CN112724281A - Method and system for removing solvent in polymer solution - Google Patents

Method and system for removing solvent in polymer solution Download PDF

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Publication number
CN112724281A
CN112724281A CN201911033282.4A CN201911033282A CN112724281A CN 112724281 A CN112724281 A CN 112724281A CN 201911033282 A CN201911033282 A CN 201911033282A CN 112724281 A CN112724281 A CN 112724281A
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polymer
solution
solution phase
polymer solution
solvent
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CN112724281B (en
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宋文波
韩书亮
王路生
金钊
李昊坤
方园园
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Sinopec Beijing Chemical Research Institute Co ltd
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/06Treatment of polymer solutions
    • C08F6/10Removal of volatile materials, e.g. solvents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08CTREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
    • C08C2/00Treatment of rubber solutions

Abstract

The invention relates to a method for removing a solvent in a polymer solution, which comprises the following steps: (1) introducing the polymer solution into a coil heater for heating, so that the polymer solution is divided into a dilute solution phase and a concentrated solution phase in the coil heater; (2) carrying out flash evaporation treatment on the concentrated solution phase obtained in the step (1) to remove the solvent in the concentrated solution phase; the polymer solution remains in a full liquid phase during the heating. The polymer solution is obtained by a solution polymerization method and comprises a polymer and a solvent; the concentration of the polymer in the polymer solution is 5-20 wt.%. By adopting the method, the mass concentration of the polymer in the treated polymer solution can reach more than 90 mass percent through the serial operation of the coil heater and the flash evaporation and the control of the process parameters in the heating and flash evaporation processes.

Description

Method and system for removing solvent in polymer solution
Technical Field
The invention relates to the field of polymer preparation, in particular to a method and a system for removing a solvent in a polymer solution.
Background
The solution polymerization process plays an important role in the polymer material industry. The process can be used for producing various products such as fiber, rubber, plastic, elastomer, paint, adhesive and the like. However, the separation of the polymer from the polymer solution produced by solution polymerization is more complicated than other processes. In China, the polymer solution is generally subjected to condensation stripping operation by introducing steam, catalyst residues are decomposed and removed, then polymer separation is carried out, finally, volatile components such as solvent, unreacted monomers and residual small amount of water are removed, the polymer is made into porous small-particle products for subsequent drying treatment, and the solvent is collected by a recovery device for recycling.
In the prior art, when synthetic rubber or elastomer (such as styrene-butadiene rubber, isoprene rubber, butadiene rubber and the like) is produced by a solution polymerization method, the obtained polymer solution is subjected to coagulation stripping process, and then is subjected to extrusion, dehydration and drying; in the case of preparing synthetic resins (such as styrene-butadiene resin and linear low-density polyethylene) by a solution polymerization method, the solvent of the obtained polymer solution cannot be removed by a condensation stripping process, and other processes are needed to increase the concentration of the polymer in the solution, and then the residual solvent in the polymer is removed by volatile removal treatment. The condensation process usually adopts double-kettle condensation or three-kettle condensation, the solvent removal effect can be improved by multi-kettle condensation operation, the residence time of the three kettles can be prolonged by adopting measures such as a concentrator and the like, and the solvent removal effect is improved.
CN102382214A discloses a coagulation process for producing a polymerization product, which adopts a process technology combining a three-kettle pressure difference coagulation with a colloidal particle concentration technology, and a concentrator is arranged between a second coagulation kettle and a third coagulation kettle to concentrate colloidal particle water, so that a new energy-saving and consumption-reducing process is formed.
Disclosure of Invention
The invention aims to overcome the defects of limitation, high energy consumption, high steam consumption and high cost in the process of removing a solvent from a polymer solution in the prior art, and provides a novel method and a novel system for removing the solvent from the polymer solution.
