Classifications

• • 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
  • B01F23/47—Mixing liquids with liquids; Emulsifying involving high-viscosity liquids, e.g. asphalt
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
  • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
  • B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
  • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
  • B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
  • B01F27/902—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms  cooperating with intermeshing elements fixed on the receptacle walls
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F2215/00—Auxiliary or complementary information in relation with mixing
  • B01F2215/04—Technical information in relation with mixing
  • B01F2215/0413—Numerical information
  • B01F2215/0436—Operational information
  • B01F2215/045—Numerical flow-rate values
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F2215/00—Auxiliary or complementary information in relation with mixing
  • B01F2215/04—Technical information in relation with mixing
  • B01F2215/0413—Numerical information
  • B01F2215/0436—Operational information
  • B01F2215/0468—Numerical pressure values
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F2215/00—Auxiliary or complementary information in relation with mixing
  • B01F2215/04—Technical information in relation with mixing
  • B01F2215/0413—Numerical information
  • B01F2215/0436—Operational information
  • B01F2215/0472—Numerical temperature values
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F2215/00—Auxiliary or complementary information in relation with mixing
  • B01F2215/04—Technical information in relation with mixing
  • B01F2215/0413—Numerical information
  • B01F2215/0436—Operational information
  • B01F2215/0481—Numerical speed values
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F2215/00—Auxiliary or complementary information in relation with mixing
  • B01F2215/04—Technical information in relation with mixing
  • B01F2215/0413—Numerical information
  • B01F2215/0486—Material property information
  • B01F2215/0495—Numerical values of viscosity of substances
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
  • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
  • B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
  • B01F27/2721—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces provided with intermeshing elements
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
  • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
  • B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
  • B01F27/2722—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces provided with ribs, ridges or grooves on one surface
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
  • B01F33/30—Micromixers
• • 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
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S366/00—Agitating
  • Y10S366/01—Micromixers: continuous laminar flow with laminar boundary mixing in the linear direction parallel to the fluid propagation with or without conduit geometry influences from the pathway
• • 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
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S366/00—Agitating
  • Y10S366/02—Micromixers: segmented laminar flow with boundary mixing orthogonal to the direction of fluid propagation with or without geometry influences from the pathway
• • 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
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S366/00—Agitating
  • Y10S366/03—Micromixers: variable geometry from the pathway influences mixing/agitation of non-laminar fluid flow
• • 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
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S366/00—Agitating
  • Y10S366/04—Micromixers: with application of energy to influence mixing/agitation, e.g. magnetic, electrical, e-m radiation, particulate radiation, or ultrasound

Definitions

• the present invention relates to a method for continuously and dynamically mixing at least two fluids. This process is particularly suitable for chemical reactions with rapid and / or complex kinetics, such as anionic polymerizations.
• the invention also relates to a micromixer capable of implementing this method.
• one of the most commonly used techniques for mixing two or more liquids consists in using a closed, semi-closed or open tank, equipped with a mechanical agitator of the propeller, turbine or other type, and in injecting one or more reagents in the tank.
• Tangential jet mixers (usable in particular for anionic polymerizations as described in EP-A- 0749987) or the RIM heads (“Reaction Injection Molding”) are mixers with confined jets, that is to say jets in contact with the wall of the mixer. They are very effective, but cause blockages when high polymer contents are involved, or require the injection of products by pumps resistant to high pressures (several hundred bars). In addition, RIM heads require discontinuous operation.
• EP 824 106 is a process for the preparation of cellulose particles having cationic and / or anionic groups, in which a dynamic mixer is used comprising a stator and a rotor provided with shaped blades. cylindrical.
• a dynamic mixer comprising a stator and a rotor provided with shaped blades.
• the disadvantage of such a mixer is that the material aggregates are subjected to multiple velocity gradients which stretch and contract them randomly, generating very large concentration gradients.
• the present invention therefore aims to provide a method and a mixer for dynamically and continuously mixing at least two fluids. It advantageously applies to the mixture of reactive fluids and in particular to the anionic polymerization of at least one (meth) acrylic monomer.
