CN106554438B - A kind of stage division of olefin polymerization catalysis suspension - Google Patents
A kind of stage division of olefin polymerization catalysis suspension Download PDFInfo
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- CN106554438B CN106554438B CN201510639667.0A CN201510639667A CN106554438B CN 106554438 B CN106554438 B CN 106554438B CN 201510639667 A CN201510639667 A CN 201510639667A CN 106554438 B CN106554438 B CN 106554438B
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Abstract
The present invention relates to olefin polymerization catalysis fields, disclose a kind of stage division of olefin polymerization catalysis suspension, carry out in cyclone；Cyclone includes cyclone body and collecting chamber, and cyclone body includes cylinder pipeline section and circular cone pipeline section from top to bottom；There is the first overflow pipe with collecting chamber airtight connection in cylinder pipeline section, cyclone body and collecting chamber only pass through the first overflow pipe and communicate；Method includes: to be introduced into cyclone body olefin polymerization catalysis suspension by feed inlet and be rotated in it；For bulky grain by conical tube pars infrasegmentalis outlet discharge, little particle enters collecting chamber by the first overflow pipe, and is discharged by the outlet of collecting chamber.Olefin polymerization catalysis suspension is classified using cyclone as above, the product granularity of cyclone upper outlet and lower outlet can be effectively controlled, meet requirement of the different alkene production technology to olefin polymerization catalysis grain diameter.
Description
Technical field
The present invention relates to olefin polymerization catalysis fields, and in particular, to a kind of point of olefin polymerization catalysis suspension
Grade method.
Background technique
The catalyst component for olefin polymerization for being used to prepare polyolefin is commonly known, generally as carrier or is divided using magnesium chloride
Dispersion media loads titanium tetrachloride on it and internal electron donor forms, and this catalytic component is typically certain shapes
Solid particle mainly has spherical shape and spherical two kinds.
In polyolefin production processes, the size distribution of polymer is required.When especially producing certain specific trades mark,
There is strict demand to the partial size of polymer, size distribution must be needed with adaptive device within the limits prescribed and product needs
It asks.Such as it is to wish polymer partial size no more than 0.3 millimeter when sizing process device produces ultra-high molecular weight polyethylene product；In
Unipol technique wishes polymer partial size in OK range to be conducive to fluidize when producing；In polypropylene loop technology and gas phase work
Process and equipment wishes that polymer macroparticle is few in favor of shifting and transmitting when producing.Meeting the requirement in terms of polymer particle size can be used
Many methods, including polymerization technique control, catalyst activity control, Polymer Fractionation etc., wherein control catalytic component granularity
It is one of main method.
At present there are mainly two types of the methods of control polyolefin catalyst component granularity, one is sieve methods, using difference
The sieve control in aperture passes through the granularity of sieve product；Another chemical preparation method leads to that is, in catalytic component preparation process
Adjustment preparation process is crossed, the granularity of catalytic component is controlled.
At present the overwhelming majority polyolefin catalyst components granularity control use chemical preparation method, using this method have at
Sheet is low, does not increase the advantages that process, but product that is affected by environment larger by the control of such method preparation process and obtaining
Broad particle distribution, for needing the polyolefin catalyst component of accurate Control granularity to prepare, this method is not applicable.
Catalyst component for olefin polymerization is generally the fine particle in 0.1-100 micron range, and common method for sieving is main
To be used to remove bulky grain and residue therein, since catalytic component partial size is smaller, method for sieving is unsuitable for for accurately controlling
The granularity of catalytic component processed.And the method such as air-flow rotation point-score for being generally used for gradation mainly uses air or water vapour to make
For medium, hence it is evident that be not suitable for the classification of this substance that need to completely cut off air, oxygen and water of catalyst component for olefin polymerization.
The above-mentioned prior art is made a general survey of, relevant gradation technology is mainly used for the classification of greater particle size particle, for alkene
The substance that this partial size of polymerized hydrocarbon catalytic component is smaller and medium requirements are stringent, still without suitable stage division.
Summary of the invention
The purpose of the invention is to overcome disadvantages described above, catalyst component for olefin polymerization can effectively be divided by providing one kind
The method of grade.
