CN104558267B - A kind of method and apparatus of solid polymer degassing - Google Patents
A kind of method and apparatus of solid polymer degassing Download PDFInfo
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- CN104558267B CN104558267B CN201310482099.9A CN201310482099A CN104558267B CN 104558267 B CN104558267 B CN 104558267B CN 201310482099 A CN201310482099 A CN 201310482099A CN 104558267 B CN104558267 B CN 104558267B
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- 238000007872 degassing Methods 0.000 title claims abstract description 310
- 229920000642 polymer Polymers 0.000 title claims abstract description 88
- 239000007787 solid Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 47
- 230000000306 recurrent effect Effects 0.000 claims abstract description 18
- 238000012545 processing Methods 0.000 claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 53
- 239000007789 gas Substances 0.000 claims description 44
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 229930195733 hydrocarbon Natural products 0.000 claims description 18
- 150000002430 hydrocarbons Chemical class 0.000 claims description 18
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 17
- -1 propylene, butylene Chemical group 0.000 claims description 16
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 11
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229920000098 polyolefin Polymers 0.000 claims description 10
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 claims description 7
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 claims description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000001273 butane Substances 0.000 claims description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 239000000178 monomer Substances 0.000 description 21
- 239000004698 Polyethylene Substances 0.000 description 17
- 108010066278 cabin-4 Proteins 0.000 description 17
- 229920000573 polyethylene Polymers 0.000 description 17
- 229920000092 linear low density polyethylene Polymers 0.000 description 15
- 239000004707 linear low-density polyethylene Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 11
- 239000012071 phase Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 8
- 239000011261 inert gas Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 150000001336 alkenes Chemical class 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000010926 purge Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000013032 Hydrocarbon resin Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000011954 Ziegler–Natta catalyst Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 238000012685 gas phase polymerization Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920006270 hydrocarbon resin Polymers 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000010094 polymer processing Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a kind of method of solid polymer degassing, comprise the following steps：i）The first order deaerates：First order degassing medium is provided, makes first order degassing medium with solid polymer to be de-gassed inversely contact so as to obtain first order degassed polymer in first order degassing cabin；ii）The second level deaerates：By step i）Obtained first order degassed polymer is passed through progress recurrent pulses formula processing in the degassing cabin of the second level, medium is deaerated to second level degassing cabin including providing the second level, makes the second level degassing medium carry out inversely contacting to obtain the second degassed polymer with first order degassed polymer in the degassing cabin of the second level；iii）The third level deaerates：Third level degassing medium is provided, makes the third level degassing medium carry out inversely contacting to obtain final degassed polymer with the second degassed polymer in third level degassing cabin.Present invention also offers a kind of solid polymer degasser for the above method.
Description
Technical field
The present invention relates to solid polymer processing technology field, and in particular to one kind utilizes gas phase reaction material, gaseous hydrocarbon
Gas in class and inert gas removing solid polymer, the particularly method of the solvent in vistanex and unreacted monomer
And device.
Background technology
In the polymerization, according to technique and the difference of physical property, different states can be presented in polymerizate, wherein comparing allusion quotation
Type is that polymer is discharged in the form of solid powdery from reactor, such as vapor phase method polyolefin process.Solid polymer is from anti-
When answering the device to discharge, often residual solvent and unreacted monomer in polymer powders are low close with gas-phase fluidized bed production of linear
Spend polyethylene（LLDPE）Exemplified by technique, unreacted monomer, comonomer and condensing agent, such as ethene are contained in LLDPE powders
（C2H4）, propylene（C3H6）, butylene（C4H8）, hexene（C6H12）, hydrogen（H2）And isopentane（C5H12）Must be Deng, these impurity
Removed in degassing drying system, it is therefore an objective to the safety of the downstream units such as guarantee is granulated and wind is sent operation and polyolefin products storage
The safety of transport is deposited, reduces the consumption of comonomer and condensing agent to greatest extent, reduces product peculiar smell.
