EP4374955A1 - Dispositif de mélange pour système de réacteur en polyéthylène - Google Patents

Dispositif de mélange pour système de réacteur en polyéthylène Download PDF

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Publication number
EP4374955A1
EP4374955A1 EP22208841.1A EP22208841A EP4374955A1 EP 4374955 A1 EP4374955 A1 EP 4374955A1 EP 22208841 A EP22208841 A EP 22208841A EP 4374955 A1 EP4374955 A1 EP 4374955A1
Authority
EP
European Patent Office
Prior art keywords
pipe
annular space
mixing device
section
flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP22208841.1A
Other languages
German (de)
English (en)
Inventor
Sara MARCOS ORTEGA
Hua Bai
Raymond Gregory WISSINGER
Bas Eugène Hans Megens
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SABIC Global Technologies BV
Original Assignee
SABIC Global Technologies BV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SABIC Global Technologies BV filed Critical SABIC Global Technologies BV
Priority to EP22208841.1A priority Critical patent/EP4374955A1/fr
Priority to PCT/EP2023/081257 priority patent/WO2024110200A1/fr
Publication of EP4374955A1 publication Critical patent/EP4374955A1/fr
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/10—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
    • B01F25/103—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components with additional mixing means other than vortex mixers, e.g. the vortex chamber being positioned in another mixing chamber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/10—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
    • B01F25/104—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components characterised by the arrangement of the discharge opening
    • B01F25/1041—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components characterised by the arrangement of the discharge opening the mixing chamber being vertical with the outlet tube at its upper side
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/23—Mixing by intersecting jets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4332—Mixers with a strong change of direction in the conduit for homogenizing the flow

