CN106554438A - 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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- CN106554438A CN106554438A CN201510639667.0A CN201510639667A CN106554438A CN 106554438 A CN106554438 A CN 106554438A CN 201510639667 A CN201510639667 A CN 201510639667A CN 106554438 A CN106554438 A CN 106554438A
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- collecting chamber
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Abstract
The present invention relates to olefin polymerization catalysis field, discloses a kind of stage division of olefin polymerization catalysis suspension, carries 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 are the first overflow pipe with collecting chamber airtight connection, cyclone body and collecting chamber only to communicate by the first overflow pipe in cylinder pipeline section；Method includes：Olefin polymerization catalysis suspension is incorporated in cyclone body by charging aperture and is rotated in which；Bulky grain is discharged by the outlet of conical tube pars infrasegmentalis, and 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, can effectively control the product granularity of cyclone upper outlet and lower outlet, 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 field, in particular it relates to a kind of olefin polymerization catalysis are outstanding
The stage division of supernatant liquid.
Background technology
It is commonly known for preparing polyolefinic catalyst component for olefin polymerization, typically with magnesium chloride be
Carrier or disperse medium, load titanium tetrachloride thereon and internal electron donor are formed, this catalytic component
The solid particle of definite shape is typically, mainly has spherical and spherical two kinds.
In polyolefin production processes, the particle size distribution of polymer is required.Some are produced especially special
When determining the trade mark, have strict demand to the particle diameter of polymer, its particle size distribution must within the limits prescribed,
Needed with adaptive device and product demand.Such as ultra-high molecular weight polyethylene product is produced in what sizing process device
Shi Xiwang polymer particle diameter is not more than 0.3 millimeter；Wish that polymer particle diameter exists in Unipol technique productions
OK range be conducive to fluidisation；Polymerization is wished when producing in polypropylene loop technology and gas phase process unit
Thing bulky grain is beneficial to transfer less and transmits.Meet the requirement in terms of polymer particle size and can adopt many sides
Method, including polymerization technique control, catalyst activity control, Polymer Fractionation etc., wherein controlling catalyst
Component particle size is one of main method.
The method of control polyolefin catalyst component granularity mainly has two kinds at present, and one kind is sieve method,
Using granularity of the screen cloth control of different pore size by screen cloth product；Another kind of chemical preparation method, that is, urging
In agent component preparation process, by adjusting preparation technology, the granularity of catalytic component is controlled.
The Task-size Controlling of overwhelming majority polyolefin catalyst component adopts chemical preparation method at present, using the party
Method has the advantages that low cost, does not increase operation, but receives environment by the control of such method preparation technology
Affect it is larger, and obtain Granularity Distribution it is wider, for the catalyzed polyolefin for needing precise control granularity
Prepared by agent component, the method is not applied to.
Catalyst component for olefin polymerization is generally the fine particle in 0.1-100 micrometer ranges, conventional sieve
Divide method, be mainly used to remove bulky grain therein and residue, as catalytic component particle diameter is less, sieve
Point method is unsuitable for the granularity for precise control catalytic component.And the method for being generally used for gradation
As air-flow rotation point-score mainly adopts air or water vapour as medium, hence it is evident that be not suitable for olefinic polymerization catalysis
The classification of this material that need to completely cut off air, oxygen and water of agent component.
Above-mentioned prior art is made a general survey of, related gradation technology is mainly used in dividing for greater particle size granule
Level, and medium requirements strict material less for this particle diameter of catalyst component for olefin polymerization still do not have
There is suitable stage division.
The content of the invention
The invention aims to overcome disadvantages described above, there is provided one kind can be to olefin polymerization catalysis group
The method for dividing effectively classification.
To achieve these goals, the present invention provides a kind of classification side of olefin polymerization catalysis suspension
Method, wherein, the classification is carried out in cyclone；
The cyclone includes cyclone body and collecting chamber, and the cyclone body includes circle from top to bottom
Column jecket section and circular cone pipeline section；Wherein, it is provided with the cylinder pipeline section and the collecting chamber airtight connection
First overflow pipe, and the cyclone body and collecting chamber only communicated by the first overflow pipe；
The method includes：By olefin polymerization catalysis suspension by the charging that is arranged on cyclone body
It is rotated during mouth is incorporated into cyclone body and in which；In the presence of revolving force, alkene gathers
Close catalyst bulky grain and discharged by being arranged on the outlet of conical tube pars infrasegmentalis, little of olefin polymerization catalysis
Grain enters collecting chamber by the first overflow pipe, and is discharged by the outlet being arranged on collecting chamber；
The olefin polymerization catalysis suspension is incorporated in cyclone body under conditions of stirring；It is described
The rotating speed of stirring is more than 20rpm.