To achieve the goals above, the present invention provides a kind of stage division of olefin polymerization catalysis suspension, wherein institute
Classification is stated to carry out in cyclone；
The cyclone includes cyclone body and collecting chamber, the cyclone body include from top to bottom cylinder pipeline section and
Circular cone pipeline section；Wherein, the first overflow pipe with the collecting chamber airtight connection, and the eddy flow are provided in the cylinder pipeline section
Device ontology and collecting chamber only pass through the first overflow pipe and communicate；
It is introduced into this method comprises: olefin polymerization catalysis suspension is passed through the feed inlet being arranged on cyclone body
It is rotated in cyclone body and in it；Under the action of rotary force, olefin polymerization catalysis bulky grain is by setting
It sets in the outlet of conical tube pars infrasegmentalis discharge, olefin polymerization catalysis little particle enters collecting chamber by the first overflow pipe, and leads to
Cross the outlet discharge being arranged on collecting chamber；
The olefin polymerization catalysis suspension is introduced into cyclone body under stirring conditions；The stirring turns
Speed is greater than 20rpm.
Preferably, the revolving speed of the stirring is 50-500rpm.
Preferably, the olefin polymerization catalysis suspension is introduced into cyclone body with the pressure of 0.1-0.6MPa.
Preferably, the aperture that the valve at conical tube pars infrasegmentalis bulky grain outlet is arranged in is 5-30%.
Preferably, dismountable second overflow in first overflow pipe is additionally provided in the cylinder pipeline section
Pipe, second overflow pipe with the material discharge pipe being arranged in the collecting chamber is closed communicates；Wherein, in the effect of rotary force
Under, the middle particle in olefin polymerization catalysis little particle enters collecting chamber by the first overflow pipe, and by being arranged in collecting chamber
On outlet discharge；Fine grained in olefin polymerization catalysis little particle enters the second overflow pipe, and by being arranged in the receipts
Collect the material discharge pipe discharge with the second overflow pipe airtight connection in room.
Olefin polymerization catalysis suspension is classified using cyclone as above, can effectively be controlled on cyclone
The product granularity of outlet and lower outlet, wants olefin polymerization catalysis grain diameter to meet different alkene production technology
It asks.In the case where preferably cooperating specific feed pressure and bottom valve aperture, the effect of the classification can be promoted further.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is a kind of cyclone of classification specific for olefin polymerization catalysis suspension.
Description of symbols
1, cyclone body 2, collecting chamber 3, the outlet being arranged on collecting chamber
4, the material discharge pipe 5 that is arranged in collecting chamber, the outlet that conical tube pars infrasegmentalis is set
11, cylinder pipeline section 12, circular cone pipeline section
111, the first overflow pipe 112, the second overflow pipe
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of stage divisions of olefin polymerization catalysis suspension, wherein the classification is in cyclone
Middle progress；
The cyclone includes cyclone body 1 and collecting chamber 2, and the cyclone body 1 includes cylindrical tube from top to bottom
Section 11 and circular cone pipeline section 12；Wherein, the first overflow pipe with 2 airtight connection of collecting chamber is provided in the cylinder pipeline section 11
111, and the cyclone body 1 and collecting chamber 2 are only communicated by the first overflow pipe 111；
Draw this method comprises: olefin polymerization catalysis suspension is passed through the feed inlet 13 being arranged on cyclone body 1
Enter and is rotated into cyclone body 1 and in it；Under the action of rotary force, olefin polymerization catalysis bulky grain is logical
The discharge of outlet 5 that 12 lower part of circular cone pipeline section is set is crossed, olefin polymerization catalysis little particle is entered by the first overflow pipe 111 to be received
Collect room 2, and the outlet 3 by being arranged on collecting chamber 2 is discharged；
The olefin polymerization catalysis suspension is introduced into cyclone body under stirring conditions；The stirring turns
Speed is greater than 20rpm.
According to the method for the present invention, the olefin polymerization catalysis suspension refers to the system in catalyst component for olefin polymerization
During standby, without vacuum drying treatment, and obtain its final products suspension.Wherein, the olefinic polymerization is urged
Agent component has meaning well known in the art, refers to catalyst granules of the partial size in 0.1-100 micron range, main component
For titanium, magnesium.Chlorine and electron donor, for example, the institutes such as Chinese patent CN85100997, CN1453298A, ZL200410062290.9
Disclosed catalytic component.
According to the method for the present invention, the concentration of the olefin polymerization catalysis suspension can be the choosing of this field routine
It selects, for example, without vacuum drying, final products are outstanding for olefin polymerization catalysis during preparing olefin polymerization catalysis
Concentration when supernatant liquid.Preferably, the concentration of olefin polymerization catalysis is preferably 10-60 in the olefin polymerization catalysis suspension
Weight %, further preferably 20-50 weight %.