• the subject of the invention is a method comprising the following steps: a) the rotor of a micromixer is rotated, comprising:
• a rotor comprising a shaft provided with blades distributed in groups, the blades of each group being arranged around the shaft in the same plane perpendicular to the longitudinal axis of the tree, and the groups of blades being spaced apart from one another others along the longitudinal axis of the tree;
• stator in the form of a hollow cylinder capable of receiving the rotor, this stator comprising, at one end of its longitudinal axis, at least one inlet for a first fluid, at least one inlet for a second fluid and, to the other end of its longitudinal axis, an outlet for micromixing fluids; b) the fluids are introduced into the micromixer; and c) a micromixture of the fluids is recovered at the outlet of the micromixer.
• the subject of the invention is also a micromixer comprising: a rotor comprising a shaft provided with blades distributed in groups, the blades of each group being arranged around the tree in the same plane perpendicular to the longitudinal axis of the tree, and the groups of blades being spaced from each other along the longitudinal axis of the shaft; and a stator substantially in the form of a hollow cylinder capable of receiving the rotor, this stator comprising, at one end of its longitudinal axis, at least one inlet for a first fluid, at least one inlet for a second fluid and, at the other end of its axis longitudinal, one outlet for micromixing fluids.
• Such a micromixer has the double advantage of not inducing a significant pressure drop and of being able to be easily adjusted so as to adapt to changes in operating conditions such as flow rates and viscosities. It suffices to change the speed of rotation of the rotor, the shape of the blades or counter blades, or their number. In addition, the efficiency of the mixture does not decrease along the longitudinal axis of the rotor as is the case in a conventional mixer in the form of a tube.
• micromixer according to the invention is very effective even when the viscosities are high.
• a polymerization process in which the dynamic mixing process and the micromixer according to the invention are implemented.
• This process comprises the following stages: (i) rotational drive of the rotor of a micromixer comprising: a rotor comprising a shaft provided with blades distributed in groups, the blades of each group being arranged around the shaft in the same perpendicular plane to the longitudinal axis of the shaft, and the groups of blades being spaced from one another along the longitudinal axis of the shaft; a stator in the form of a hollow cylinder capable of receiving the rotor, this stator comprising, at one end of its longitudinal axis, at least one inlet for a first fluid, at least one inlet for a second fluid and, at the other end from its longitudinal axis, an outlet for micromixing fluids;
• FIGS. 6 and 7 are curves showing the influence of the speed of rotation of the rotor of the micromixer according to the invention, on the quality of the product obtained, at constant fluid flow rates;
• FIGS. 6 and 7 are curves showing the influence of the speed of rotation of the rotor of the micromixer according to the invention, on the quality of the product obtained, at constant fluid flow rates;
• the dynamic and continuous mixing process according to the invention has been described generally above. It can be used to mix more than two fluids. However, for reasons of simplicity, it will now be detailed for implementation with two fluids.
• the rotor can be rotated at a speed of up to 30,000 rpm.
• a rotor rotation speed greater than 5,000 revolutions / min is chosen, in order to obtain a homogeneous mixture and less than 20,000 revolutions / min, so as to limit the phenomena of heating.
• the introduction of the first and second fluids is preferably carried out at at least two places diametrically opposite with respect to the axis of the rotor of the micromixer.
• the method according to the invention is generally implemented with a temperature of the fluids between -100 ° C and 300 ° C. It is preferably used with temperatures between -80 ° C and 110 ° C.
• It can be implemented with fluid pressures between 0.1 and 100 bar absolute. Preferably, it is implemented with pressures between 1 and 50 bar absolute.
• the fluids can be introduced into the mixer at a flow rate between 1 g / h and 10,000 kg / h.
• the flow rate of the fluids is between 1 kg / h and 5,000 kg / h.
• the ratio of mass flow rates of fluids can be very variable. It is generally between 0.01 and 100 preferably between 0.1 and 10.
• the method according to the invention can make it possible to mix fluids whose viscosity is between 1 mPa.s and 10 3 Pa.s. Preferably, this viscosity is between 10 mPa.s and 10 Pa.s.
• the method according to the invention is implemented with residence times of the fluids in the micromixer generally greater than 1 ms.