Typical solid polymer degassing method is to purge polymer powders in a reservoir with inert gas.United States Patent (USP)
US4372758 discloses a kind of method that unreacted monomer is removed from vistanex, gathers from the solid of reaction system discharge
Compound enters degassing container from top, while purification gas enters from degassing container bottom, is inversely contacted with solid polymer,
The unreacted gaseous monomer remained in polymer is removed in contact process, described purification gas contains nitrogen, and not oxygenous.
The patent is also mentioned that discharge gas can return to as powder carry gas caused by degassing container, or returns and take off as purification gas
Gas container.Publication No. CN88102601A Chinese invention patent discloses a kind of polymer segmentation degassing method, resin first with
Pure nitrogen gas inversely contacts, then is inversely contacted with steam-laden nitrogen, and the effect of vapor makes in solid polyolefin hydrocarbon resin
Ziegler-Natta catalyst and organo-metallic catalyst inactivation, continue to react after preventing polymer outflow degassing container.
It is known to use nitrogen as degassing gas treatment solid polymer, and widely used in production.
In addition to nitrogen, specific polymer degassing can use other gases or admixture of gas, such as carbon dioxide, aliphatic saturated hydrocarbon, gas
State hydrocarbon mixture etc..United States Patent (USP) US5376742, which is disclosed, utilizes fluidized-bed reactor eluting gas（Recyclegas）As de-
Gas medium, deaerated for vistanex, the heavy hydrocarbon before degassing in circulating air separates from gas, and the deficiency of the method is de-
For gas medium dependent on the condition in reactor, pressure and composition etc. can not stability contortings.European patent EP 0127253A1 is disclosed
It is a kind of to discharge gas Returning reactor using reacting gas or a kind of monomer as the polyethylene powder degassing method of degassing medium, this
Sample is avoided using inert gas（Such as nitrogen）And the process of discharge gas separation and recovery, it is largely to arrange the shortcomings that the method
Deflation Returning reactor will impact to the stable operation of reactor, while still contain in the polyethylene powder after the completion of degassing
There are reaction monomers, the presence of reaction monomers can influence the safety of lower procedure and powder storage, influence product quality, Er Qiezeng
Big consumption of raw materials and production cost.Notification number is that CN100537609C Chinese invention patent discloses one kind using propane work
For the polyvinyl resin degassing method for the medium that deaerates, discharge gas reclaims ethene and higher boiling alkene, propane returns through two-phase seperation
The degassing of polyolefin particles is carried out, is to contain propane in the polyolefin particles after degassing the shortcomings that the method, downstream process is produced
It is raw to influence.
Except it is above-mentioned with inert gas purge solid polymer come the method for imurity-removal component in addition to, degassing can be with
Using other methods, for example, decompression tank in carry out after polymerization method, as United States Patent (USP) US6465608B1 discloses use
Polymerized monomer is as degassing medium, the process for being depressurized and being deaerated in fluid bed, while after polymerization occurs, this method
The partial reaction monomer of removing can be changed into product, improve degassing efficiency, but the product quality of after polymerization is difficult to control, and is increased
Equipment and running cost are added.Degassing can also use and not be passed through nitrogen（Or including vapor）Under conditions of medium, such as
Notification number is that CN1733810A Chinese invention patent discloses a kind of polypropylene powder after-treating method, in mechanical agitation or
Under mechanical agitation and the double action of heating（Including using rotary dryer）, or be used as and purged by the use of the recovery hydro carbons of circulation
Medium（Including fluidisation or unfluidized state）, or under low pressure under conditions of long-time standing by polymer powders
Quite a few hydro carbons removes out.
In summary, existing solid polymer degassing method exist degassing efficiency is not high, energy consumption is big, consumption of raw materials is big,
The shortcomings of environment is unfriendly, therefore, invent a kind of high degassing efficiency, energy-conservation and environment-friendly solid polymer degassing method tool
There are very high economic interests and realistic meaning.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of method and apparatus of solid polymer degassing.
Specifically, it is related to a kind of method and apparatus for removing solvent present in pulverulent solids polymer and unreacted monomer.
Described solvent refers to material that is needed for reaction process and not chemically reacting, as organic solvent, water, the aqueous solution, gas phase are gathered
Condensing agent in conjunction.