In order to achieve the above object, the present invention provides a method for removing a solvent from a polymer solution, comprising:
(1) introducing the polymer solution into a coil heater for heating treatment, so that the polymer solution is divided into a dilute solution phase and a concentrated solution phase in the coil heater;
(2) carrying out flash evaporation treatment on the concentrated solution phase obtained in the step (1) to remove the solvent in the concentrated solution phase;
the polymer solution remains in a full liquid phase state during the heat treatment.
According to some embodiments of the invention, the polymer solution is a solution polymerization process resulting in a polymer solution comprising a polymer and a solvent; the concentration of the polymer in the polymer solution is 5 to 20 wt.%, preferably 6 to 15 wt.%.
According to a preferred embodiment of the present invention, the polymer in the polymer solution comprises one or more of a rubber, a thermoplastic elastomer and an acrylic resin, wherein the rubber preferably comprises one or more of butadiene-styrene rubber, butadiene rubber, isoprene rubber and styrene-isoprene rubber, and the thermoplastic elastomer preferably comprises one or more of ethylene- α -olefin copolymer (POE), ethylene- α -olefin-non-conjugated diene copolymer, styrene-butadiene-styrene block copolymer and hydrogenated styrene-butadiene-styrene block copolymer.
According to a preferred embodiment of the present invention, the solvent in the polymer solution includes at least one of cyclohexane, cycloheptane, toluene, benzene, xylene, n-hexane, n-heptane, n-octane, and n-decane.
According to some specific embodiments of the present invention, the ethylene- α -olefin copolymer is EPR, an ethylene-1-butene copolymer elastomer or an ethylene-1-octene copolymer elastomer.
According to some embodiments of the invention, in step (1), the polymer solution is heated in a coil heater to stratify the polymer solution, the upper layer being a dilute solution phase having a polymer concentration of less than 1 wt.%, the lower layer being a concentrated solution phase having a polymer concentration of 20 to 50 wt.%, the upper olefin solution phase being predominantly solvent.
According to a preferred embodiment of the present invention, the coil heater is heated by steam, preferably, the heating temperature is 100 to 250 ℃, more preferably 150 to 220 ℃; and/or the pressure in the coil heater is 10-50 atm.
According to the preferred embodiment of the present invention, the polymer solution is introduced into the coil heater to be heated, so that the polymer solution is separated into a dilute solution phase and a concentrated solution phase in the coil, wherein the dilute solution phase is separated and discharged, and the concentrated solution phase is introduced into the step (2) to continue the treatment.
According to a preferred embodiment of the present invention, in the step (2), the concentrated solution phase is introduced into a flash apparatus to be subjected to a flash treatment, and the solvent in the concentrated solution phase is further removed.
According to the preferred embodiment of the invention, the flash device is preferably a flash tank, wherein the flash tank adopts adiabatic operation, and the operating pressure is 1.1-2.0 atm, preferably 1.3-1.8 atm;
according to a preferred embodiment of the invention, the operating liquid level of the concentrated solution phase in the flash tank is controlled to be 1/5-1/2, preferably 1/4-1/3 of the total volume of the flash tank.
According to a preferred embodiment of the invention, the concentrated solution phase is introduced into a flash tank, where it is subjected to a flash treatment due to the lower pressure in the flash tank, further removing the solvent therefrom, the removed solvent being discharged from the top of the flash tank, and the polymer concentration in the remaining mass, higher than 90 wt.%, being discharged from the bottom of the flash tank.
According to some embodiments of the invention, the method comprises performing a plurality of primary flashing operations.
Wherein the first stage flash operation is defined as the heating of the polymer solution by the coil heater and the flash processing by the flash tank.
Preferably, the process comprises more than one flash tank and the heating of the polymer solution by means of a coil and one flash tank flash is referred to as a first stage flash operation. After the first-stage flash evaporation operation, if the solvent removal effect in the polymer solution does not meet the process requirements, the multistage heating and flash evaporation series operation, preferably the first-stage flash evaporation operation, can be adopted on the premise of ensuring that the polymer solution can be conveyed.