• the operating conditions are adjusted so that the residence time is between 5 ms and 10 s.
• the mixing process which has just been described is particularly suitable for micromixing reactive fluids. It preferably applies to reactive liquids.
• the mixing process according to the invention can constitute part of a more general polymerization process.
• This polymerization process according to the invention applies in particular to the mixture of reactive fluids intended for anionic polymerization, at least one of which comprises at least one (meth) acrylic monomer.
• (meth) acrylic monomer mention may therefore be made in particular of acrylic anhydride, methacrylic anhydride, methyl, ethyl, propyl, n- and tert-butyl, ethyl hexyl, nonyl, 2-dimethyl amino ethyl and methyl, ethyl, propyl and n- and tert-butyl methacrylates, ethyl hexyl, nonyl, 2-dimethyl amino ethyl.
• the actual polymerization can occur outside the micromixer according to the invention, or it can start inside the micromixer and continue outside this micromixer, for example in a suitable reactor.
• the method according to the invention can be implemented in any polymerization installation. Mention may be made in particular of that illustrated by FIG. 1 on page 14 of the aforementioned patent application EP 749 987.
• the method according to the invention can in particular be implemented for preparing polymers according to the methods described in the European patent applications published under the numbers EP 749 987, EP 722 958 and EP 524 054.
• micromixer according to the invention is capable of implementing the process which has just been described.
• the micromixer according to the invention comprises a rotor 1 comprising a shaft 2 of substantially cylindrical shape provided with blades 3.
• blades 3 are divided into groups 3a, 3b, 3c, 3d, 3e, 3f and 3g, the blades of each group are arranged around the shaft 2, in the same plane perpendicular to the longitudinal axis of the shaft 2 and the groups of blades are spaced from each other along the longitudinal axis of the shaft 2. This is clearly visible in FIG. 1, where each group 3a to 3g appears as a disc. In Figure 2, the rotor is shown in top view. We therefore see a group 3a of six blades 3. The blades are arranged regularly around the tree, in a star and each is inclined by 60 degrees relative to its two closest neighbors. The blades are substantially identical to each other and are shaped like a blade. One of their longitudinal sides forms a tangent to the circumference of the shaft 2. The free end of each blade 3 can be tapered.
• a rotation of the shaft of 60 degrees allows a blade to occupy the place occupied by one of its two neighbors before this rotation.
• the blades 3 of a group of blades 3a are preferably aligned respectively with the blades of another group of blades 3b along the longitudinal axis of the rotor, so that when viewed from above and looking in the direction from the longitudinal axis of rotor 1 ( Figure 2), you can only see one group of blades, the others being eclipsed below.
• the rotor 1 is intended to cooperate with a stator 4 which is seen first of all in FIG. 1.
• This stator 4 has substantially the shape of a hollow cylinder. It has dimensions which make it suitable for accommodating at least part of the rotor 1.
• the stator 4 comprises at one end of its longitudinal axis, an inlet 5 for a first fluid, an inlet 6 for a second fluid and at the other end of its longitudinal axis, an outlet 7 for the micromixing of fluids.
• the inlet 6 is diametrically opposite with respect to the inlet 5.
• the stator 4 comprises discs 8 which can be seen taken out of the stator in FIG. 1.
• Each disc 8 has in its center a recess 9 which allows it to accommodate a group of blades 3a or 3b at 3g, while allowing the latter to rotate in union with the rotor 1.
• the recess 9 has the form d 'a circular hole, part of which is occupied by extensions 10 of the disc 8. These extensions 10 project relative to the wall 11 of the disc 8 delimiting the recess 9.
• each disc 8 therefore comprises its group of six counter-blades 10 arranged regularly on the circumference of the wall 11. Each counter-blade is inclined by 60 degrees relative to its two closest neighbors. As for the blades 3 of the rotor 1, a rotation of a disc 8 by 60 degrees allows a counter blade 10 to occupy the space occupied by one of its two neighbors before this rotation.
• the counter-blades 10 of a group of counter-blades 10 are also preferably aligned respectively with the counter-blades of another group of counter-blades 10 along the longitudinal axis of the stator, so that seen from above and looking in the direction of the longitudinal axis of the stator 4 (FIG. 3), one can only see one group of counter blades 10, the others being eclipsed below.
