CN104558267A - Solid polymer degassing method and device - Google Patents
Solid polymer degassing method and device Download PDFInfo
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- CN104558267A CN104558267A CN201310482099.9A CN201310482099A CN104558267A CN 104558267 A CN104558267 A CN 104558267A CN 201310482099 A CN201310482099 A CN 201310482099A CN 104558267 A CN104558267 A CN 104558267A
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Abstract
The invention provides a solid polymer degassing method. The solid polymer degassing method comprises the following steps: i) performing first-stage degassing: providing a first-stage degassing medium and enabling the first-stage degassing medium to be in reverse contact with a solid polymer to be degassed in a first-stage degassing bin to obtain a first-stage degassed polymer; ii) performing second-stage degassing: introducing the first-stage degassed polymer obtained in the step i) into a second-stage degassing bin to perform periodic pulse treatment, namely providing a second-stage degassing medium to the second-stage degassing bin and enabling the second-stage degassing medium to be in reverse contact with the first-stage degassed polymer in the second-stage degassing bin to obtain a second degassed polymer; iii) performing third-stage degassing: providing a third-stage degassing medium and enabling the third-stage degassing medium to be in reverse contact with the second degassed polymer in a third-stage degassing bin to obtain a final degassed polymer. The invention further provides a solid polymer degassing device for the method.
Description
Technical field
The present invention relates to solid polymer processing technology field, be specifically related to the method and apparatus of solvent in a kind of gas, particularly polyolefin resin that utilize gas-phase reaction material, gaseous hydrocarbons and rare gas element to remove in solid polymer and unreacted monomer.
Background technology
In the polymerization, according to the difference of technique and physical property, polymerisate can present different states, wherein more typically polymkeric substance with the form of solid powdery from reactor discharging, as vapor phase process polyolefin process.When solid polymer is discharged from reactor, often residual solvent and unreacted monomer in polymer powders, for gas-phase fluidized bed production of linear Low Density Polyethylene (LLDPE) technique, containing unreacted monomer, comonomer and condensing agent in LLDPE powder, as ethene (C
2h
4), propylene (C
3h
6), butylene (C
4h
8), hexene (C
6h
12), hydrogen (H
2) and iso-pentane (C
5h
12) etc., these impurity must be removed in degassed dehumidification system, object ensures that the safety of the downstream unit operations such as granulation and wind send and polyolefin products store the safety of transporting, and reduces the consumption of comonomer and condensing agent to greatest extent, reduce product peculiar smell.
Typical solid polymer degas method purges polymer powders in a reservoir with rare gas element.US Patent No. 4372758 discloses a kind of method removing unreacted monomer from polyolefin resin, the solid polymer of discharging from reactive system enters degassing container from top, Purge gas enters bottom degassing container simultaneously, contact with solid polymer is reverse, unreacted gaseous monomer residual in polymkeric substance is removed in contact process, described Purge gas contains nitrogen, and oxygen-free gas.The discharge gas that this patent also mentions degassing container generation can return as powder carry gas, or returns degassing container as Purge gas.Publication number is that the Chinese invention patent of CN88102601A discloses a kind of polymkeric substance segmentation degas method, resin first contacts with pure nitrogen gas is reverse, contact with steam-laden nitrogen is reverse again, the effect of water vapour makes Ziegler-Natta catalyst in solid polyolefin hydrocarbon resin and organo-metallic catalyst inactivation, continues reaction after preventing polymkeric substance from flowing out degassing container.