Preferably, the rotating speed of the stirring is 50-500rpm.
Preferably, the olefin polymerization catalysis suspension is incorporated into cyclone with the pressure of 0.1-0.6MPa
In body.
Preferably, the aperture of the valve being arranged at conical tube pars infrasegmentalis bulky grain outlet is 5-30%.
Preferably, dismountable be additionally provided with the cylinder pipeline section in first overflow pipe
Two overflow pipes, second overflow pipe is closed with the material discharge pipe being arranged in the collecting chamber to be communicated；
Wherein, in the presence of revolving force, the middle granule in olefin polymerization catalysis little particle passes through the first overflow
Pipe enters collecting chamber, and is discharged by the outlet being arranged on collecting chamber；Olefin polymerization catalysis little particle
In fine grained enter the second overflow pipe, it is and close with the second overflow pipe in the collecting chamber by being arranged on
The material discharge pipe for closing connection is discharged.
Olefin polymerization catalysis suspension is classified using cyclone as above, effectively can be controlled
Cyclone upper outlet and the product granularity of lower outlet, it is poly- to alkene so as to meet different alkene production technology
Close the requirement of catalyst granules particle diameter.In the situation for preferably coordinating specific feed pressure and bottom valve aperture
Under, the effect of the classification further can be lifted.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Accompanying drawing is, for providing a further understanding of the present invention, and to constitute the part of description, with
Detailed description below is used for explaining the present invention together, but is not construed as limiting the invention.
In accompanying drawing：
Fig. 1 is a kind of cyclone of the classification specific for olefin polymerization catalysis suspension.
Description of reference numerals
1st, cyclone body 2, collecting chamber 3, the outlet being arranged on collecting chamber
4th, the material discharge pipe 5 being arranged in collecting chamber, the outlet for being arranged on conical tube pars infrasegmentalis
11st, cylinder pipeline section 12, circular cone pipeline section
111st, the first overflow pipe 112, the second overflow pipe
Specific embodiment
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that this place is retouched
The specific embodiment stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of stage division of olefin polymerization catalysis suspension, wherein, the classification
Carry out in cyclone；
The cyclone includes cyclone body 1 and collecting chamber 2, and the cyclone body 1 is from top to bottom
Including cylinder pipeline section 11 and circular cone pipeline section 12；Wherein, it is provided with and the receipts in the cylinder pipeline section 11
Collect the first overflow pipe 111 of 2 airtight connection of room, and the cyclone body 1 and collecting chamber 2 only pass through
First overflow pipe 111 is communicated；
The method includes：By olefin polymerization catalysis suspension by being arranged on entering on cyclone body 1
It is rotated during material mouth 13 is incorporated into cyclone body 1 and in which；In the presence of revolving force,
Olefin polymerization catalysis bulky grain is discharged by being arranged on the outlet 5 of 12 bottom of circular cone pipeline section, and alkene gathers
Close small catalyst particles and collecting chamber 2 is entered by the first overflow pipe 111, and by being arranged on collecting chamber 2
On outlet 3 discharge；
The olefin polymerization catalysis suspension is incorporated in cyclone body under conditions of stirring；It is described
The rotating speed of stirring is more than 20rpm.
The method according to the invention, the olefin polymerization catalysis suspension are referred in olefin polymerization catalysis
In the preparation process of component, vacuum drying treatment is not carried out, and makes what its final products was obtained for suspension.
Wherein, the catalyst component for olefin polymerization has implication well known in the art, refers to particle diameter in 0.1-100
Catalyst granules in micrometer range, key component are titanium, magnesium.Chlorine and electron donor, for example, China
Catalyst group disclosed in patent CN85100997, CN1453298A, ZL200410062290.9 etc.
Point.
The method according to the invention, the concentration of the olefin polymerization catalysis suspension can be normal for this area
The selection of rule, for example, during preparing olefin polymerization catalysis, be not vacuum dried, final to produce
Concentration when product are olefin polymerization catalysis suspension.Preferably, the olefin polymerization catalysis suspension
The concentration of middle olefin polymerization catalysis is preferably 10-60 weight %, more preferably 20-50 weight %.