• FIG. 4 shows, in top view, a group of blades 3 of the rotor 1 around which a disc 8 has been placed.
• the counter-blades 10 have a thickness less than that of the body 12 of the disc 8 which they extend.
• the discs 8 are in contact with each other, stacked inside the stator 4, so that each group of blades 3 (except the first and the last) is inserted between two groups of counter blades 10.
• each group of blades 3 can rotate freely, that is to say without being hindered by the groups of adjacent counter-blades 10.
• the blades 3 and the counter blades 10 are preferably inclined in opposite directions, so that during the rotation of the rotor, they approach each other like the blades of a chisel, and thus generate a shear fluids.
• a space 13 is provided, in the longitudinal direction, between each group of blades 3 and the group of counter blades 10 which precedes it (except in the case of the first group of blades located near the stator input) and another space 14 is also provided between each group of blades 3 and the group of counter-blades 10 which follows it (except in the case of the last group of blades located near the output of the stator).
• the spaces 15 have a minimum size in the case of FIG. 4, where the side of each blade 3 which is tangent to the shaft 2 is arranged parallel to the longitudinal sides of a counter-blade 10.
• the spaces 15 have a size maximum when, looking in the direction of the axis of the shaft 2, the blades 3 are superimposed on the counter-blades 10 and eclipse them.
• a bore 16 can be provided through the thickness of the discs 8 and in the stator 4, so that a rod or a screw can be introduced therein.
• stator 4 further comprises a fluid distributor 17 substantially in the form of a washer and located at the level of the stator 4 supply and upstream of the discs.
• the distributor 17 comprises at least one orifice for the first fluid and at least one other orifice for the second fluid, these orifices being drilled radially in the washer and communicate respectively with the inputs 5 and 6 of the stator 4. Thus, the fluids entering through the inputs 5 and 6 are led through the orifices of the distributor 17 near
• the central hole 18 of the distributor 17 has a diameter substantially equal to that of the circular hole of a disc 18 delimited by the wall 11 of this disc. It follows that when the rotor 1 is mounted in the stator 4, a first group of blades 3 of the rotor 1 can possibly be inserted inside the central hole 18 and rotate there freely.
• the distributor 17 At its lower end, that is to say that opposite to that which is in contact with a disc 18, the distributor 17 optionally has a bore 19 intended to receive an annular seal 20 which is also in contact with the shaft 2 rotor 1.
• the stator 4 is generally fixed on a support 21 in a conventional manner by means of screws (not shown).
• the rotor 1 is generally driven in rotation in a conventional manner by means of rotation drive such as an electric motor (not shown). However, it is preferable to choose a motor capable of maintaining a constant speed of rotation, independent of the resistive torque that it can undergo (eg milling motor).
• the direction of rotation of the rotor is that of the inclination of the blades 3.
• the micromixer is supplied by the inlet 5 by means of a first fluid and by the inlet 6 by the means a second fluid.
• the orifices of the distributor 17 conduct the fluids towards the center, in the central hole 18.
• the fluids are then confined between the shaft 2 and the walls of the central hole 18 and are in contact with a first group of blades 3.
• the first blades in cooperation with the first counter blades, will shear the fluids which will progress through the spaces 14, then 15 and 13. The fluids then quickly meet other blades 3 and counter blades 10 to the outlet 7 of the mixer where they are intimately mixed.
• the intimate mixture of fluids can then be used in many applications.
• it can be introduced into a tubular or other reactor, and give rise to chemical reactions, as described above.