Utilize nitrogen to be known as degassed gas processing solid polymer, and widely apply aborning.Except nitrogen, concrete polymkeric substance is degassed adopts other gases or gaseous mixture, as carbonic acid gas, aliphatic saturated hydrocarbon, gaseous hydrocarbon mixture etc.US Patent No. 5376742 discloses and utilizes fluidized-bed reactor eluting gas (recycle gas) as degassed medium, degassed for polyolefin resin, heavy hydrocarbon before degassed in circulation gas is separated from gas, the deficiency of this method is the condition of degassed Medium Dependent in reactor, and pressure and composition etc. cannot stability contorting.European patent EP 0127253A1 discloses a kind of using reactant gases or a kind of monomer as the polyethylene powder degas method of degassed medium, discharge gas Returning reactor, this avoid the process using rare gas element (as nitrogen etc.) and discharge gas Separation and Recovery, the shortcoming of this method is that a large amount of discharge gas Returning reactors will impact the stable operation of reactor, simultaneously degassed complete after polyethylene powder in still containing reaction monomers, the existence of reaction monomers can affect the safety of lower procedure and powder storage, affect quality product, and increase raw material consumption and production cost.Notification number is that the Chinese invention patent of CN100537609C discloses a kind of propane that utilizes as the polyvinyl resin degas method of degassed medium, discharge gas is through two-phase seperation, recovered ethylene and high boiling point alkene, propane returns and carries out the degassed of polyolefin particles, the shortcoming of this method be degassed after polyolefin particles in containing propane, downstream process is had an impact.
Except above-mentioned use inert gas purge solid polymer comes except the method for imurity-removal component, the degassed method that can also adopt other, in decompression tank, such as carry out the method for after polymerization, as US Patent No. 6465608B1 discloses with polymerization single polymerization monomer as degassed medium, carry out reducing pressure and degassed process in fluidized-bed, there is after polymerization simultaneously, the partial reaction conversion of monomer removed can be become product by this method, improve degassing efficiency, but the quality product of after polymerization is difficult to control, and adds equipment and running cost.Degassed can also adopt the condition not passing into nitrogen (or comprising water vapour) medium under, such as notification number is that the Chinese invention patent of CN1733810A discloses a kind of polypropylene powder after-treating method, under mechanical stirring or the dual function in mechanical stirring and heating (comprise and adopt rotary dryer), or with the recovery hydro carbons circulated as blowing medium (comprising fluidisation or unfluidized state), or under the condition under low pressure left standstill for a long time, quite a few hydro carbons in polymer powders is removed out.
In sum, there is the shortcomings such as degassing efficiency is not high, energy consumption is large, raw material consumption is large, environment is unfriendly in existing solid polymer degas method, therefore, invent that a kind of degassing efficiency is high, energy-conservation and eco-friendly solid polymer degas method has very high economic interests and realistic meaning.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the method and apparatus that a kind of solid polymer is degassed is provided.Specifically, a kind of method and apparatus solvent existed in pulverulent solids polymkeric substance and unreacted monomer removed is related to.Described solvent refers to needed for reaction process and the material of chemical reaction does not occur, as the condensing agent in organic solvent, water, the aqueous solution, vapour phase polymerization.
The present invention is preferably applicable to the degassed of polyolefin resin, but be not limited to polyolefine, the all available method disclosed by the invention of any granular solid polymer is degassed, and the production technique of polymkeric substance comprises vapour phase polymerization, solution polymerization, mass polymerization, letex polymerization etc.
The method that solid polymer is degassed, comprises the following steps:
I) first step is degassed: solid polymer to be de-gassed is passed into first step degassing cabin, there is provided the degassed medium of the first step to first step degassing cabin, make the degassed medium of the first step carry out with solid polymer to be de-gassed reversely contacting thus obtaining first step degassed polymer in first step degassing cabin, then will obtain first row venting and discharge from first step degassing cabin through the first step is degassed;
Ii) the second stage is degassed: by step I) first step degassed polymer that obtains passes in the degassing cabin of the second stage and carries out the process of recurrent pulses formula and obtain the second degassed polymer, the process of described recurrent pulses formula comprises provides the degassed medium in the second stage to second stage degassing cabin, make the degassed medium in the described second stage carry out reverse contact with first step degassed polymer in the degassing cabin of the second stage, then the second row venting that obtain degassed through the second stage is discharged from the degassing cabin of the second stage;
Iii) the third stage is degassed: by step I i) second stage degassed polymer that obtains passes in third stage degassing cabin, there is provided the degassed medium of the third stage to third stage degassing cabin, make the degassed medium of the described third stage in third stage degassing cabin, carry out reverse contact with the second degassed polymer and obtain final degassed polymer, then discharge through degassed the 3rd discharge gas obtained of the third stage from third stage degassing cabin.