The method according to the invention, the solvent in the olefin polymerization catalysis suspension can be this area
Conventional inertia alkane washing as above.The aliphatic hydrocarbon of the direct-connected or side chain of preferably C1-C7, more
The aliphatic hydrocarbon of the direct-connected or side chain of preferably C5-C7, for example, the aliphatic hydrocarbon of the direct-connected or side chain of C5,
The aliphatic hydrocarbon of the aliphatic hydrocarbon of direct-connected or side chain, the direct-connected of C7 or side chain of C6.More preferably positive penta
At least one in alkane, isopentane, hexane and heptane, most preferably isopentane and/or hexane.
The method according to the invention, under pressure, by the olefin polymerization catalysis suspension by
The cylinder pipeline section 11 that charging aperture 13 is entered into inside cyclone body 1, due to by cylinder pipeline section 11
Tube wall and the current limliting at top, force suspension to do from top to bottom in cylinder pipeline section 11 and circular cone pipeline section 12
Rotary motion so as to form contour stealth, suspension turn during form powerful centrifugal force, bulky grain
Under the action of the centrifugal force, gradually move to outer wall, and fall along barrel rotation in the presence of making a concerted effort, directly
Extremely discharge from underflow opening 5；Rotation decline contour stealth because by circular cone pipeline section 12 contraction affected and gradually
Collect to center, start to return rising when declining to a certain extent, form one rotation fortune from bottom to top
It is dynamic so as to form inward eddy, little particle with spiral to inward eddy, in cyclone body 1 radially along in
The heart is ascending to 1 wall direction particle diameter of cyclone body, vertically from top to bottom particle diameter by little
To big, the inward eddy of rising enters collecting chamber 2 from the first overflow pipe 111, and by being arranged on collecting chamber
Outlet 3 on 2 is discharged.Thus, complete the classification of olefin polymerization catalysis suspension.
The method according to the invention, in order to further improve the effect of the classification, it is ensured that urge in suspension
The dispersibility of agent component, the olefin polymerization catalysis suspension are preferably added under conditions of stirring
In the cyclone body 1, the speed of the stirring can be 50-500rpm, preferably 50-300rpm,
More preferably 70-200rpm.
The method according to the invention, in order to the olefin polymerization catalysis suspension is formed in cyclone 1
Expected eddy flow, to ensure its grading effect in cyclone 1, the olefin polymerization catalysis suspend
Liquid is preferably incorporated in cyclone body 1, more preferably with 0.2-0.5MPa with the pressure of 0.1-0.6MPa
Pressure, further preferably with the pressure of 0.25-0.4MPa.So stable pressure is to graded product
Granularity and grading effect play the role of positive.
The method according to the invention, it was found by the inventors of the present invention that being arranged on circular cone pipeline section 12 by adjustment
The aperture of the valve at the outlet 5 of bottom, can effectively adjust the granularity of the product of acquisition.Preferably,
In order to obtain being adapted to the catalyst particle size requirement of different alkene polymerization technique, opening for the valve can be with
For 5-30%, preferably 10-30%.
The method according to the invention, first overflow pipe 111 is by being arranged on 2 lower surface of collecting chamber
Opening is closed with collecting chamber 2 to be communicated, wherein, can also arrange in the upper surface of cylinder pipeline section 11 and have
The dividing plate of the opening matched with the opening of 2 lower surface of collecting chamber, so as to be conducive to the first overflow pipe 111
Closed with collecting chamber 2 is communicated.In addition, during eddy flow, for the granule grade particles thing isolated
Material can be smoothly entered in collecting chamber 2.The caliber of first overflow pipe 111 is equal to or less than to be received
The aperture of the opening of collection 2 lower surface of room.
According to one kind of the invention preferred embodiment, in order to effectively adjustment classification products obtained therefrom
Granularity, depth of first overflow pipe 111 in cylinder pipeline section 11 be it is adjustable, it is therefore preferable that
, 111 bottom of the first overflow pipe is also equipped with the regulation dress of 111 depth of the first overflow pipe of scalable
Put.The adjusting means can be the device that can arbitrarily adjust 111 depth of the first overflow pipe, for example,
It can be regulation ring.
The method according to the invention, it is more etc. in order to be divided into olefin polymerization catalysis suspension
Level, according to one kind of the invention preferred embodiment, as a example by being divided into 3 kinds of grades, the cylinder pipeline section
Dismountable second overflow pipe 112 in first overflow pipe 111 is additionally provided with 11, it is described
Second overflow pipe 112 is closed with the material discharge pipe 4 being arranged in the collecting chamber 2 to be communicated, that is,
Say, the granule in second overflow pipe 112 does not enter collecting chamber 2, but is directly discharged by material
Pipe 4 discharges cyclone.