Present invention is preferably applicable to the degassing of vistanex, but polyolefin is not limited to, any granular solid gathers
Compound can use method disclosed by the invention to deaerate, and the production technology of polymer is gathered including gas-phase polymerization, polymerisation in solution, body
Conjunction, emulsion polymerization etc..
A kind of method of solid polymer degassing, comprises the following steps：
i）The first order deaerates：Solid polymer to be de-gassed is passed through first order degassing cabin, there is provided first order degassing medium
To first order degassing cabin, first order degassing medium is set inversely to be connect with solid polymer to be de-gassed in first order degassing cabin
Touch so as to obtain first order degassed polymer, then will deaerate to obtain first row through the first order and deflate and be arranged from first order degassing cabin
Go out；
ii）The second level deaerates：By step i）Obtained first order degassed polymer, which is passed through in the degassing cabin of the second level, carries out week
Phase property pulsed handles to obtain the second degassed polymer, and the recurrent pulses formula processing includes providing second level degassing medium extremely
Second level degassing cabin, the second level degassing medium is set inversely to be connect with first order degassed polymer in the degassing cabin of the second level
Touch, then the second row for deaerating to obtain through the second level is deflated and discharged from the degassing cabin of the second level；
iii）The third level deaerates：By step ii）Obtained second level degassed polymer is passed through in third level degassing cabin, there is provided
The third level deaerates medium to third level degassing cabin, makes the third level degassing medium poly- with the second degassing in third level degassing cabin
Compound carries out reverse contact and obtains final degassed polymer, then discharges gas from the third level by the deaerate to obtain through the third level the 3rd
Discharged in degassing cabin.
Described recurrent pulses formula processing is to be passed through the second level degassing continuous several times moment in the degassing cabin of the second level to be situated between
Matter and moment discharge second row are deflated.
In a preferred embodiment of the present invention, described solid polymer is polyolefin.
In a preferred embodiment of the present invention, described first order degassing medium, the second degassing medium and the 3rd
Degassing medium is gaseous reactant material after fresh gaseous reactant material, recycling, in gaseous hydrocarbons and gaseous inert gas extremely
Few one kind.
In a preferred embodiment of the present invention, described first row is deflated, second row is deflated and the 3rd discharge
Gas is partially recycled or is all expelled to flare system.
In a preferred embodiment of the present invention, step 2）In, degassing medium in the second level is provided to the pulsed
The pressure of second level degassing cabin can be risen into 0.5-2.0MPa, preferably 0.5-1.0MPa within the 1-60 seconds；The pulsed
The second row that ground discharge deaerates to obtain through the second level is deflated and the pressure of second level degassing cabin can be down into 0.15- within the 1-60 seconds
0.45MPa, preferably 0.2-0.4MPa；
In a preferred embodiment of the present invention, 1- is carried out to first order degassed polymer in the degassing cabin of the second level
10 step ii）Described in recurrent pulses formula processing.
In a preferred embodiment of the present invention, the period interval time between each recurrent pulses formula processing is
0-600 seconds, preferably 5-60 seconds.
Preferably, in recurrent pulses formula processing, second level degassing medium is provided to the second level and deaerated
High pressure is risen to when in storehouse and by the pressure of second level degassing cabin（0.5~2.0MPa）When, keep the second level degassing cabin
High pressure 1-1000 seconds, preferably 5-60 seconds, the time of the maintenance high pressure turn into pulse width.And, it is advantageous to when by the second level
When discharge gas is discharged from the degassing cabin of the second level and the pressure of second level degassing cabin is dropped into low pressure（0.15~0.45MPa）,
The low pressure 0-600 seconds of the second level degassing cabin, preferably 5-60 seconds are maintained, when the time of the maintenance low pressure is referred to as period distances
Between.Then, recurrent pulses formula processing next time is then carried out.
The gaseous hydrocarbons be selected from methane, ethane, propane, butane, pentane, isopentane, hexane, ethene, propylene, butylene,
At least one of amylene and hexene.
Described inert gas is selected from least one of nitrogen, carbon dioxide, neon or argon gas, preferably nitrogen.