Described recurrent pulses formula process is that continuous several times passes into the degassed medium in the second stage instantaneously and discharges second row venting instantaneously in the degassing cabin of the second stage.
In a preferred embodiment of the present invention, described solid polymer is polyolefine.
In a preferred embodiment of the present invention, the degassed medium of the described first step, the second degassed medium and the 3rd degassed medium are at least one in gaseous reactant material, gaseous hydrocarbons and the gaseous inert gas after fresh gaseous reactant material, recycling.
In a preferred embodiment of the present invention, described first row is exitted, second row is exitted and the 3rd discharge gas is partially recycled or be all expelled to flare system.
In a preferred embodiment of the present invention, step 2) in, provide to described pulsed the degassed medium in the second stage within 1-60 second, the pressure of second stage degassing cabin can be risen to 0.5-2.0MPa, be preferably 0.5-1.0MPa; Described pulsed ground discharge through the degassed second row venting obtained in the second stage can within 1-60 second by the Pressure Drop of second stage degassing cabin to 0.15-0.45MPa, be preferably 0.2-0.4MPa;
In a preferred embodiment of the present invention, in the degassing cabin of the second stage to first step degassed polymer carry out 1-10 step ii) described in the process of recurrent pulses formula.
In a preferred embodiment of the present invention, the period interval time between the process of each recurrent pulses formula is 0-600 second, is preferably 5-60 second.
Preferably, in the process of described recurrent pulses formula, during when degassed for second stage medium is provided in the degassing cabin of the described second stage and by the pressure increase of second stage degassing cabin to high pressure (0.5 ~ 2.0MPa), keep the high pressure 1-1000 second of described second stage degassing cabin, preferred 5-60 second, the time of this maintenance high pressure becomes pulse width.And, advantageously, when the second stage to be discharged when gas is discharged from the degassing cabin of the second stage and by the pressure drop of second stage degassing cabin to low pressure (0.15 ~ 0.45MPa), maintain the low pressure 0-600 second of described second stage degassing cabin, preferred 5-60 second, the time of this maintenance low pressure is called period interval time.Subsequently, recurrent pulses formula process next time is then carried out.
Described gaseous hydrocarbons is selected from least one in methane, ethane, propane, butane, pentane, iso-pentane, hexane, ethene, propylene, butylene, amylene and hexene.
Described rare gas element is selected from least one in nitrogen, carbonic acid gas, neon or argon gas, is preferably nitrogen.
Present invention also offers a kind of solid polymer de-gassing vessel, comprise
For the treatment of the first step degassing cabin that the first step is degassed;
The degassed medium providing unit of the first step, it is connected with first step degassing cabin, for providing degassed medium for first step degassing cabin;
Second stage degassing cabin, it is connected with first step degassing cabin, for accepting the degassed product of the first step through the degassed process of the first step from first step degassing cabin, and carries out the degassed process in the second stage to the degassed product of the described first step;
The degassed medium providing unit in the second stage, it is connected with second stage degassing cabin, for the degassed medium in the second stage in degassed for second stage medium providing unit is provided to second stage degassing cabin; Described second stage degassing cabin is provided with exhaust unit, makes the degassed second row venting obtained through the second stage in the degassing cabin of the described second stage can discharge described second stage degassing cabin;
Third stage degassing cabin, it is connected with second stage degassing cabin, for accepting the second degassed product of the degassed process through the second stage from second stage degassing cabin, and carries out the degassed process of the third stage to described second degassed product;
The degassed medium providing unit of the third stage, it is connected with third stage degassing cabin, for providing the third stage degassed medium for third stage degassing cabin.
In a preferred embodiment of the present invention, described de-gassing vessel also comprises:
Product surge tank, it is connected with first step degassing cabin, for the polymer product providing band degassed for first step degassing cabin;
Product discharge tank, it is connected with product surge tank, for providing the polymer product in autoreactor for product surge tank.