• the polymerization installation used is that shown diagrammatically in FIG. 1, page 14 of the aforementioned European patent application no. EP 749 987 and in which a micromixer according to invention having the following characteristics: internal volume of the micromixer: 1.62 ml - diameter of the rotor shaft in the mixing zone: 5.4 mm thickness of the rotor blades: 1 mm thickness of the counter blades of the discs: 1 mm space, measured in the direction of the longitudinal axis of the rotor, between a rotor counter-blade and each of the adjacent rotor blades: 0.4 mm (thickness of the stator discs: 2.8 mm) number of groups of blades 7 number of discs 6
• the triblocks (triblock copolymers) ABC 100, ABC 101 and ABC 104 as identified in Examples 1 to 6 are prepared according to the procedure described in the European patent application published under the number EP 524 054 or in the aforementioned application EP 749 987. The following abbreviations have been used: PS
• SB diblock (two-block copolymer) poly (styrene- - butadiene)
• SBM triblock (three-block terpolymer formed from a polystyrene block, a polybutadiene block and a poly (methyl methacrylate) block)
• PS-b-PB-jb-PMMA terpolymer formed from a polystyrene block, a polybutadiene block and a poly (methyl methacrylate) block
• mass composition 32/35/33
• M n (PS) number-average molar mass of the polystyrene block
• ABC 101 PS-b-PB-jb-PMMA of mass composition (20/30/50) and having a number-average molar mass M n (PS) of 20,000 g / mol
• ABC 104 PS-i-PB- Jb-PMMA of mass composition (20/30/50) and having a number-average molar mass M n (PS) of 20,000 g / mol Q (SB) - flow rate of the poly (styrene - - butadiene) solution -butadienyl lithium, at the inlet of the micromixer, in kg / h Q (M): flow rate of the methyl methacrylate solution at the inlet of the micromixer in kg / h V0: 0 rpm
• the number-average molar mass of the PS sequence was determined by steric exclusion chromatography (CES) in polystyrene equivalent, after sampling of this sequence during the experiment.
• the PS, PB and PMMA mass fractions were determined by proton NMR.
• PS poly (styrene-jb-butadiene)
• SB poly (styrene-jb-butadiene) block copolymer
• the glass transition temperature (T g ) of the PB sequence is approximately -90 ° C.
• PMMA sequences are more than 70% syndiotactic and have a T g of 135 ° C.
• the flow rates are kept constant, namely, 40 kg / h for Q (SB) and 20 kg / h for Q (M).
• the intensity of the detection I is measured by CES as a function of the elution volume Ve.
• the volume energy dissipated in the micromixing zone is less important, which has the consequence that the contact between the reagents is less intimate.
• Example 2 The influence of the speed of rotation of the rotor of the micromixer according to the invention on the quality of a synthesized ABC 101 triblock is studied.
• Example 3 To do this, proceed as in Example 1. The results are represented in FIG. 7. The same conclusions are reached as in Example 1, namely: no significant difference is observed between the ABC 101s synthesized when we go from VI to V4; in all cases, the presence in the product obtained of residual SB is noted; the proportion of SB in the ABC 100 synthesized is significantly higher at V0 (static mixer) than for VI, V2, V3 or V4, which again shows that the dynamic micromixer according to the invention is more efficient than a static mixer .
• V0 static mixer
• the sum of the flow rates Q (SB) and Q (M), respectively, 30 kg / h and 15 kg / h, is equal to 45 kg / h.
• Example 5 the procedure was as in Example 5, except that higher total flow rates were used, namely 60 kg / h instead of 45 kg / h.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Civil Engineering (AREA)
• Structural Engineering (AREA)
• Mixers Of The Rotary Stirring Type (AREA)
• Physical Or Chemical Processes And Apparatus (AREA)
• Polymerisation Methods In General (AREA)

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• 2002
  • 2002-06-07 FR FR0207025A patent/FR2840546B1/fr not_active Expired - Fee Related
• 2003
  • 2003-05-23 CA CA002489088A patent/CA2489088A1/fr not_active Abandoned
  • 2003-05-23 US US10/517,190 patent/US7287899B2/en not_active Expired - Fee Related
  • 2003-05-23 CN CNB038132397A patent/CN1326602C/zh not_active Expired - Fee Related
  • 2003-05-23 JP JP2004510934A patent/JP2005528978A/ja active Pending
  • 2003-05-23 EP EP03757093A patent/EP1513605A1/de not_active Withdrawn
  • 2003-05-23 AU AU2003260568A patent/AU2003260568A1/en not_active Abandoned
  • 2003-05-23 WO PCT/FR2003/001570 patent/WO2003103818A1/fr active Application Filing

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