In the method, the solvent recovered after the multi-stage heating and flash evaporation series operation can enter a solvent recovery and refining system, and light components, heavy components and other impurities in the solvent are removed and then the solvent is recycled.
To solve the object of the present invention, the present invention also provides a system for removing a solvent from a polymer solution, comprising:
the coil heater is used for heating the polymer solution to enable the polymer solution to be divided into a dilute solution phase and a concentrated solution phase in the coil;
a vertical tube comprising an inlet, a first outlet and a second outlet, wherein the inlet is connected to a coil heater, the first outlet is used to separate a dilute solution phase, the second outlet is connected to a flash apparatus, and the first outlet is located above the second outlet;
and the flash evaporation device is used for carrying out flash evaporation treatment on the concentrated solution phase. According to some embodiments of the invention, a temperature monitoring device and a pressure monitoring device are disposed on the riser. Wherein the temperature monitoring device comprises a remote thermometer and the pressure monitoring device comprises a pressure regulating valve.
In the present invention, in order to allow the polymer solution to phase separate before introduction into the flash tank, it is preferred to provide a telemetric thermometer on the vertical tube of the polymer solution from the coil to the flash tank for monitoring the temperature of the polymer solution after the outlet of the coil and before the flash tank. In order to enable phase separation of the polymer solution before introduction into the flash tank, a pressure regulating valve is preferably provided on the riser of the polymer solution from the heater to the flash tank for monitoring the pressure after the outlet of the heater and before the flash tank.
To solve the object of the present invention, the present invention also provides a use of the above system for removing a solvent from a polymer solution, comprising:
(1) introducing the polymer solution into a coil heater for heating treatment, so that the polymer solution is divided into a dilute solution phase and a concentrated solution phase in the coil and enters the vertical pipe through an inlet of the vertical pipe;
(2) the dilute solution phase is separated and discharged through a first outlet of the vertical pipe, and the concentrated solution phase enters a flash evaporation device through a second outlet of the vertical pipe;
(3) and carrying out flash evaporation treatment on the concentrated solution phase in a flash evaporation device to remove the solvent in the polymer solution.
According to some embodiments of the invention, the polymer solution is a solution polymerization process; the concentration of the polymer in the polymer solution is 5 to 20 wt.%, preferably 6 to 15 wt.%.
According to a preferred embodiment of the present invention, the polymer in the polymer solution comprises one or more of a rubber, a thermoplastic elastomer and an acrylic resin, wherein the rubber preferably comprises one or more of butadiene-styrene rubber, butadiene rubber, isoprene rubber and styrene-isoprene rubber, and the thermoplastic elastomer preferably comprises one or more of ethylene- α -olefin copolymer (POE), ethylene- α -olefin-non-conjugated diene copolymer, styrene-butadiene-styrene block copolymer and hydrogenated styrene-butadiene-styrene block copolymer.
According to a preferred embodiment of the present invention, the solvent in the polymer solution includes at least one of cyclohexane, cycloheptane, toluene, benzene, xylene, n-hexane, n-heptane, n-octane, and n-decane.
According to some specific embodiments of the present invention, the ethylene- α -olefin copolymer is EPR, an ethylene-1-butene copolymer elastomer or an ethylene-1-octene copolymer elastomer.
According to a preferred embodiment of the present invention, the coil heater is heated by steam, preferably, the heating temperature is 100 to 250 ℃, more preferably 150 to 220 ℃; and/or the pressure in the coil heater is 10-50 atm.
According to the preferred embodiment of the invention, the flash device is preferably a flash tank, wherein the flash tank adopts adiabatic operation, and the operating pressure is 1.1-2.0 atm, preferably 1.3-1.8 atm;
according to a preferred embodiment of the invention, the operating liquid level of the concentrated solution phase in the flash tank is controlled to be 1/5-1/2, preferably 1/4-1/3 of the total volume of the flash tank.