Beneficial effect of the present invention:
Method and apparatus of the present invention can remove varsol or the unreacted monomer of solid polymer particle surface and external diffusion absorption and be dissolved in the alkene of polymeric inner.
Method and apparatus of the present invention compares traditional method can reduce degassing time, reduce the usage quantity of the degassed medium of postorder, and can efficient recovery solvent and unreacted monomer, ensure to there is the safety that lower procedure and powder store very strong realistic meaning and using value.
Accompanying drawing explanation
Fig. 1 is the structural representation of solid polymer de-gassing vessel of the present invention;
Fig. 2 is the process flow sheet of solid polymer degas method of the present invention;
In figure, 1-fluidized-bed reactor, 2-product discharge tank, 3-product surge tank, 4-first step degassing cabin, 5-second stage degassing cabin, 6-third stage degassing cabin, the 7-first step degassed medium providing unit, the 8-second stage degassed medium providing unit, the degassed medium providing unit of the 9-third stage.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in detail, but scope of the present invention is not limited to following examples.
As shown in Figure 1, the degassed device of solid polymer of the present invention its be connected with fluidized-bed reactor 1, described polymer degassing plant comprises: product discharge tank 2, product surge tank 3, for the treatment of the degassed first step degassing cabin 4 of the first step, for the treatment of the degassed second stage degassing cabin 5 in the second stage with for the treatment of the degassed third stage degassing cabin 6 of the third stage, wherein:
The degassed medium providing unit of the first step is connected with first step degassing cabin 4, for providing degassed medium for first step degassing cabin 4;
Second stage degassing cabin, it is connected with first step degassing cabin 4, for accepting the degassed product of the first step through the degassed process of the first step from first step degassing cabin 4, and carries out the degassed process in the second stage to the degassed product of the described first step;
The degassed medium providing unit in the second stage, it is connected with second stage degassing cabin 5, for the degassed medium in the second stage in degassed for second stage medium providing unit 8 can be provided to second stage degassing cabin 5; Described second stage degassing cabin 5 is also provided with exhaust unit (not shown), makes the degassed second row venting obtained through the second stage in described second stage degassing cabin 5 can discharge to pulsed described second stage degassing cabin 5;
Third stage degassing cabin 6, it is connected with second stage degassing cabin 5, for accepting the second degassed product of the degassed process through the second stage from second stage degassing cabin 5, and carries out the degassed process of the third stage to described second degassed product;
The degassed medium providing unit 9 of the third stage, it is connected with third stage degassing cabin 6, for providing the third stage degassed medium for third stage degassing cabin 6.
As depicted in figs. 1 and 2, a kind of method that solid polymer is degassed, comprises the following steps:
1) first step is degassed: solid polymer to be de-gassed is passed into first step degassing cabin 4, there is provided the degassed medium of the first step to first step degassing cabin 4, make the degassed medium of the first step carry out with solid polymer to be de-gassed reversely contacting thus obtaining first step degassed polymer in first step degassing cabin 4, then will obtain first row venting and discharge from first step degassing cabin 4 through the first step is degassed;
2) second stage is degassed: first step degassed polymer step 1) obtained passes in second stage degassing cabin 5, carry out the process of recurrent pulses formula and obtain the second degassed polymer, the process of described recurrent pulses formula comprises provides the degassed medium in the second stage to second stage degassing cabin 5, make the degassed medium in the described second stage, within 1-60 second, the pressure of second stage degassing cabin 5 risen to 0.5-2.0MPa, and reverse contact is carried out with solid polymer in second stage degassing cabin 5, then the second row venting that obtain degassed through the second stage is discharged from second stage degassing cabin 5, to make the Pressure Drop of second stage degassing cabin 5 within 1-60 second to 0.15-0.45MPa,
3) third stage is degassed: by step 2) second stage degassed polymer that obtains passes in third stage degassing cabin 6, there is provided the degassed medium of the third stage to third stage degassing cabin 6, make the degassed medium of the described third stage in third stage degassing cabin 6, carry out reverse contact with the second degassed polymer and obtain final degassed polymer, then discharge through degassed the 3rd discharge gas obtained of the third stage from third stage degassing cabin 6.