Present invention also offers a kind of solid polymer degasser, including
For handling the first order degassing cabin of first order degassing；
First order degassing medium provides unit, and it is connected with first order degassing cabin, de- for being provided for first order degassing cabin
Gas medium；
Second level degassing cabin, it is connected with first order degassing cabin, for receiving from first order degassing cabin through first
The first order degassing product of level degassing process, and second level degassing process is carried out to first order degassing product；
Second level degassing medium provides unit, and it is connected with second level degassing cabin, for second level degassing medium to be provided
Second level degassing medium in unit is provided to second level degassing cabin；Exhaust unit is provided with the second level degassing cabin, is made
The second row for deaerating to obtain through the second level deflation obtained in the second level degassing cabin can discharge the second level degassing cabin；
Third level degassing cabin, it is connected with second level degassing cabin, for receiving from second level degassing cabin through the second level
Second degassing product of degassing process, and third level degassing process is carried out to the described second degassing product；
Third level degassing medium provides unit, and it is connected with third level degassing cabin, for providing for third level degassing cabin
Three-level degassing medium.
In a preferred embodiment of the present invention, the degasser also includes：
Product surge tank, it is connected with first order degassing cabin, for providing the polymer with degassing for first order degassing cabin
Product；
Product discharge tank, it is connected with product surge tank, for providing the polymerization come in autoreactor for product surge tank
Thing product.
Beneficial effects of the present invention：
Methods and apparatus of the present invention can remove solid polymer particle surface and external diffusion absorption varsol or
Unreacted monomer and the alkene for being dissolved in polymeric inner.
Methods and apparatus of the present invention can reduce degassing time compared to conventional method, reduce the use of postorder degassing medium
Amount, and can effectively recycling design and unreacted monomer, ensure the safety of lower procedure and powder storage, show with very strong
Sincere justice and application value.
Brief description of the drawings
Fig. 1 is the structural representation of solid polymer degasser of the present invention；
Fig. 2 is the process chart of solid polymer of the present invention degassing method；
In figure, 1- fluidized-bed reactors, 2- product discharge tanks, 3- products surge tank, 4- first order degassing cabin, the 5- second level
Degassing cabin, 6- third level degassing cabin, 7- first order degassing medium provide unit, 8- second level degassing medium provides unit, 9- the
Three-level degassing medium provides unit.
Embodiment
The present invention is described in detail with accompanying drawing with reference to embodiments, but the scope of the present invention is not limited to following reality
Apply example.
As shown in figure 1, the device of solid polymer of the present invention degassing its be connected with fluidized-bed reactor 1, the polymer
Degasser includes：Product discharge tank 2, product surge tank 3, for handle the first order degassing first order degassing cabin 4, for locating
The second level degassing cabin 5 of reason second level degassing and the third level degassing cabin 6 for handling third level degassing, wherein：
First order degassing medium provides unit and is connected with first order degassing cabin 4, for providing degassing for first order degassing cabin 4
Medium；
Second level degassing cabin, it is connected with first order degassing cabin 4, for receiving from first order degassing cabin 4 through the
The first order degassing product of one-level degassing process, and second level degassing process is carried out to first order degassing product；
Second level degassing medium provides unit, and it is connected with second level degassing cabin 5, for second level degassing medium to be provided
Second level degassing medium in unit 8 can be provided to second level degassing cabin 5；It is also equipped with the second level degassing cabin 5
Exhaust unit（Do not show）So that the second row for deaerating to obtain through the second level in the second level degassing cabin 5 is deflated being capable of arteries and veins
Discharge the second level degassing cabin 5 with rushing formula；
Third level degassing cabin 6, it is connected with second level degassing cabin 5, for receiving from second level degassing cabin 5 through second
Second degassing product of level degassing process, and third level degassing process is carried out to the described second degassing product；
Third level degassing medium provides unit 9, and it is connected with third level degassing cabin 6, for being provided for third level degassing cabin 6
Third level degassing medium.