Definitions

  • the present invention relates to a mixing device.
  • the present invention further relates to the use of such mixing device in a high pressure ethylene reactor system and a process for the preparation of an ethylene-based polymer using such reactor system under high pressure conditions.
  • LDPE low density polyethylene
  • LDPE low density polyethylene
  • LDPE can be used alone, blended or co extruded for a variety of packaging, construction, agricultural, industrial and consumer applications.
  • the largest application of LDPE is in films produced for example by the blown or cast extrusion process in both mono and co extrusions. Films made with LDPE exhibit good optical properties, strength, flexibility, seal ability and chemical inertness.
  • the end-use applications include packaging of bakery items, snack foods, consumer durables, disposable diapers, textiles, agricultural film and shrink film.
  • Polyethylene such as LDPE can be prepared via free radical polymerization.
  • LDPE low density polyethylene
  • WO2010/081684 describes a process for the preparation of polyethylene in a high pressure reactor with at least two spatially separated initiator injection points by polymerizing ethylene and optionally further monomers in the presence of at least two different mixtures of free-radical polymerization initiators.
  • the process comprises a) providing at least two different initiators as solution in a suitable solvent or in liquid state, b) mixing the initiators and optionally additional solvent in at least two static mixers and c) feeding each of the mixtures to a different initiator injection point of the high pressure reactor.
  • static mixers give a desirable degree of mixing
  • the structure of static mixers is rather complex, resulting in a higher cost for fabrication.
  • the present invention provides a mixing device comprising:
  • the mixing device according to the invention is a mixing device for making a mixture of liquid substances, preferably a mixture of liquid substances comprising initiators, additives and/or solvents for the preparation of an ethylene-based polymer.
  • the mixing device is particularly suitable for making such mixture in a flow having a Reynolds number of at most 1000.
  • the mixing device according to the invention can make a mixture in a generally laminar low.
  • the device according to the invention provides a desired degree of mixing of liquid substances comparable to known static mixers, while having a simple structure mainly using commonly available pipes such as standard pipes.
  • the mixing device according to the invention may be designed to be more compact than known static mixers and achieve a comparable degree of mixing. Further, the mixing device according to the invention may achieve a comparable degree of pressure drop and residence time as known static mixers.
  • the mixing device comprises a supply section and a pipe-in-pipe section.
  • the pipe-in-pipe section comprises an outer pipe and an inner pipe.
  • a flow of liquid substances is supplied from the supply section to the pipe-in-pipe section via the outer flow inlet provided on the outer pipe of the pipe-in-pipe section. The flow enters the annular space between the outer pipe and the inner pipe, and then enters the inner pipe via the inner flow inlets.
  • the outer flow inlet is provided at a lower vertical position than the inner flow inlets and is provided such that a tangential flow is generated in the annular space.
  • a tangential flow is generated in the annular space.
  • the inner flow inlets may be formed by two passages through a circumferential wall of the inner pipe.
  • the number of the inner flow inlets may be two, three, four or more.
  • the at least two inner flow inlets comprise two inner flow inlets spaced apart in circumferential direction over an angle of between 150 and 210 degrees, preferably of 180 degrees, with respect to each other.
  • the two inner flow inlets may herein sometimes be referred as facing each other.
  • Such positioning of the inner flow inlets increases the effect of the impinging flows on mixing.
  • the at least two inner flow inlets consist of two inner flow inlets facing each other.
  • the at least two inner flow inlets consist of four inner flow inlets consisting of two pairs of two inner flow inlets facing each other.
  • the vertical distance between the bottom end of the annular space and the top end of the annular space is 100 to 300 mm. This ensures a sufficient distance for the upward circulating flow to induce good mixing while keeping the size of the mixing device to become too large. More preferably, the height of the annular space is 100 to 200 mm. This has a further advantage of decreasing the residence time.
  • the vertical distance between the outer flow inlet and the bottom end of the annular space is 20% of the vertical distance between the bottom end of the annular space and the top end of the annular space (height of the annular space).
  • the vertical distance between the inner flow inlets and the top end of the annular space is 20% of the vertical distance between the bottom end of the annular space and the top end of the annular space.
  • the outer pipe may have an inner diameter ID1, for example of 20 to 40 mm.
  • the inner pipe may have an inner diameter ID2, for example of 5.0 to 15 mm.
  • the inner pipe may have an outer diameter OD2, for example of 15 to 20 mm.
  • ID1 is larger than OD2.
  • ID1-OD2 is 5.0 to 25 mm.
  • outer pipe and the inner pipe allow the use of standard pipe schedule (e.g. 1", 1 ⁇ 2", 3/8", 1/8" SCH40) and lowers the cost of fabrication.
  • the inner flow inlets may have a diameter IFD, for example of 5.0 to 10 mm.
  • the outer flow inlet may have a diameter of OFD, for example of 5.0 to 10 mm.
  • Such diameters of the inner flow inlets and the outer flow inlet provides desired velocity and momentum for mixing action while lowering the risk of plugging.
  • At least one, preferably both, of the following conditions are satisfied:
  • the ratio of the vertical distance between the bottom end of the annular space and the top end of the annular space to ID1 3.0 to 20, preferably 4.0 to 10.
  • [ID1-OD2]/OFD is more than 1.0.