Described recurrent pulses formula process is that continuous several times passes into the degassed medium in the second stage instantaneously and discharges second row venting instantaneously in second stage degassing cabin 5; Described solid polymer is polyolefine; The degassed medium of the described first step, the second degassed medium and the 3rd degassed medium be fresh gaseous reactant material, recycling after gaseous reactant material, gaseous hydrocarbons or gaseous inert gas in one or several.Described first row venting, second row venting and the 3rd discharge gas are partially recycled or be all expelled to flare system.
Described rare gas element is the combination of one or more in nitrogen, carbonic acid gas, neon or argon gas.Described rare gas element is nitrogen.
Embodiment 1
Adopt said apparatus, with gas-phase fluidized bed explained hereafter Ethylene/Butylene copolymerization linear low density polyethylene (LLDPE) product, the temperature of reaction of fluidized-bed reactor 1 88 DEG C, reaction pressure 2.1MPa, adopts non-condensing operation.In output streams, each composition flow rate is: LLDPE powder 40t/h, nitrogen 200kg/h, hydrogen 3kg/h, ethene 2600kg/h, 1-butylene 2500kg/h.Wherein ethene and 1-butylene are unreacted monomer, solvent-free.First the LLDPE product of discharging from fluidized-bed reactor 1 enters product discharge tank 2 under the drive of delivering gas, and enter product surge tank 3 subsequently, pressure is 0.7MPa, removes the hydro carbons of part polyethylene particle surface absorption, enters three grades of degasification process subsequently.The degassed medium of the first step adopts nitrogen, the flow of the degassed medium of the first step is 200kg/h, and reverse contact is carried out with solid polymer in first step degassing cabin 4, remove the unreacted monomer of polyethylene particle surface and external diffusion absorption, discharge first row venting from first step degassing cabin 4 top; Second degassed medium is the gas mixture of nitrogen and ethene, the flow of the second degassed medium is 500kg/h, in second stage degassing cabin 5, pass into the degassed medium in the second stage under the time conditions of 1 second makes the pressure of second stage degassing cabin 5 increase to 0.5MPa, and discharge under the time conditions of 1 second second row venting make the pressure of second stage degassing cabin 5 reduce to 0.4MPa, carry out recurrent pulses formula so process 10 times, pulse width 1s, the period interval time of operation is 5s.Second degassed medium carries out reverse contact with solid polymer in second stage degassing cabin 5, under the large pressure reduction that the process of recurrent pulses formula causes, remove polyethylene duct and be dissolved in the alkene of polymeric inner, discharge second row venting from second stage degassing cabin 5 top; 3rd degassed medium adopts nitrogen, and the flow of the 3rd degassed medium is 500kg/h, and carries out reverse contact with solid polymer in third stage degassing cabin 6, removes the hydro carbons of residue absorption, discharges the 3rd discharge gas from third stage degassing cabin 6 top.In solid polymer particles after degassed through three grades, foreign matter content is in 20ppm(quality) below.
At identical conditions, compared with being 100min with traditional technology degassing time, total purge time of the degassed medium of the present embodiment is 90min, decreases 10%.