Compared with the prior art, the invention has the following characteristics:
adopt coil pipe heater, practice thrift installation space, but unit replacement, later maintenance is convenient, and more importantly polymer solution is high viscosity system, mostly is laminar flow state in the pipeline, and flow rate is lower, and heat transfer mass transfer is more difficult, adopts coil pipe heat exchanger to carry out the heat transfer more abundant, can guarantee that liquid pressure drop is less simultaneously. By adopting the method, the mass concentration of the polymer in the treated polymer solution can reach more than 90 mass percent through the serial operation of the coil heater and the flash evaporation and the control of the process parameters in the heating and flash evaporation processes; the polymer glue solution which can be subjected to condensation stripping operation or not subjected to condensation flash evaporation can be sent to a post-treatment system for extrusion, devolatilization, granulation and other operations, and finally the removal of the solvent is finished, and the material consumption and the energy consumption in the whole process can be respectively reduced by about 50 percent and 20 percent compared with the prior art.
Drawings
FIG. 1 is a process flow diagram of a preferred embodiment of the process of the present invention.
Description of reference numerals: 1. a polymer solution obtained after solution polymerization; 2. a coil heater; 3. a flash tank; 4. a concentrated solution phase solvent recovery system; 5. a glue solution post-treatment system; 6. dilute solution phase recovery system.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
According to a specific embodiment, the system for removing a solvent from a polymer solution according to the present invention is shown in fig. 1, and comprises: coil heater 2, flash distillation plant 3 and riser 7, the flash tank entrance is provided with the governing valve, wherein, riser 7 is including the import, first export and the second export that are located riser 7 middle part, coil heater 2's exit linkage to the import of riser 7, first export is located on the second export, first exit linkage to weak solution phase solvent recovery system 6, the second exit linkage to flash distillation plant 3's entry, still be provided with teletransmission thermometer and/or pressure regulating valve on the riser 7. The flash evaporation device comprises a concentrated solution phase solvent outlet and a glue solution outlet, the glue solution outlet is connected to a glue solution post-treatment system 5, and the concentrated solution phase solvent outlet is connected to a concentrated solution phase solvent recovery system 4.
The process flow of the method for removing the solvent by using the solvent removal unit is as follows, specifically:
the polymer solution 1 obtained after solution polymerization firstly enters a coil heater 2, the temperature of the polymer solution at the outlet of the coil heater 2 is controlled by controlling the steam flow for supplying heat, the pressure of the polymer solution in the coil heater and a vertical pipe is controlled by adjusting the opening degree of an adjusting valve at the inlet of a flash tank 3, so that the polymer solution is in a liquid-liquid phase separation state before entering the flash tank 3, and the polymer solution in the phase separation state comprises a dilute solution phase with the polymer concentration of less than 1 wt.% and a concentrated solution phase with the polymer concentration of 20-50 wt.%. In the vertical pipe 7, the dilute solution phase density is lower on the upper layer and the concentrated solution phase density is higher on the lower layer after phase splitting, the dilute solution phase on the upper layer is directly conveyed to the dilute solution phase recovery system 6 through the first outlet of the vertical pipe 7 for solvent recovery treatment, the concentrated solution phase enters the flash tank 3 through the second outlet of the vertical pipe for solvent flash evaporation, the solvent is discharged from the outlet 4 of the flash tank, and the residual polymer solution flows out from the outlet 5 at the bottom of the flash tank. The polymer solution after solvent removal is directly sent into a post-treatment system through a condensation system or without the condensation system, and finally solvent removal is completed; and condensing the gas phase solvent obtained by flash evaporation, and then taking the condensed gas phase solvent as the removed solvent to enter a solvent recovery and refining system, thereby finally realizing the recycling of the solvent.
The present invention will be described in detail below by way of examples.
In the following examples, various raw materials used are commercially available without specific description.