  • [ID1-OD2]/IFD is more than 1.0.
  • the closed top end of the annular space is configured to be removable, i.e. the closed top end of the annular space is provided with a structure or mechanism which allows easy attachment to and detachment from the outer pipe and inner pipe. This allows easy cleaning of the annular space.
  • the supply section comprises a supply pipe having a first, vertically extending pipe section of a first inner diameter, followed, in a direction of the flow, by a second, vertically extending pipe section of a second, reduced inner diameter, which second pipe section in turn is followed by a third, horizontally extending pipe section of the second inner diameter, wherein the horizontally extending pipe connects to the outer flow inlet.
  • the transition from the first, vertically extending pipe section to the second, vertically extending pipe section may be achieved by a section in which the inner diameter gradually decreases (herein sometimes referred as a diameter reducer) from the first inner diameter to the second inner diameter.
  • This reduction in the inner diameter increases the velocity of the flow supplied to the outer flow inlet and achieves a higher degree of mixing.
  • the diameter reducer preferably has an inner wall in the shape of a truncated cone.
  • the inner wall of the diameter reducer may be angled by e.g. 30 to 60° such as 45° with respect to the longitudinal axis of the first and the second pipe sections.
  • the ratio of the first inner diameter to the second, reduced inner diameter is at least 1.1, preferably at least 1.5, more preferably 1.8 to 3.0.
  • the transition from the second, vertically extending pipe section to the third, horizontally extending pipe section may be achieved by an elbow section, preferably a curved elbow section.
  • the degree of mixing increases at this elbow section.
  • the mixing device further comprises a pre-mixing section arranged upstream of the supply section, wherein the pre-mixing section comprises a main supply pipe section connecting to the vertically extending pipe section and at least two initiator supply pipe sections connecting to the main supply pipe section along the main supply pipe section.
  • the pre-mixing section comprises a main supply pipe section connecting to the vertically extending pipe section and at least two initiator supply pipe sections connecting to the main supply pipe section along the main supply pipe section.
  • the main supply pipe section comprises a horizontally extending part and the two or more initiator supply pipes extend vertically and connect to the horizontally extending part.
  • the invention further provides a process for making a mixture of liquid substances, preferably a mixture of liquid substances comprising initiators, additives and/or solvents for the preparation of an ethylene-based polymer, comprising feeding the liquid substances to the mixing device according to the invention.
  • the liquid substances comprises initiators and solvents of the initiators.
  • the initiators may be fed to the mixing device as a solution of the initiators in a solvent.
  • the mixing device is preferably operated at a pressure of at most 10 bar, preferably 1.0 to 4.0 bar.
  • the invention further relates to a reactor system comprising the mixing device according to the invention and a polymerization reactor for high pressure polymerization of an ethylene-based polymer, the polymerization reactor comprising an ethylene inlet for ethylene and a liquid mixture inlet connected to the outlet of the mixing device.
  • the polymerization reactor may comprise further various inlets for other components such as optional comonomer(s), and other elements necessary for high pressure polymerization.
  • the polymerization reactor is per se well-known, e.g. from WO2010081684 and is not described herein in detail.
  • the invention further relates to a high pressure polymerization process for the preparation of an ethylene-based polymer using the reactor system according to the invention, comprising feeding the liquid substances to the mixing device to obtain the mixture and feeding the mixture to the liquid mixture inlet and feeding ethylene to the ethylene inlet.
  • the process comprises polymerizing ethylene and optional comonomers in the presence of the mixture at temperatures of 100 to 350 °C and pressures of 160 to 350 MPa.
  • the process comprises pressurizing the mixture obtained by the mixing device to a pressure of 160 to 350 MPa before feeding it to the liquid mixture inlet.
  • Suitable comonomers include ⁇ , ⁇ -unsaturated carboxylic acids, in particular but not limited to maleic acid, fumaric acid, itaconic acid, acrylic acid, methacrylic acid and crotonic acid;
  • the initiator used in the present invention is typically an organic peroxide.
  • Suitable organic peroxides include for example peroxyester, peroxyketone, peroxyketal and peroxycarbonate such as for example di-2-ethylhexyl-peroxydicarbonate, diacetylperoxydicarbonate, dicyclohexyl-peroxydicarbonate, tert. -amylperpivalate, cumyl perneodecanoate, tert. - butylpemeodecanoate, tert. -butyl perpivalate, tert. - butylpermaleinate, tert.
  • the suitable solvents used in the present invention are those for making a solution of the initiators.
  • suitable solvents are alcohols, ketones and aliphatic hydrocarbons, in particular octane, decane and isododecane and also other saturated C7 to C30 hydrocarbons, in particular linear C7 to C30 alkanes.
  • the solution may comprise the initiators in proportions of from 2 to 65% by weight, preferably from 5 to 40% by weight.
  • the term 'comprising' does not exclude the presence of other elements.
  • a description on a product/composition comprising certain components also discloses a product/composition consisting of these components.
  • the product/composition consisting of these components may be advantageous in that it offers a simpler, more economical process for the preparation of the product/composition.
  • a description on a process comprising certain steps also discloses a process consisting of these steps. The process consisting of these steps may be advantageous in that it offers a simpler, more economical process.