According to the method for the present invention, the solvent in the olefin polymerization catalysis suspension can be as described above for this field
Conventional inertia alkane washing.Direct-connected or branch the aliphatic hydrocarbon of preferably C1-C7, the direct-connected or branch of more preferably C5-C7
The aliphatic hydrocarbon of chain, for example, the direct-connected or branch of direct-connected or branch the aliphatic hydrocarbon of direct-connected or branch the aliphatic hydrocarbon of C5, C6, C7
Aliphatic hydrocarbon.Further preferably at least one of pentane, isopentane, hexane and heptane, most preferably isopentane and/or
Hexane.
According to the method for the present invention, under pressure, by the olefin polymerization catalysis suspension by feed inlet 13
The cylinder pipeline section 11 inside cyclone body 1 is entered, due to the current limliting by 11 tube wall of cylinder pipeline section and top, forces suspension
Liquid does top-down rotary motion in cylinder pipeline section 11 and circular cone pipeline section 12 to form contour stealth, turns over journey in suspension
Middle to form powerful centrifugal force, bulky grain under the action of the centrifugal force, is gradually moved to outer wall, and along barrel under the action of resultant force
Rotation is fallen, until being discharged from underflow opening 5；The contour stealth of rotation decline by the contraction of circular cone pipeline section 12 due to being influenced gradually in
The heart collects, decline to a certain extent when start to return and rise, form one rotary motion from bottom to top to form inward eddy,
Little particle with spiral to inward eddy, cyclone body 1 radially along center to 1 wall direction particle diameter of cyclone body by
Small to greatly, along axial direction, particle diameter is ascending from top to bottom, and the inward eddy of rising enters collecting chamber 2 from the first overflow pipe 111,
And the outlet 3 by being arranged on collecting chamber 2 is discharged.The classification of olefin polymerization catalysis suspension is completed as a result,.
According to the method for the present invention, in order to further increase the effect of the classification, guarantee catalytic component in suspension
Dispersibility, the olefin polymerization catalysis suspension is preferably added under stirring conditions in the cyclone body 1, institute
The speed for stating stirring can be 50-500rpm, preferably 50-300rpm, more preferably 70-200rpm.
According to the method for the present invention, expected rotation is formed in cyclone 1 for the olefin polymerization catalysis suspension
Stream, to guarantee its grading effect in cyclone 1, the olefin polymerization catalysis suspension is preferably with the pressure of 0.1-0.6MPa
Power is introduced into cyclone body 1, more preferably with the pressure of 0.2-0.5MPa, further preferably with the pressure of 0.25-0.4MPa.
Pressure stable in this way plays the role of the granularity and grading effect of graded product positive.
According to the method for the present invention, it was found by the inventors of the present invention that by adjusting going out for 12 lower part of circular cone pipeline section is arranged in
The aperture of valve at mouth 5, can effectively adjust the granularity of the product of acquisition.Preferably, different in order to obtain being suitble to
The catalyst particle size requirement of olefin polymetiation process, opening for the valve can be 5-30%, preferably 10-30%.
According to the method for the present invention, first overflow pipe 111 passes through the opening and collection that 2 lower surface of collecting chamber is arranged in
Room 2 is closed to be communicated, wherein can also be arranged in the upper surface of cylinder pipeline section 11 with the opening phase with 2 lower surface of collecting chamber
The partition for the opening matched communicates to be conducive to the first overflow pipe 111 with the closed of collecting chamber 2.In addition, during eddy flow,
In order to which the granule grade particles material isolated can smoothly enter in collecting chamber 2.The caliber etc. of first overflow pipe 111
In or less than 2 lower surface of collecting chamber opening aperture.
A kind of preferred embodiment according to the present invention, in order to effectively adjust the granularity of classification products obtained therefrom, institute
State depth of first overflow pipe 111 in cylinder pipeline section 11 be it is adjustable, it is preferred, therefore, that 111 lower part of the first overflow pipe
It is also equipped with the regulating device of adjustable first overflow pipe, 111 depth.The regulating device can be that can arbitrarily adjust first
The device of 111 depth of overflow pipe, for example, can be adjusting ring.
According to the method for the present invention, in order to be divided into more grades to olefin polymerization catalysis suspension, according to this
A kind of preferred embodiment is invented, for being divided into 3 kinds of grades, is additionally provided in the cylinder pipeline section 11 positioned at described first
Dismountable second overflow pipe 112 in overflow pipe 111, the object the second overflow pipe 112 and be arranged in the collecting chamber 2
Expect that discharge pipe 4 is closed to communicate, that is to say, that the particle in second overflow pipe 112 does not enter collecting chamber 2, but directly logical
It crosses material discharge pipe 4 and cyclone is discharged.