As depicted in figs. 1 and 2, a kind of method of solid polymer degassing, comprises the following steps：
1）The first order deaerates：Solid polymer to be de-gassed is passed through first order degassing cabin 4, there is provided first order degassing medium
To first order degassing cabin 4, first order degassing medium is set to be carried out in first order degassing cabin 4 with solid polymer to be de-gassed reverse
Then contact will deaerate to obtain first row deflation from first order degassing cabin 4 so as to obtain first order degassed polymer through the first order
Middle discharge；
2）The second level deaerates：By step 1）Obtained first order degassed polymer is passed through in second level degassing cabin 5, carries out week
Phase property pulsed handles to obtain the second degassed polymer, and the recurrent pulses formula processing includes providing second level degassing medium extremely
Second level degassing cabin 5, make the second level degassing medium that the pressure of second level degassing cabin 5 risen into 0.5- within the 1-60 seconds
2.0MPa, and inversely being contacted with solid polymer in the second level degassing cabin 5, then will deaerate to obtain through the second level the
Two discharge gas are discharged from second level degassing cabin 5 so that the pressure of second level degassing cabin 5 is down into 0.15- within the 1-60 seconds
0.45MPa；
3）The third level deaerates：By step 2）Obtained second level degassed polymer is passed through in third level degassing cabin 6, there is provided the
Three-level deaerates medium to third level degassing cabin 6, makes the third level degassing medium poly- with the second degassing in third level degassing cabin 6
Compound carries out reverse contact and obtains final degassed polymer, then discharges gas from the third level by the deaerate to obtain through the third level the 3rd
Discharged in degassing cabin 6.
Described recurrent pulses formula processing is to be passed through the second level degassing continuous several times moment in second level degassing cabin 5 to be situated between
Matter and moment discharge second row are deflated；Described solid polymer is polyolefin；Described first order degassing medium, the second degassing
Medium and the 3rd degassing medium are gaseous reactant material, gaseous hydrocarbons or the inertia after fresh gaseous reactant material, recycling
One or several kinds in gaseous state.Described first row is deflated, second row is deflated and the 3rd discharge gas is partially recycled or whole
It is expelled to flare system.
Described inert gas is one or more of combinations in nitrogen, carbon dioxide, neon or argon gas.Described is lazy
Property gas is nitrogen.
Embodiment 1
Using said apparatus, LLDPE is copolymerized with gas-phase fluidized bed technique productions Ethylene/Butylene
（LLDPE）Product, 88 DEG C of the reaction temperature of fluidized-bed reactor 1, reaction pressure 2.1MPa, is operated using non-condensing.Go out material
Each group shunt volume is in stream：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.The LLDPE products discharged from fluidized-bed reactor 1 exist
Convey and initially enter product discharge tank 2 under the drive of gas, subsequently enter product surge tank 3, pressure 0.7MPa, remove part
The hydro carbons of polyethylene particle adsorption, subsequently enter three-level degasification process.First order degassing medium uses nitrogen, and the first order takes off
The flow of gas medium is 200kg/h, and is inversely contacted with solid polymer in first order degassing cabin 4, removes polyethylene
Particle surface and the unreacted monomer of external diffusion absorption, from the top of first order degassing cabin 4, discharge first row is deflated；Second degassing is situated between
Matter is the gaseous mixture of nitrogen and ethene, and the flow of the second degassing medium is 500kg/h, in second level degassing cabin 51 second when
Between under the conditions of be passed through second level degassing medium and the pressure of second level degassing cabin 5 is increased to 0.5MPa, and under the time conditions of 1 second
Discharge second row is deflated and the pressure of second level degassing cabin 5 is reduced to 0.4MPa, is carried out recurrent pulses formula so and is handled 10 times,
Pulse width 1s, the period interval time of operation is 5s.Second degassing medium enters in second level degassing cabin 5 with solid polymer
The reverse contact of row, under big pressure difference caused by the processing of recurrent pulses formula, remove polyethylene duct and be dissolved in polymeric inner
Alkene, from the top of second level degassing cabin 5 discharge second row deflate；3rd degassing medium uses nitrogen, the 3rd degassing medium
Flow is 500kg/h, and is inversely contacted with solid polymer in third level degassing cabin 6, removes the hydro carbons of remaining absorption,
From the discharge gas of the top of third level degassing cabin 6 discharge the 3rd.Impurity content exists in solid polymer particles after three-level deaerates
20ppm（Quality）Below.