Embodiment 2
Adopt the device identical with embodiment 1, with gas-phase fluidized bed explained hereafter polyethylene-hexene copolymerization linear low density polyethylene (LLDPE) product, the temperature of reaction of fluidized-bed polymerization reactor 1 88 DEG C, reaction pressure 2.1MPa, adopts non-condensing operation.In output streams, each composition flow rate is: LLDPE powder 40t/h, nitrogen 180kg/h, hydrogen 3kg/h, ethene 2600kg/h, hexene 2000kg/h.Wherein ethene and hexene are unreacted monomer, solvent-free.First the LLDPE product of discharging from fluidized-bed reactor 1 enters product discharge tank 2 under the drive of delivering gas, and next enters product surge tank 3, removes the hydro carbons of part polyethylene particle surface absorption, enters three grades of degasification process subsequently.The degassed medium of the first step adopts nitrogen, the flow of the degassed medium of the first step is 300kg/h, and reverse contact is carried out with solid polymer in first step degassing cabin 4, remove the unreacted monomer of polyethylene particle surface and external diffusion absorption, discharge first row venting from first step degassing cabin 4 top; Second degassed medium is nitrogen, the flow of the second degassed medium is 550kg/h, in second stage degassing cabin 5, pass into the degassed medium in the second stage under the time conditions of 60 seconds makes the pressure of second stage degassing cabin 5 increase to 0.5MPa, and under the time conditions of 60 second discharge second row venting make the pressure of second stage degassing cabin 5 reduce to 0.2MPa, carry out recurrent pulses formula like this process 4 times, pulse width is 5s, and the period interval time of operation is 20 seconds.Second degassed medium carries out reverse contact with solid polymer in second stage degassing cabin 5, under the large pressure reduction that the process of recurrent pulses formula causes, remove polyethylene duct and be dissolved in the alkene of polymeric inner, discharge second row venting from second stage degassing cabin 5 top; 3rd degassed medium adopts nitrogen, and the flow of the 3rd degassed medium is 550kg/h, and carries out reverse contact with solid polymer in third stage degassing cabin 6, removes the hydro carbons of residue absorption, discharges the 3rd discharge gas from third stage degassing cabin 6 top.In solid polymer particles after degassed through three grades, foreign matter content is in 20ppm(quality) below.
At identical conditions, compared with being 140min with the degassing time of traditional technology, total purge time of the degassed medium of the present embodiment is 95min, decreases 32%.
Embodiment 3
Adopt the device identical with embodiment 1, with gas-phase fluidized bed explained hereafter Ethylene/Butylene copolymerization linear low density polyethylene (LLDPE) product, the temperature of reaction of fluidized-bed reactor 1 88 DEG C, reaction pressure 2.1MPa, adopts condensation operation.In output streams, each composition flow rate is: LLDPE powder 40t/h, nitrogen 160kg/h, hydrogen 3kg/h, ethene 2580kg/h, 1-butylene 2300kg/h, iso-pentane 2500kg/h.Wherein ethene and 1-butylene are unreacted monomer, and iso-pentane is solvent.First the LLDPE product of discharging from fluidized-bed reactor 1 enters product discharge tank 2 under the drive of delivering gas, and next enters product surge tank 3, removes the hydro carbons of part polyethylene particle surface absorption, enters three grades of degasification process subsequently.The degassed medium of the first step adopts nitrogen, the flow of the degassed medium of the first step is 300kg/h, and reverse contact is carried out with solid polymer in first step degassing cabin 4, remove varsol or the unreacted monomer of polyethylene particle surface and external diffusion absorption, discharge first row venting from first step degassing cabin 4 top; Second degassed medium is nitrogen, the flow of the second degassed medium is 550kg/h, in second stage degassing cabin 5, pass into the degassed medium in the second stage under the time conditions of 30 seconds makes the pressure of second stage degassing cabin 5 increase to 1.0MPa, and discharge under the time conditions of 30 seconds second row venting make the pressure of second stage degassing cabin 5 reduce to 0.3MPa, carry out recurrent pulses formula like this process 5 times, pulse width is 40 seconds, and the interval time of operation is 0 second.Second degassed medium carries out reverse contact with solid polymer in second stage degassing cabin 5, under the large pressure reduction that the process of recurrent pulses formula causes, remove polyethylene duct and be dissolved in the alkene of polymeric inner, discharge second row venting from second stage degassing cabin 5 top; 3rd degassed medium adopts nitrogen, and the flow of the 3rd degassed medium is 550kg/h, and carries out reverse contact with solid polymer in third stage degassing cabin 6, removes the hydro carbons of residue absorption, discharges the 3rd discharge gas from third stage degassing cabin 6 top.In solid polymer particles after degassed through three grades, foreign matter content is in 20ppm(quality) below.
At identical conditions, compared with being 120min with traditional technology degassing time, total purge time of the degassed medium of the present embodiment is 85min, decreases 29%.