Specifically, under pressure, the olefin polymerization catalysis suspension is entered eddy flow by feed inlet 13
Cylinder pipeline section 11 inside device ontology 1 forces suspension in cylindrical tube due to the current limliting by 11 tube wall of cylinder pipeline section and top
Top-down rotary motion is done in section 11 and circular cone pipeline section 12 to form contour stealth, is formed during suspension turns powerful
Centrifugal force, bulky grain under the action of the centrifugal force, gradually moves to outer wall, and rotates and fall along barrel under the action of resultant force,
Until being discharged from underflow opening 5；The contour stealth for rotating decline gradually collects to center due to being influenced by the contraction of circular cone pipeline section 12, under
Start to return when dropping to a certain degree and rise, form one rotary motion from bottom to top to form inward eddy, little particle with
Spiral is ascending to 1 wall direction particle diameter of cyclone body radially along center in cyclone body 1 to inward eddy,
Along axial direction, particle diameter is ascending from top to bottom, and the middle particle in the inward eddy of rising enters from the first overflow pipe 111 to be collected
Room 2, and the outlet 3 by being arranged on collecting chamber 2 is discharged；Fine grained in olefin polymerization catalysis little particle enters second and overflows
Flow tube 112, and the discharge of material discharge pipe 4 with 112 airtight connection of the second overflow pipe by being arranged in the collecting chamber 2.
3 kinds of different grades of olefin polymerization catalysis suspension have been obtained as a result,.
Wherein, the caliber of second overflow pipe 112 is equal to or less than the diameter of the second material discharge pipe 4, so as to
It can be by being smoothly discharged out through second material discharge pipe 4 in thin particulate matter during eddy flow, isolated.
According to the method for the present invention, in order to more subtly adjusting the middle grain products being classified by the above little particle
With fine grained product, it is described adjust 112 depth of the second overflow pipe device, when the second overflow pipe 112 insertion depth increase when,
Material fine grained increases in second overflow pipe 112, and middle particle is reduced, and insertion depth reduces, and fine granular materials are reduced, middle particulate matter
Material increases.
Wherein, the present invention is not particularly limited the regulating device, as long as can be realized to the second overflow pipe
The adjusting of 112 depth.For example, the regulating device can be connect with 4 outer wall of second material discharge pipe, and in top lifting
Setting runner in end realizes the lifting of the second overflow pipe 112 by the rotation of runner.
According to the method for the present invention, it in order to be formed with the contour stealth and inward eddy that are conducive to classification in cyclone, receives
Collecting the ratio between height of room 2, cylinder pipeline section 11 and circular cone pipeline section 12 is (10-20): (10-20): (25-35), preferably (12-
18): (14-18): (28-32).
According to the method for the present invention, the taper of the circular cone pipeline section 12 can be 10-20 degree.
According to the method for the present invention, this method further include after being classified resulting material be dried in vacuo.Wherein, described true
The dry method of sky is the selection of this field routine, and details are not described herein by the present invention.
The present invention will be described in detail by way of examples below.In following embodiment, to incite somebody to action in following embodiment
Olefin polymerization catalysis suspension is illustrated for being divided into two-stage.
Table 1
Embodiment 1-7 and comparative example 1-3
Olefin polymerization catalysis suspension is prepared according to 1 method of patent CN85100997 embodiment, only catalyst
Component washed with hexane after without vacuum drying, obtain the olefin polymerization catalyst slurry as shown in embodiment 1-10 suspension
Liquid.