Under the same conditions, compared with traditional handicraft degassing time is 100min, the total of medium that deaerate of the present embodiment
Purge time is 90min, reduces 10%.
Embodiment 2
Using device same as Example 1, linea low density is copolymerized with gas-phase fluidized bed technique productions polyethylene-hexene
Polyethylene（LLDPE）Product, 88 DEG C of the reaction temperature of fluidized-bed polymerization reactor 1, reaction pressure 2.1MPa, is grasped using non-condensing
Make.Each group shunt volume is in output streams：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.The LLDPE products discharged from fluidized-bed reactor 1
Product discharge tank 2 is initially entered under the drive of conveying gas, secondly enters product surge tank 3, removes part polyethylene particle
The hydro carbons of adsorption, subsequently enter three-level degasification process.First order degassing medium uses nitrogen, the stream of first order degassing medium
Measure as 300kg/h, and inversely contacted with solid polymer in first order degassing cabin 4, removing polyethylene particle surface and
The unreacted monomer of external diffusion absorption, from the top of first order degassing cabin 4, discharge first row is deflated；Second degassing medium is nitrogen,
The flow of second degassing medium is 550kg/h, is passed through second level degassing under the time conditions of 60 seconds in second level degassing cabin 5
Medium makes the pressure of second level degassing cabin 5 increase to 0.5MPa, and second discharge second row deflation makes second under 60 time conditions
The pressure of level degassing cabin 5 reduces to 0.2MPa, carries out such recurrent pulses formula and handles 4 times, pulse width 5s, the cycle of operation
Interval time is 20 seconds.Second degassing medium is inversely contacted in second level degassing cabin 5 with solid polymer, periodically
Under big pressure difference caused by pulsed processing, remove polyethylene duct and be dissolved in the alkene of polymeric inner, deaerated from the second level
The top of storehouse 5 discharge second row is deflated；3rd degassing medium use nitrogen, and the 3rd flow for deaerating medium is 550kg/h, and the
Inversely contacted with solid polymer in three-level degassing cabin 6, the hydro carbons of remaining absorption is removed, from the top of third level degassing cabin 6
Discharge the 3rd discharge gas.Impurity content is in 20ppm in solid polymer particles after three-level deaerates（Quality）Below.
Under the same conditions, compared with the degassing time of traditional handicraft is 140min, the degassing medium of the present embodiment
Total purge time is 95min, reduces 32%.
Embodiment 3
Using device same as Example 1, linea low density is copolymerized with gas-phase fluidized bed technique productions Ethylene/Butylene
Polyethylene（LLDPE）Product, 88 DEG C of the reaction temperature of fluidized-bed reactor 1, reaction pressure 2.1MPa, using condensation operation.Go out
Each group shunt volume is in material stream：LLDPE powder 40t/h, nitrogen 160kg/h, hydrogen 3kg/h, ethene 2580kg/h, 1- butylene
2300kg/h, isopentane 2500kg/h.Wherein ethene and 1- butylene are unreacted monomer, and isopentane is solvent.It is anti-from fluid bed
Answer the LLDPE products that device 1 is discharged to initially enter product discharge tank 2 under the drive of conveying gas, secondly enter product surge tank
3, the hydro carbons of removing part polyethylene particle surface absorption, subsequently enter three-level degasification process.First order degassing medium uses nitrogen
Gas, the flow of first order degassing medium is 300kg/h, and is inversely contacted with solid polymer in first order degassing cabin 4,
The varsol or unreacted monomer of polyethylene particle surface and external diffusion absorption are removed, is discharged from the top of first order degassing cabin 4
First row is deflated；Second degassing medium be nitrogen, and the flow of the second degassing medium is 550kg/h, in the second level degassing cabin 5 it is interior
Second level degassing medium is passed through under the time conditions of 30 seconds makes the pressure of second level degassing cabin 5 increase to 1.0MPa, and at 30 seconds
Second row is discharged under time conditions and is deflated makes the pressure of second level degassing cabin 5 reduce to 0.3MPa, carries out such recurrent pulses formula
Processing 5 times, pulse width are 40 seconds, and the interval time of operation is 0 second.Second degassing medium is in second level degassing cabin 5 and solid
Body polymer is inversely contacted, and under big pressure difference caused by the processing of recurrent pulses formula, is removed polyethylene duct and is dissolved in
The alkene of polymeric inner, from the top of second level degassing cabin 5, discharge second row is deflated；3rd degassing medium uses nitrogen, and the 3rd
The flow of degassing medium is 550kg/h, and is inversely contacted with solid polymer in third level degassing cabin 6, and removing is remaining
The hydro carbons of absorption, from the discharge gas of the top of third level degassing cabin 6 discharge the 3rd.It is miscellaneous in solid polymer particles after three-level deaerates
Matter content is in 20ppm（Quality）Below.