Examples ethylene-propylene rubber (EPR), polybutadiene rubber or polyolefin elastomer (POE) is used as an example, and the solvent is a mixture of cyclohexane and n-hexane (80% by weight of n-hexane). Wherein the weight average molecular weight of the ethylene propylene rubber is 14 ten thousand, the molecular weight distribution is 2.0, and the ethylene mass fraction is 50%; the weight average molecular weight of POE is 13 ten thousand, the molecular weight distribution is 2.0, the ethylene mass fraction is 60-62%, the weight average molecular weight of polybutadiene rubber is 39 ten thousand, and the molecular weight distribution is 3.8.
The glue solution flow entering the coil heater in the following examples is 10 kg/h.
Example 1
The EPR concentration is 10 wt%, the glue solution temperature is 90 ℃, the pressure is 20atm, the glue solution is sent into a coil heater 2, the glue solution temperature is raised to 220 ℃, the pressure in the coil heater 2 is ensured to be 40atm at the moment, the glue solution is divided into two phases, the upper layer is a dilute solution phase, the EPR concentration is less than 1%, the lower layer is a concentrated solution phase, the EPR concentration is 35%, the dilute solution phase directly enters a dilute solution phase recovery system 6, and the concentrated solution enters a flash tank 3; the flash tank 3 is in adiabatic operation, the operating pressure is 1.3atm (absolute pressure), the operating liquid level of the polymer solution in the primary flash tank 3 is 1/3 of the total volume of the flash tank 3, after flash evaporation, the concentration of the polymer in the EPR glue solution is increased to 90 wt%, the temperature of the EPR glue solution is reduced to 92.7 ℃, the solvent enters the concentrated solution phase solvent recovery system 4 through an upper outlet of the flash tank, the concentrated glue solution enters the post-treatment system 5, and finally the removal of the solvent is completed.
The material consumption and energy consumption of the whole process are as follows: no water washing method is used for coagulation, and the water vapor consumption is 1.8 tons per ton of dry glue.
Example 2
The EPR concentration is 10 wt%, the glue solution temperature is 90 ℃, the pressure is 20atm, the glue solution is sent into a coil heater 2, the glue solution temperature is raised to 200 ℃, the pressure in the coil heater 2 is ensured to be 30atm at the moment, the glue solution is divided into two phases, the upper layer is a dilute solution phase, the EPR concentration is less than 0.5%, the lower layer is a concentrated solution phase, the EPR concentration is 33%, the dilute solution phase directly enters a dilute solution phase recovery system 6, and the concentrated solution phase enters a flash tank 3; the flash tank 3 is in adiabatic operation, the operating pressure is 1.3atm (absolute pressure), the operating liquid level of the polymer solution in the primary flash tank 3 is 1/3 of the total volume of the flash tank, after flash evaporation, the concentration of the polymer in the EPR glue solution is increased to 90 wt%, the temperature of the EPR glue solution is reduced to 94.3 ℃, the solvent enters the concentrated solution phase solvent recovery system 4 through an upper outlet of the flash tank 3, the concentrated glue solution enters the post-treatment system 5, and finally the removal of the solvent is completed.
The material consumption and energy consumption of the whole process are as follows: no water washing method is used for coagulation, and the water vapor consumption is 1.6 tons per ton of dry glue.
Example 3
The EPR concentration is 6 wt%, the glue solution temperature is 90 ℃, the pressure is 20atm, the glue solution is sent into a coil heater 2, the glue solution temperature is raised to 220 ℃, the pressure in the coil heater 2 is ensured to be 50atm at the moment, the glue solution is divided into two phases, the upper layer is a dilute solution phase, the EPR concentration is less than 1%, the lower layer is a concentrated solution phase, the EPR concentration is 31%, the dilute solution phase directly enters a dilute solution phase recovery system 6, and the concentrated solution enters a flash tank 3; the flash tank 3 is in adiabatic operation, the operating pressure is 1.3atm (absolute pressure), the operating liquid level of the polymer solution in the primary flash tank 3 is 1/3 of the total volume of the flash tank 3, after flash evaporation, the concentration of the polymer in the EPR glue solution is increased to 90 wt%, the temperature of the EPR glue solution is reduced to 95.0 ℃, the solvent enters the concentrated solution phase solvent recovery system 4 through an upper outlet of the flash tank 3, the concentrated glue solution enters the post-treatment system 5, and finally the removal of the solvent is completed.
