a polymer solution outlet for leading the polymer solution with the volatile components removed out of the tank body;
a first gas flow inlet for introducing a first gas flow into the tank;
the first air flow outlet is used for leading the first air flow and the volatile component mixed gas out of the tank body;
the upper end socket comprises a second flow outlet for discharging a second flow, and the lower end socket comprises a second flow inlet for allowing the second flow to enter;
an upper baffle for separating the upper head from the tank, wherein the upper baffle is located in an upper region of the tank and above the polymer solution inlet;
a lower baffle for separating the lower head from the tank, wherein the lower baffle is located in a lower region of the tank and below the first gas inlet;
and the hollow internal components are uniformly and orderly arranged in the tank body, penetrate through the upper partition plate and the lower partition plate and extend into the upper end enclosure and the lower end enclosure.
9. A devolatilization apparatus as claimed in claim 8,
the device is provided with a liquid distributor and a first airflow distributor, wherein the liquid distributor is positioned in the tank body, is positioned below the polymer solution inlet and above the first airflow outlet, and is a partition plate, the liquid distributor is provided with openings with the same number as the tubes, each opening is concentrically arranged with the tube, and the diameter of each opening is larger than that of the tube, so that a circular seam is formed for the polymer liquid to form a film and flow, and the specific surface area is increased; the first air flow distributor is a partition plate, the tubes pass through the first air flow distributor without gaps, the first air flow distributor is provided with holes between the tubes and at the periphery of the tubes and is upwards connected with an air outlet pipe, and the height of the air outlet pipe exceeds the height of the liquid outlet pipeline.
10. A devolatilization apparatus for carrying out the process of claim 1, in which said second stream is a gas stream, said apparatus comprising:
a tank for receiving the polymer solution,
a polymer solution inlet for introducing a polymer solution into the tank;
a polymer solution outlet for leading the polymer solution with the volatile components removed out of the tank body;
the upper end socket and the lower end socket are used for being connected with the tank body, the upper end socket comprises a second flow outlet for discharging a second flow, and the lower end socket comprises an airflow inlet;
a first gas flow outlet for leading the first gas flow and the volatile component mixed gas out of the tank body;
an upper baffle for separating the upper head from the tank, wherein the upper baffle is located in an upper region of the tank and above the polymer solution inlet;
the liquid distributor is a partition plate, the liquid distributor is provided with openings the number of which is the same as that of the tubes, each opening is concentrically arranged with the tube in the tube, the diameter of each opening is larger than that of the tube, so that a circular seam is formed for the film forming flow of the polymer liquid and the specific surface area is increased, and the liquid distributor is positioned above the first airflow outlet;
the first air flow distributor is used for separating the lower end socket from the tank body, the opening of the first air flow distributor is connected with an air outlet pipe, and the height of the air outlet pipe is at least higher than that of the liquid outlet pipeline;
the hollow internal components are used for enabling the polymer solution to flow in a membrane mode and a second stream in the pipe to flow, wherein the hollow internal components are uniformly and orderly arranged in the tank body, and the upper end and the lower end of each hollow internal component respectively penetrate through the upper partition plate and the first air flow distributor and extend into the upper end socket and the lower end socket; the part of the airflow entering from the airflow inlet of the lower end socket enters a closed space formed by the outer surface of the hollow inner member and the inner surface of the container from an air outlet pipe of the first airflow distributor to be used as first airflow; and the part of the air flow entering from the air flow inlet of the lower end socket enters the hollow inner component to be used as a second flow strand.
11. A devolatilization apparatus as claimed in claim 10, further comprising: a first air flow make-up inlet; the first air flow supplement inlet is used for supplementing a first air flow to a closed space formed by the outer surface of the hollow inner member and the inner surface of the container, and the supplemented first air flow is used as a part of the first air flow in the container.
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| WO2025029188A1 (en) * | 2023-08-03 | 2025-02-06 | Sui Jianjun | Devolatilization apparatus and method for a polymer solution |
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| WO2025029188A1 (en) * | 2023-08-03 | 2025-02-06 | Sui Jianjun | Devolatilization apparatus and method for a polymer solution |
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