Under the same conditions, compared with traditional handicraft degassing time is 120min, the total of medium that deaerate of the present embodiment
Purge time is 85min, reduces 29%.
Embodiment 4
Using device same as Example 1, linea low density is copolymerized with gas-phase fluidized bed technique productions polyethylene-hexene
Polyethylene（LLDPE）Product, 88 DEG C of the reaction temperature of fluidized-bed reactor 1, reaction pressure 2.1MPa, using condensation operation.Go out
Each group shunt volume is in material stream：LLDPE powder 40t/h, nitrogen 160kg/h, hydrogen 3kg/h, ethene 2580kg/h, isopentane
2500kg/h, hexene 2000kg/h.Wherein ethene and hexene are unreacted monomer, and isopentane is solvent.From fluidized-bed reactor 1
The LLDPE products of discharge initially enter product discharge tank 2 under the drive of conveying gas, secondly enter product surge tank 3, remove
The hydro carbons of part polyethylene particle surface absorption, subsequently enters three-level degasification process.First order degassing medium uses nitrogen, and first
The flow of level degassing medium is 300kg/h, and is inversely contacted with solid polymer in first order degassing cabin 4, and removing is poly-
Ethene particle surface and the varsol or unreacted monomer of external diffusion absorption, first row is discharged from the top of first order degassing cabin 4
Deflate；Second degassing medium is the gaseous mixture of nitrogen and ethene, and the flow of the second degassing medium is 550kg/h, is taken off in the second level
Being passed through second level degassing medium in gas storehouse 5 under conditions of 10 seconds makes the pressure of second level degassing cabin 5 increase to 0.7MPa, and 10
Second row is discharged under conditions of second and is deflated makes the pressure of second level degassing cabin 5 reduce to 0.4MPa, carries out such recurrent pulses formula
Processing 1 time, pulse width are 60 seconds, and the interval time of operation is 60 seconds.Second degassing medium is in second level degassing cabin 5 and solid
Body polymer is inversely contacted, and under big pressure difference caused by the processing of recurrent pulses formula, is removed polyethylene duct and is dissolved in
The alkene of polymeric inner, from the top of second level degassing cabin 5, discharge second row is deflated；3rd degassing medium uses nitrogen, and the 3rd
The flow of degassing medium is 550kg/h, and is inversely contacted with solid polymer in third level degassing cabin 6, and removing is remaining
The hydro carbons of absorption, from the discharge gas of the top of third level degassing cabin 6 discharge the 3rd.It is miscellaneous in solid polymer particles after three-level deaerates
Matter content is in 20ppm（Quality）Below.
Under the same conditions, traditional handicraft degassing time is compared for 130min, and the degassing medium of the present embodiment always blows
Flyback time is 87min, reduces 33%.