The material consumption and energy consumption of the whole process are as follows: no water washing method is used for coagulation, and the water vapor consumption is 2.0 ton/ton of dry glue.
Example 4
The EPR concentration is 6 wt%, the glue solution temperature is 90 ℃, the pressure is 20atm, the glue solution is sent to a coil heater, the glue solution temperature is raised to 190 ℃, the pressure in the coil is ensured to be 30atm at the moment, the glue solution is divided into two phases, the upper layer is dilute solution, the EPR concentration is less than 1%, the lower layer is concentrated solution, the EPR concentration is 30%, the dilute solution phase directly enters a dilute solution phase recovery system 6, and the concentrated solution enters a flash tank 3; the flash tank is in adiabatic operation, the operating pressure is 1.6atm (absolute pressure), the operating liquid level of the polymer solution in the primary flash tank is 1/3 of the total volume of the flash tank, after flash evaporation, the concentration of the polymer in the EPR glue solution is increased to 90 wt%, the temperature of the EPR glue solution is reduced to 99.1 ℃, the solvent enters a concentrated solution phase solvent recovery system 4 through an upper outlet of the flash tank 3, the concentrated glue solution enters a post-treatment system 5, and finally the solvent is removed.
The material consumption and energy consumption of the whole process are as follows: no water washing method is used for coagulation, and the water vapor consumption is 2.2 tons per ton of dry glue.
Example 5
The concentration of butadiene rubber is 10 wt%, the temperature of the glue solution is 90 ℃, the pressure is 20atm, the glue solution is sent into a coil heater 2, the temperature of the glue solution is raised to 220 ℃, the pressure in the coil heater 2 is ensured to be 30atm at the moment, the glue solution is divided into two phases, the upper layer is a dilute solution phase, the concentration of butadiene rubber is less than 1%, the lower layer is a concentrated solution phase, the concentration of butadiene rubber is 37%, the dilute solution phase directly enters a dilute solution phase recovery system 6, and the concentrated solution enters a flash tank 3; the flash tank 3 is in adiabatic operation, the operation pressure is 1.3atm (absolute pressure), the operation liquid level of the polymer solution in the primary flash tank 3 is 1/3 of the total volume of the flash tank 3, after flash evaporation, the concentration of the polymer in the butene elastomer glue solution is increased to 95 wt%, the temperature of the glue solution is reduced to 93.4 ℃, the solvent enters a concentrated solution phase solvent recovery system 4 through an upper outlet of the flash tank 3, the concentrated glue solution enters a post-treatment system 5, and finally the removal of the solvent is completed.
The material consumption and energy consumption of the whole process are as follows: no water washing method is used for coagulation, and the water vapor consumption is 2.8 tons per ton of dry glue.
Example 6
The concentration of the ethylene-1-butene copolymer elastomer is 6 wt%, the temperature of the glue solution is 80 ℃, the pressure is 20atm, the glue solution is sent to a coil heater 2, the temperature of the glue solution is raised to 200 ℃, the pressure in the coil heater 2 is ensured to be 40atm at the moment, the glue solution is divided into two phases, the upper layer is a dilute solution phase, the concentration of the butene elastomer is less than 1%, the lower layer is a concentrated solution phase, the concentration of the butene elastomer is 35%, the dilute solution phase directly enters a dilute solution phase recovery system 6, and the concentrated solution enters a flash tank 3; the flash tank is in adiabatic operation, the operation pressure is 1.3atm (absolute pressure), the operation liquid level of the polymer solution in the primary flash tank 3 is 1/3 of the total volume of the flash tank 3, after flash evaporation, the concentration of the polymer in the ethylene-1-butene copolymer elastomer glue solution is increased to 93 wt%, the temperature of the glue solution is reduced to 130 ℃, the solvent enters a concentrated solution phase solvent recovery system 4 through an upper outlet of the flash tank 3, the concentrated glue solution enters a post-treatment system 5, and finally the removal of the solvent is completed.