  • Figure 1 shows a front view of an embodiment of a mixing device according to the invention.
  • the mixing device comprises a pre-mixing section 300, a supply section 200 and a pipe-in-pipe section 100.
  • the pre-mixing section 300 comprises a main supply pipe section consisting of a vertically extending part 310 and a horizontally extending part 320.
  • Sub-supply pipes 331-335 are provided along the length of the horizontally extending part 320 of the main supply pipe.
  • the vertically extending part 310 of the main supply pipe section is connected to the supply section 200.
  • Figure 2A and 2B show, in vertical cross-section, an enlarged view of part of the mixing device of Figure 1 .
  • the supply section 200 and the pipe-in-pipe section 100 are shown.
  • Figure 2A shows the pipe-in-pipe section 100 in more detail.
  • Figure 2B shows the supply section 200 in more detail.
  • the supply section 200 comprises a supply pipe having a first, vertically extending pipe section 210 of a first inner diameter.
  • the first, vertically extending pipe section 210 is followed, in a direction of the flow, by a second, vertically extending pipe section 220 of a second, reduced inner diameter.
  • a diameter reducer 240 is present between the first, vertically extending pipe section 210 and the second, vertically extending pipe section 220, in which the inner diameter decreases from the first inner diameter to the second inner diameter.
  • the diameter reducer 240 has an inner wall in the shape of a truncated cone.
  • the second, vertically extending pipe section 220 connects to a third, horizontally extending pipe section 230 of the second inner diameter.
  • a curved elbow section 250 is present between the second, vertically extending pipe section 220 and the third, horizontally extending pipe section 230.
  • the third, horizontally extending pipe section 230 is connected to the pipe-in-pipe section 100.
  • the pipe-in-pipe section 100 comprises an outer pipe 110 extending vertically and an inner pipe 120 having a closed top end and having an outlet for the mixture at a bottom end.
  • the inner pipe 120 is arranged concentrically to the outer pipe 110 inside the outer pipe 110 such that an annular space 130 having a closed top end and a closed bottom end is formed between the outer pipe 110 and the inner pipe 120.
  • the inner pipe 120 is provided with two inner flow inlets 121, 122 for receiving a flow from the annular space 130 into the inner pipe 120.
  • the outer pipe 110 is provided with an outer flow inlet 111 for receiving a flow from the supply section 200 into the annular space 130.
  • the third, horizontally extending pipe section 230 of the supply section 200 connects to the outer flow inlet 111.
  • the outer flow inlet 111 is provided such that a tangential flow is generated in the annular space 130.
  • the two inner flow inlets 121, 122 are provided higher than the outer flow inlet 111, i.e. the vertical distance from the closed bottom end of the annual space 130 to two inner flow inlets 121, 122 is larger than the vertical distance from the closed bottom end of the annual space 130 to the outer flow inlet 111.
  • Figure 3 is a top cross section of Figure 2B . It can be understood that the outer flow inlet 111 is provided at such a position of the outer pipe 110 that a tangential flow is generated in the annular space 130.
  • Figure 4 illustrates a cross section of an example of a mixing device not according to the invention.
  • the mixing device has the same pre-mixing section as the pre-mixing section 300 shown in Figure 1 .
  • the mixing device of Figure 4 comprises a static mixer.
  • the different types of initiators fed to the vertically extending sub-pipes 331 to 335 contact each other at the junctions between and the vertically extending sub-pipes 331 to 335 and the horizontally extending part 320 of the main supply pipe section and a flow comprising the initiators flows down the vertically extending pipe part 310 of the main supply pipe section.
  • the flow comprising the initiators from the pre-mixing section 300 flows down to the supply pipe of the supply section 200.
  • the flow comprising the initiators enters the first, vertically extending pipe section 210 of a first inner diameter and continues to the diameter reducer 240 at which mixing occurs.
  • the flow enters the second, vertically extending pipe section 220 and continues to the third, horizontally extending pipe section 230 via the curved elbow section 250 at which mixing occurs.
  • the flow enters the outer flow inlet 111 of the outer pipe 110 from the third, horizontally extending pipe section 230.
  • the mixing device of Figure 4 has the same pre-mixing section as that in Figure 1 .
  • the static mixer of Figure 4 has a total length of 52 cm, of which the total length of mixing elements is 42 cm.
  • Initiators four different peroxides having varying densities in the range of 760 to 815 kg/m 3 (at 20 °C) and varying viscosities in the range of 1.1 to 2.57 mPas (at 20 °C).
  • Solvent density of 748 kg/m 3 at 20 °C and viscosity of 1.5 mPas at 20 °C
  • the peroxides are fed to the vertically extending sub-pipes 331 to 334 as a 30% concentration solution in the solvent.
  • the solvent is fed to the vertically extending sub-pipe 335.
  • the feed velocities and Reynolds numbers of the flows are selected such that the flow in the pre-mixing section would be laminar.
  • the values of Coefficient of variation (CoV) were calculated as a factor of the location in the mixing device.
  • the mixing device according to the invention having a pipe-in-pipe section with a much lower length (152.0 mm) than the mixing device having a static mixer with a length (520 mm) achieves comparable degree of mixing.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
EP22208841.1A 2022-11-22 2022-11-22 Dispositif de mélange pour système de réacteur en polyéthylène Pending EP4374955A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP22208841.1A EP4374955A1 (fr) 2022-11-22 2022-11-22 Dispositif de mélange pour système de réacteur en polyéthylène
PCT/EP2023/081257 WO2024110200A1 (fr) 2022-11-22 2023-11-09 Dispositif de mélange pour système de réacteur en polyéthylène