Embodiment 4
Adopt the device identical with embodiment 1, with gas-phase fluidized bed explained hereafter polyethylene-hexene copolymerization linear low density polyethylene (LLDPE) product, the temperature of reaction of fluidized-bed reactor 1 88 DEG C, reaction pressure 2.1MPa, adopts condensation operation.In output streams, each composition flow rate is: LLDPE powder 40t/h, nitrogen 160kg/h, hydrogen 3kg/h, ethene 2580kg/h, iso-pentane 2500kg/h, hexene 2000kg/h.Wherein ethene and hexene are unreacted monomer, and iso-pentane is solvent.First the LLDPE product of discharging from fluidized-bed reactor 1 enters product discharge tank 2 under the drive of delivering gas, and next enters product surge tank 3, removes the hydro carbons of part polyethylene particle surface absorption, enters three grades of degasification process subsequently.The degassed medium of the first step adopts nitrogen, the flow of the degassed medium of the first step is 300kg/h, and reverse contact is carried out with solid polymer in first step degassing cabin 4, remove varsol or the unreacted monomer of polyethylene particle surface and external diffusion absorption, discharge first row venting from first step degassing cabin 4 top; Second degassed medium is the gas mixture of nitrogen and ethene, the flow of the second degassed medium is 550kg/h, in second stage degassing cabin 5, pass into the degassed medium in the second stage under the condition of 10 seconds makes the pressure of second stage degassing cabin 5 increase to 0.7MPa, and discharge under the condition of 10 seconds second row venting make the pressure of second stage degassing cabin 5 reduce to 0.4MPa, carry out recurrent pulses formula like this process 1 time, pulse width is 60 seconds, and the interval time of operation is 60 seconds.Second degassed medium carries out reverse contact with solid polymer in second stage degassing cabin 5, under the large pressure reduction that the process of recurrent pulses formula causes, remove polyethylene duct and be dissolved in the alkene of polymeric inner, discharge second row venting from second stage degassing cabin 5 top; 3rd degassed medium adopts nitrogen, and the flow of the 3rd degassed medium is 550kg/h, and carries out reverse contact with solid polymer in third stage degassing cabin 6, removes the hydro carbons of residue absorption, discharges the 3rd discharge gas from third stage degassing cabin 6 top.In solid polymer particles after degassed through three grades, foreign matter content is in 20ppm(quality) below.
At identical conditions, traditional technology degassing time is that 130min compares, and total purge time of the degassed medium of the present embodiment is 87min, decreases 33%.
Claims (10)
1. the method that solid polymer is degassed, comprises the following steps:
I) first step is degassed: solid polymer to be de-gassed is passed into first step degassing cabin, there is provided the degassed medium of the first step to first step degassing cabin, make the degassed medium of the first step carry out with solid polymer to be de-gassed reversely contacting thus obtaining first step degassed polymer in first step degassing cabin, then will obtain first row venting and discharge from first step degassing cabin through the first step is degassed;
Ii) the second stage is degassed: by step I) first step degassed polymer that obtains passes in the degassing cabin of the second stage and carries out the process of recurrent pulses formula and obtain the second degassed polymer, the process of described recurrent pulses formula comprises provides the degassed medium in the second stage to second stage degassing cabin, make the degassed medium in the described second stage carry out reverse contact with first step degassed polymer in the degassing cabin of the second stage, then the second row venting that obtain degassed through the second stage is discharged from the degassing cabin of the second stage;
Iii) the third stage is degassed: by step I i) second stage degassed polymer that obtains passes in third stage degassing cabin, there is provided the degassed medium of the third stage to third stage degassing cabin, make the degassed medium of the described third stage in third stage degassing cabin, carry out reverse contact with the second degassed polymer and obtain final degassed polymer, then discharge through degassed the 3rd discharge gas obtained of the third stage from third stage degassing cabin.
2. method according to claim 1, is characterized in that, described solid polymer is polyolefine.