The material consumption and energy consumption of the whole process are as follows: no water washing method is used for coagulation, and the water vapor consumption is 2.9 tons per ton of dry glue.
Example 7
The concentration of the ethylene-1-octene copolymer elastomer is 6 wt%, the temperature of the glue solution is 90 ℃, the pressure is 20atm, the glue solution is sent to a coil heater, the temperature of the glue solution is raised to 220 ℃, the pressure in the coil is ensured to be 40atm at the moment, the glue solution is divided into two phases, the upper layer is a dilute solution phase, the concentration of the ethylene-1-octene copolymer elastomer is less than 1%, the lower layer is a concentrated solution phase, the concentration of the ethylene-1-octene copolymer elastomer is 30%, the dilute solution phase directly enters a dilute solution phase recovery system 6, and the concentrated solution enters a flash tank 3; the flash tank 3 is in adiabatic operation, the operation pressure is 1.3atm (absolute pressure), the operation liquid level of the polymer solution in the primary flash tank 3 is 1/3 of the total volume of the flash tank 3, after flash evaporation, the concentration of the polymer in the octene elastomer glue solution is increased to 90 wt%, the temperature of the glue solution is reduced to 95.4 ℃, the solvent enters a concentrated solution phase solvent recovery system 4 through an upper outlet of the flash tank 3, the concentrated glue solution enters a post-treatment system 5, and finally the removal of the solvent is completed.
The material consumption and energy consumption of the whole process are as follows: no water washing method is used for coagulation, and the water vapor consumption is 1.9 ton/ton of dry glue.
Comparative example 1
The comparative example was carried out by a process similar to that of example 1, except that in the comparative example, a flash evaporation operation was not employed, but an EPR glue solution obtained by solution polymerization was directly sent to a conventional three-pot coagulation system, and the glue solution after coagulation and stripping was sent to a post-treatment system, thereby finally completing the removal of the solvent. The energy consumption and material consumption of the whole process are as follows: the consumption of solvent oil is 32 kg/ton dry glue, and the consumption of water vapor is 3.7 ton/ton dry glue.
The comparison shows that the method provided by the invention can obviously reduce the energy consumption and the steam consumption compared with the prior art when the solvent is removed from the polymer solution, thereby greatly reducing the production cost.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition. In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. A method for removing solvent from a polymer solution comprising:
(1) introducing the polymer solution into a coil heater for heating, so that the polymer solution is divided into a dilute solution phase and a concentrated solution phase in the coil heater;
(2) carrying out flash evaporation treatment on the concentrated solution phase obtained in the step (1) to remove the solvent in the concentrated solution phase;
the polymer solution remains in a full liquid phase during the heating.
2. The method of claim 1, wherein the polymer solution is a solution polymerization polymer solution comprising a polymer and a solvent; the concentration of the polymer in the polymer solution is 5 to 20 wt.%, preferably 6 to 15 wt.%.
3. The method of claim 1 or 2, wherein the polymer in the polymer solution comprises one or more of a rubber, a thermoplastic elastomer, and an acrylic resin, wherein the rubber preferably comprises one or more of a butadiene-styrene rubber, a butadiene rubber, an isoprene rubber, and a styrene-isoprene rubber, and the thermoplastic elastomer preferably comprises one or more of an ethylene- α -olefin copolymer, an ethylene- α -olefin-non-conjugated diene copolymer, a styrene-butadiene-styrene block copolymer, and a hydrogenated styrene-butadiene-styrene block copolymer.