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP22208841.1A EP4374955A1 (fr) 2022-11-22 2022-11-22 Dispositif de mélange pour système de réacteur en polyéthylène

Publications (1)

Publication Number Publication Date
EP4374955A1 true EP4374955A1 (fr) 2024-05-29

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EP22208841.1A Pending EP4374955A1 (fr) 2022-11-22 2022-11-22 Dispositif de mélange pour système de réacteur en polyéthylène

Country Status (2)

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EP (1) EP4374955A1 (fr)
WO (1) WO2024110200A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6054046A (en) * 1997-04-02 2000-04-25 Nelson; William R. System for re-circulating a gas mixture to treat liquids
US6361688B1 (en) * 1997-04-02 2002-03-26 William R. Nelson Treating a liquid with a gas
US7097160B2 (en) * 2004-10-13 2006-08-29 Ozone Safe Food, Incorporated Apparatus for treating a liquid with a gas
WO2010081684A1 (fr) 2009-01-16 2010-07-22 Basell Polyolefine Gmbh Polymérisation d'éthylène dans un réacteur à haute pression avec une introduction améliorée d'initiateurs

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6054046A (en) * 1997-04-02 2000-04-25 Nelson; William R. System for re-circulating a gas mixture to treat liquids
US6361688B1 (en) * 1997-04-02 2002-03-26 William R. Nelson Treating a liquid with a gas
US7097160B2 (en) * 2004-10-13 2006-08-29 Ozone Safe Food, Incorporated Apparatus for treating a liquid with a gas
WO2010081684A1 (fr) 2009-01-16 2010-07-22 Basell Polyolefine Gmbh Polymérisation d'éthylène dans un réacteur à haute pression avec une introduction améliorée d'initiateurs

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