Specifically, under pressure, by the olefin polymerization catalysis suspension by charging aperture 13
The cylinder pipeline section 11 entered into inside cyclone body 1, due to by 11 tube wall of cylinder pipeline section and top
Current limliting, force suspension to do top-down rotary motion in cylinder pipeline section 11 and circular cone pipeline section 12
So as to form contour stealth, powerful centrifugal force is formed during suspension turns, bulky grain is in centrifugation masterpiece
With under, gradually move to outer wall, and fall along barrel rotation in the presence of making a concerted effort, until from underflow opening
5 discharge；The contour stealth that rotation declines gradually is collected to center because affecting by the contraction of circular cone pipeline section 12,
Start to return when declining to a certain extent and rise, one rotary motion from bottom to top is formed so as in being formed
Eddy flow, little particle with spiral to inward eddy, in cyclone body 1 radially along center to cyclone sheet
1 wall direction particle diameter of body is ascending, and particle diameter is ascending from top to bottom vertically, rising
Middle granule in inward eddy enters collecting chamber 2 from the first overflow pipe 111, and by being arranged on collecting chamber 2
On outlet 3 discharge；Fine grained in olefin polymerization catalysis little particle enters the second overflow pipe 112,
And the material discharge pipe 4 with 112 airtight connection of the second overflow pipe by being arranged in the collecting chamber 2
Discharge.Thus, 3 kinds of different grades of olefin polymerization catalysis suspensions have been obtained.
Wherein, the caliber of second overflow pipe 112 is equal to or less than the second material discharge pipe 4
Diameter, the thin particulate matter in order to, during eddy flow, isolate can be discharged by Jing second materials
Pipe 4 is smoothly discharged out.
The method according to the invention, is obtained by the classification of above little particle in order to more subtly adjust
Grain products and fine grained product, the device of 112 depth of the second overflow pipe of the regulation, when the second overflow
When the insertion depth of pipe 112 increases, in the second overflow pipe 112, material fine grained increases, and middle granule is reduced,
Insertion depth reduces, and fine granular materials are reduced, and middle granule materials increase.
Wherein, the present invention is not particularly limited to the adjusting means, as long as which can be realized to the
The regulation of two overflow pipes, 112 depth.For example, the adjusting means can be arranged with the second material
4 outer wall of outlet pipe connects, and arranges runner top is played, and by the rotation of runner, realizes the second overflow pipe
112 lifting.
The method according to the invention, in order to the contour stealth and interior beneficial to classification is formed with cyclone
Eddy flow, the ratio of the height of collecting chamber 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).
The method according to the invention, the taper of the circular cone pipeline section 12 can be 10-20 degree.
The method according to the invention, the method also include being vacuum dried resulting material after classification.Its
In, the vacuum drying method is the conventional selection in this area, and the present invention will not be described here.
Hereinafter will be described the present invention by embodiment.In following examples, following examples
In illustrated as a example by olefin polymerization catalysis suspension is 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,
It is not vacuum dried after simply catalytic component is washed with hexane, is obtained as shown in embodiment 1-10
Olefin polymerization catalyst slurry suspension.
According to the condition shown in embodiment 1-7 and comparative example 1-3, reactor pipeline and cyclone are entered
Mouth pipeline is connected, outlet (abbreviation upper outlet) and be arranged on circle that opening cyclone is arranged on collecting chamber
The outlet (referred to as lower to export) of 12 bottom of Taper Pipe section, under conditions of nitrogen atmosphere pressure and stirring, makes
Suspension is entered in cyclone.Determine
The grain graininess of supernatant liquid.Wherein, Malvern 2000 laser particle size of the measure of grain graininess using Britain
Instrument.The results are shown in Table 2
Table 2
Note：The granularity difference for exporting up and down can be bigger with the effect of Assessment for classification, particle mean size difference, and grading effect is better
As can be seen from Table 2, by embodiment 1-7 compared with comparative example 1-3, using the method for the present invention
Can the product granularity that exports up and down of effective control cyclone, so as to realize polyolefin catalyst component point
Level.By embodiment 1-3 compared with embodiment 4-7, by the aperture of the lower outlet valve of control, suspension
The mixing speed introduced when pressure and suspension are introduced, can further improve grading effect, adjust
The granularity of product.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the present invention, can be to the technical side of the present invention
Case carries out various simple variants, and these simple variants belong to protection scope of the present invention.
It is further to note that each particular technique described in above-mentioned specific embodiment is special
Levy, in the case of reconcilable, can be combined by any suitable means.In order to avoid need not
The repetition wanted, the present invention are no longer separately illustrated to various possible compound modes.