4. The method of any one of claims 1-3, wherein the solvent in the polymer solution comprises at least one of cyclohexane, cycloheptane, toluene, benzene, xylene, n-hexane, n-heptane, n-octane, and n-decane.
5. The method according to any one of claims 1-4, wherein the polymer concentration of the dilute solution phase is less than 1 wt.%, and the polymer concentration of the concentrated solution phase is 20-50 wt.%.
6. The method according to any one of claims 1 to 5, wherein the coil heater is heated by steam, preferably at a temperature of 100 to 250 ℃, more preferably 150 to 220 ℃; and/or the pressure in the coil heater is 10-50 atm.
7. The method as claimed in any one of claims 1 to 6, wherein the polymer solution is introduced into a coil heater for heating treatment to cause the polymer solution to separate into a dilute solution phase and a concentrated solution phase in the coil, wherein the dilute solution phase is separated and discharged and the concentrated solution phase is introduced into step (2) for further treatment.
8. The method according to any one of claims 1 to 7, wherein the concentrated solution phase in step (2) is introduced into a flash apparatus to be subjected to a flash treatment, and the solvent in the concentrated solution phase is further removed; the flash evaporation device is preferably a flash evaporation tank, wherein the flash evaporation tank is operated in an adiabatic mode, and the operating pressure is 1.1-2.0 atm, preferably 1.3-1.8 atm; and controlling the operating liquid level of the concentrated solution phase in the flash tank to be 1/5-1/2, preferably 1/4-1/3 of the total volume of the flash tank.
9. A system for removing solvent from a polymer solution, comprising:
the coil heater is used for heating the polymer solution to enable the polymer solution to be divided into a dilute solution phase and a concentrated solution phase in the coil;
the device comprises a vertical pipe and a flash evaporation device, wherein the vertical pipe comprises an inlet, a first outlet and a second outlet, the inlet is connected with a coil heater, the first outlet is positioned at the top of the vertical pipe and used for separating a dilute solution phase, and the second outlet is positioned at the bottom of the vertical pipe and connected with the flash evaporation device;
and the flash evaporation device is used for carrying out flash evaporation treatment on the concentrated solution phase.
10. Use of the system of claim 9 for removing solvent from a polymer solution, comprising:
(1) introducing the polymer solution into a coil heater for heating treatment, so that the polymer solution is divided into a dilute solution phase and a concentrated solution phase in the coil and enters the vertical pipe through an inlet of the vertical pipe;
(2) the dilute solution phase is separated and discharged through a first outlet of the vertical pipe, and the concentrated solution phase enters a flash evaporation device through a second outlet of the vertical pipe;
(3) and carrying out flash evaporation treatment on the concentrated solution phase in a flash evaporation device to remove the solvent in the polymer solution.
CN201911033282.4A 2019-10-28 2019-10-28 Method and system for removing solvent in polymer solution Active CN112724281B (en)

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Citations (3)

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Publication number Priority date Publication date Assignee Title
US4623712A (en) * 1984-06-25 1986-11-18 Exxon Research & Engineering Co. Method for high temperature phase separation of solutions containing polymers
CN102786681A (en) * 2012-08-08 2012-11-21 金发科技股份有限公司 Polymer purification device and purification method
CN107614541A (en) * 2015-06-15 2018-01-19 埃克森美孚化学专利公司 Continuous solution polymerization method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4623712A (en) * 1984-06-25 1986-11-18 Exxon Research & Engineering Co. Method for high temperature phase separation of solutions containing polymers
CN102786681A (en) * 2012-08-08 2012-11-21 金发科技股份有限公司 Polymer purification device and purification method
CN107614541A (en) * 2015-06-15 2018-01-19 埃克森美孚化学专利公司 Continuous solution polymerization method

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