According to condition shown in embodiment 1-7 and comparative example 1-3, by reaction kettle pipeline and cyclone inlet pipeline phase
Even, the outlet (abbreviation upper outlet) and the outlet (letter that 12 lower part of circular cone pipeline section is set that cyclone is arranged on collecting chamber are opened
Claim lower outlet), under conditions of nitrogen atmosphere pressure and stirring, enter suspension in cyclone.Measurement enter cyclone it
The grain graininess of suspension obtained by preceding suspension, upper outlet and lower outlet.Wherein, the measurement of grain graininess uses the Ma Er of Britain
Literary 2000 laser particle analyzers.It the results are shown in Table 2
Table 2
Note: the granularity difference exported up and down can be with the effect of Assessment for classification, and average particle size difference is bigger, and grading effect is better
As can be seen from Table 2, it by embodiment 1-7 compared with comparative example 1-3, can effectively be controlled using method of the invention
The product granularity that cyclone exports up and down, to realize the classification of polyolefin catalyst component.By embodiment 1-3 and embodiment 4-
7 compare, mixing speed when aperture, the introducing pressure of suspension and the suspension by controlling lower outlet valve introduce, energy
It is enough further to improve grading effect, adjust the granularity of product.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (8)
1. a kind of stage division of olefin polymerization catalysis suspension, which is characterized in that the classification carries out in cyclone；
The cyclone includes cyclone body (1) and collecting chamber (2), and the cyclone body (1) includes cylinder from top to bottom
Pipeline section (11) and circular cone pipeline section (12)；Wherein, it is provided with and the collecting chamber (2) airtight connection in the cylinder pipeline section (11)
First overflow pipe (111), and the cyclone body (1) and collecting chamber (2) are only communicated by the first overflow pipe (111)；
This method comprises: olefin polymerization catalysis suspension is drawn by the feed inlet (13) being arranged on cyclone body (1)
Enter and is rotated in cyclone body (1) and in it；Under the action of rotary force, olefin polymerization catalysis bulky grain
By the way that outlet (5) discharge in circular cone pipeline section (12) lower part is arranged, olefin polymerization catalysis little particle passes through the first overflow pipe
(111) enter collecting chamber (2), and the discharge of the outlet (3) by being arranged on collecting chamber (2)；
Wherein, the olefin polymerization catalysis suspension is introduced under stirring conditions in cyclone body (1)；The stirring
Revolving speed be 70-200rpm；
The olefin polymerization catalysis suspension is introduced into cyclone body (1) with the pressure of 0.25-0.4MPa；
The ratio between height of collecting chamber (2), cylinder pipeline section (11) and circular cone pipeline section (12) is 10-20:10-20:25-35；
The aperture that the valve at the outlet (5) of circular cone pipeline section (12) lower part is arranged is 5-30%.
2. according to the method described in claim 1, wherein, first overflow pipe (111) is by being arranged in collecting chamber (2) following table
The opening in face with collecting chamber (2) is closed communicates, the caliber of first overflow pipe (111) is equal to or less than collecting chamber (2) following table
The aperture of the opening in face.
3. method according to claim 1 or 2, wherein the first overflow pipe (111) lower part is also equipped with adjustable
The regulating device of one overflow pipe (111) depth.
4. according to the method described in claim 1, wherein, being additionally provided in the cylinder pipeline section (11) positioned at first overflow
Dismountable second overflow pipe (112) in (111) is managed, second overflow pipe (112) and setting are in the collecting chamber (2)
Material discharge pipe (4) closed communicate；
Wherein, under the action of rotary force, middle particle in olefin polymerization catalysis little particle by the first overflow pipe (111) into
Enter collecting chamber (2), and the discharge of the outlet (3) by being arranged on collecting chamber (2)；Thin in olefin polymerization catalysis little particle
Grain enter the second overflow pipe (112), and by be arranged in the collecting chamber (2) with the second overflow pipe (112) airtight connection
Material discharge pipe (4) discharge.
5. according to the method described in claim 4, wherein, the aperture of second overflow pipe (112) is equal to or less than described set
Set the aperture of the material discharge pipe in the collecting chamber (2).
6. method according to claim 4 or 5, wherein the cyclone includes and the second overflow pipe (112) outer wall
The regulating device of the second overflow pipe of adjusting (112) depth of connection.
7. according to the method described in claim 1, wherein, the taper of the circular cone pipeline section (12) is 10-20 degree.
8. according to the method described in claim 1, wherein, this method further include after being classified resulting material be dried in vacuo.
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| CN113166292A (en) * | 2018-11-30 | 2021-07-23 | 博里利斯股份公司 | Washing process |
| CN111151169A (en) * | 2020-01-15 | 2020-05-15 | 江苏龙创新材料科技有限公司 | Cyclone for processing paint for enameled wire and control method thereof |
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| CN202778747U (en) * | 2012-07-18 | 2013-03-13 | 杜振宝 | Classifying cyclone |
| CN104858044A (en) * | 2014-02-21 | 2015-08-26 | 中国石油化工股份有限公司 | Catalyst carrier classification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202778747U (en) * | 2012-07-18 | 2013-03-13 | 杜振宝 | Classifying cyclone |
| CN104858044A (en) * | 2014-02-21 | 2015-08-26 | 中国石油化工股份有限公司 | Catalyst carrier classification method |
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