Claims (10)
1. a kind of method of solid polymer degassing, comprises the following steps：
I) first order deaerates：Solid polymer to be de-gassed is passed through first order degassing cabin, there is provided the first order deaerates medium to the
One-level degassing cabin, make the first order deaerate medium carried out in first order degassing cabin with solid polymer to be de-gassed it is reverse contact from
And first order degassed polymer is obtained, it then will deaerate to obtain first row through the first order and deflate and be discharged from first order degassing cabin；
Ii) second level deaerates：The first order degassed polymer that step i) is obtained is passed through in the degassing cabin of the second level and carried out periodically
Pulsed handles to obtain the second degassed polymer, and the recurrent pulses formula processing includes providing second level degassing medium to second
Level degassing cabin, the second level degassing medium is set inversely to be contacted with first order degassed polymer in the degassing cabin of the second level,
Then the second row for deaerating to obtain through the second level is deflated and discharged from the degassing cabin of the second level；
Iii) third level deaerates：By step ii) obtained second level degassed polymer is passed through in third level degassing cabin, there is provided the 3rd
Level degassing medium to third level degassing cabin, make the third level deaerate medium in third level degassing cabin with the second degassed polymer
Carry out reverse contact and obtain final degassed polymer, then the 3rd discharge gas for deaerating to obtain through the third level deaerates from the third level
Discharged in storehouse；
Wherein, step ii) in second level degassing medium be provided enabled to second level degassing cabin within the 1-60 seconds
Pressure rises to 0.5-2.0MPa；The discharge second row for deaerating to obtain through the second level, which is deflated, to be enabled in the 1-60 seconds
The interior pressure by second level degassing cabin is down to 0.15-0.45MPa；
Wherein, described solid polymer is polyolefin.
2. according to the method for claim 1, it is characterised in that described first order degassing medium, the second degassing medium and
3rd degassing medium is gaseous reactant material, gaseous hydrocarbons, nitrogen, the titanium dioxide after fresh gaseous reactant material, recycling
At least one of carbon, neon or argon gas.
3. method according to claim 1 or 2, it is characterised in that described first row is deflated, second row is deflated and the
Three discharge gas are partially recycled or are all expelled to flare system.
4. method according to claim 1 or 2, it is characterised in that step ii) in provide second level degassing medium with
Make it possible to that the pressure of second level degassing cabin is risen into 0.5-1.0MPa within the 1-60 seconds；The discharge is described to deaerate through the second level
Obtained second row is deflated and enables to that the pressure of second level degassing cabin is down into 0.2-0.4MPa within the 1-60 seconds.
5. method according to claim 1 or 2, it is characterised in that deaerate and polymerize to the first order in the degassing cabin of the second level
Thing carry out 1-10 step ii) described in recurrent pulses formula handle.
6. method according to claim 1 or 2, it is characterised in that step ii) described in the pulse width of pulse be 1-
1000 seconds.
7. the pulse width of pulse described according to the method for claim 6, it is characterised in that step ii) is 5-60
Second.
8. according to the method for claim 2, it is characterised in that the gaseous hydrocarbons be selected from methane, ethane, propane, butane,
At least one of pentane, isopentane, hexane, ethene, propylene, butylene, amylene and hexene.
9. a kind of solid polymer degasser, including
For handling the first order degassing cabin of first order degassing；
First order degassing medium provides unit, and it is connected with first order degassing cabin, is situated between for providing degassing for first order degassing cabin
Matter；
Second level degassing cabin, it is connected with first order degassing cabin, for receiving being taken off through the first order from first order degassing cabin
The first order degassing product of gas disposal, and second level degassing process is carried out to first order degassing product；
Second level degassing medium provides unit, and it is connected with second level degassing cabin, for providing second level degassing medium to unit
In the second level degassing medium provide to second level degassing cabin；Exhaust unit is provided with the second level degassing cabin so that institute
The second row for deaerating to obtain through the second level deflation stated in the degassing cabin of the second level can discharge the second level degassing cabin；
Third level degassing cabin, it is connected with second level degassing cabin, for receiving being deaerated through the second level from second level degassing cabin
Second degassing product of processing, and third level degassing process is carried out to the described second degassing product；
Third level degassing medium provides unit, and it is connected with third level degassing cabin, for providing the third level for third level degassing cabin
Deaerate medium,
Wherein, described solid polymer is polyolefin.
10. device according to claim 9, it is characterised in that the degasser also includes：
Product surge tank, it is connected with first order degassing cabin, for providing the polymer product with degassing for first order degassing cabin；
Product discharge tank, it is connected with product surge tank, for providing the polymerization produce come in autoreactor for product surge tank
Thing.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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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