Additionally, combination in any between a variety of embodiments of the present invention, can also be carried out, as long as its
Without prejudice to the thought of the present invention, which should equally be considered as content disclosed in this invention.
Claims (12)
1. a kind of stage division of olefin polymerization catalysis suspension, it is characterised in that the classification exists
Carry out in cyclone；
The cyclone includes cyclone body (1) and collecting chamber (2), the cyclone body (1)
Include cylinder pipeline section (11) and circular cone pipeline section (12) from top to bottom；Wherein, the cylinder pipeline section (11)
The first overflow pipe (111) with the collecting chamber (2) airtight connection, and the cyclone are provided with inside
Body (1) and collecting chamber (2) are only communicated by the first overflow pipe (111)；
The method includes：By olefin polymerization catalysis suspension by being arranged on cyclone body (1)
Charging aperture (13) be incorporated into cyclone body (1) in and be rotated in which；In rotation
In the presence of power, olefin polymerization catalysis bulky grain is by being arranged on the outlet of circular cone pipeline section (12) bottom
(5) discharge, olefin polymerization catalysis little particle passes through the first overflow pipe (111) into collecting chamber (2),
And discharged by the outlet (3) being arranged on collecting chamber (2)；
Wherein, the olefin polymerization catalysis suspension is incorporated into cyclone body under conditions of stirring
(1) in；The rotating speed of the stirring is more than 20rpm.
2. method according to claim 1, wherein, the rotating speed of the stirring is 50-500rpm.
3. method according to claim 1 and 2, wherein, the olefin polymerization catalysis suspend
Liquid is incorporated in cyclone body (1) with the pressure of 0.1-0.6MPa.
4. the method according to any one in claim 1-3, wherein, it is arranged on circular cone pipeline section
(12) aperture of the valve at outlet (5) place of bottom is 5-30%.
5. method according to claim 1, wherein, first overflow pipe (111) is by setting
Put that the opening in collecting chamber (2) lower surface is closed with collecting chamber (2) to be communicated, first overflow pipe (111)
Caliber be equal to or less than collecting chamber (2) lower surface opening aperture.
6. method according to claim 1 or 5, wherein, under first overflow pipe (111)
Portion is also equipped with the adjusting means of scalable the first overflow pipe (111) depth.
7. method according to claim 1, wherein, also sets up in the cylinder pipeline section (11)
There is dismountable second overflow pipe (112) in first overflow pipe (111), described second
Overflow pipe (112) is closed with the material discharge pipe (4) being arranged in the collecting chamber (2) to be communicated；
Wherein, in the presence of revolving force, the middle granule in olefin polymerization catalysis little particle passes through first
Overflow pipe (111) is into collecting chamber (2), and the outlet (3) by being arranged on collecting chamber (2)
Discharge；Fine grained in olefin polymerization catalysis little particle enters the second overflow pipe (112), and by setting
Put the material discharge pipe (4) with the second overflow pipe (112) airtight connection in the collecting chamber (2)
Discharge.
8. method according to claim 7, wherein, the aperture of second overflow pipe (112)
Equal to or less than the aperture of the material discharge pipe being arranged in the collecting chamber (2).
9. the method according to claim 7 or 8, wherein, the cyclone includes and described
The adjusting means of regulation the second overflow pipe (112) depth of two overflow pipes (112) outer wall connection.
10. method according to claim 1, wherein, collecting chamber (2), cylinder pipeline section (11)
Ratio with the height of circular cone pipeline section (12) is 10-20：10-20：25-35.
11. methods according to claim 1, wherein, the taper of the circular cone pipeline section (12) is
10-20 degree.
12. methods according to claim 1-11, wherein, the method is also included institute after classification
Obtain material to be vacuum dried.
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| CN107141376A (en) * | 2016-03-01 | 2017-09-08 | 中国石油化工股份有限公司 | The stage division and olefin polymerization catalysis suspension and olefin polymerization catalysis of a kind of olefin polymerization catalysis |
| 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 |
| WO2020109452A1 (en) * | 2018-11-30 | 2020-06-04 | Borealis Ag | Washing process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107141376A (en) * | 2016-03-01 | 2017-09-08 | 中国石油化工股份有限公司 | The stage division and olefin polymerization catalysis suspension and olefin polymerization catalysis of a kind of olefin polymerization catalysis |
| WO2020109452A1 (en) * | 2018-11-30 | 2020-06-04 | Borealis Ag | Washing process |
| 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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