3. method according to claim 1 and 2, it is characterized in that, the degassed medium of the described first step, the second degassed medium and the 3rd degassed medium are at least one in gaseous reactant material, gaseous hydrocarbons and the gaseous inert gas after fresh gaseous reactant material, recycling.
4. the method according to any one of claim 1-3, is characterized in that, is exitted by described first row, second row is exitted and the 3rd discharge gas is partially recycled or be all expelled to flare system.
5. the method according to any one of claim 1-4, is characterized in that, step 2) in provide the degassed medium in the described second stage to make it possible to, within 1-60 second, the pressure of second stage degassing cabin is risen to 0.5-2.0MPa, be preferably 0.5-1.0MPa; Described discharge described through the second stage the degassed second row venting obtained to make it possible to the Pressure Drop of second stage degassing cabin within 1-60 second, to 0.15-0.45MPa, be preferably 0.2-0.4MPa.
6. the method according to any one of claim 1-5, is characterized in that, in the degassing cabin of the second stage to first step degassed polymer carry out 1-10 step ii) described in the process of recurrent pulses formula.
7. the method according to any one of claim 1-6, is characterized in that, step 2) described in the pulse width of pulse be 1-1000 second, be preferably 5-60 second.
8. the method according to any one of claim 1-7, is characterized in that, described gaseous hydrocarbons is selected from least one in methane, ethane, propane, butane, pentane, iso-pentane, hexane, ethene, propylene, butylene, amylene and hexene.
9. a solid polymer de-gassing vessel, comprises
For the treatment of the first step degassing cabin that the first step is degassed;
The degassed medium providing unit of the first step, it is connected with first step degassing cabin, for providing degassed medium for first step degassing cabin;
Second stage degassing cabin, it is connected with first step degassing cabin, for accepting the degassed product of the first step through the degassed process of the first step from first step degassing cabin, and carries out the degassed process in the second stage to the degassed product of the described first step;
The degassed medium providing unit in the second stage, it is connected with second stage degassing cabin, for the degassed medium in the second stage in degassed for second stage medium providing unit is provided to second stage degassing cabin; Described second stage degassing cabin is provided with exhaust unit, makes the degassed second row venting obtained through the second stage in the degassing cabin of the described second stage can discharge described second stage degassing cabin;
Third stage degassing cabin, it is connected with second stage degassing cabin, for accepting the second degassed product of the degassed process through the second stage from second stage degassing cabin, and carries out the degassed process of the third stage to described second degassed product;
The degassed medium providing unit of the third stage, it is connected with third stage degassing cabin, for providing the third stage degassed medium for third stage degassing cabin.
10. device according to claim 9, is characterized in that, described de-gassing vessel also comprises:
Product surge tank, it is connected with first step degassing cabin, for the polymer product providing band degassed for first step degassing cabin;
Product discharge tank, it is connected with product surge tank, for providing the polymer product in autoreactor for product surge tank.
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| CN110734558A (en) * | 2018-07-18 | 2020-01-31 | 高煦 | Post-treatment method for polypropylene and polyethylene powder |
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| EP0127253A1 (en) * | 1983-04-29 | 1984-12-05 | Mobil Oil Corporation | Process for removal of residual monomers from ethylene copolymers |
| US6465608B1 (en) * | 1999-05-18 | 2002-10-15 | Basell Polyolefine Gmbh | Method for drying and degassing polyolefins |
| CN102161715A (en) * | 2011-01-31 | 2011-08-24 | 浙江大学 | Method and device for degassing solid polymer and recovering effluent gas |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0127253A1 (en) * | 1983-04-29 | 1984-12-05 | Mobil Oil Corporation | Process for removal of residual monomers from ethylene copolymers |
| US6465608B1 (en) * | 1999-05-18 | 2002-10-15 | Basell Polyolefine Gmbh | Method for drying and degassing polyolefins |
| CN102161715A (en) * | 2011-01-31 | 2011-08-24 | 浙江大学 | Method and device for degassing solid polymer and recovering effluent gas |
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| CN110734558A (en) * | 2018-07-18 | 2020-01-31 | 高煦 | Post-treatment method for polypropylene and polyethylene powder |
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