Method of Producing Uniform Polymer Beads of Various Sizes

• US 20140264984A1
• Filed: 03/15/2013
• Published: 09/18/2014
• Est. Priority Date: 03/15/2013
• Status: Active Grant

• Current Assignee: Purolite LLC (Ecolab, Inc.)
• Original Assignee: Purolite Corporation (Ecolab, Inc.)
• Inventors: Kosvintsev, Serguei Rudolfovich
• Granted Patent: US 9,028,730 B2
• Time in Patent Office: Days
• US Class Current: 264/8
• CPC Class Codes: B01F 27/80 with stirrers rotating about a substantially vertical axis
• CPC Class Codes: B01F 31/441 performing a rectilinear reciprocating movement
• CPC Class Codes: B01F 33/82 Combinations of dissimilar mixers
• CPC Class Codes: B01F 35/71755 using means for feeding components in a pulsating or intermittent manner
• CPC Class Codes: B01J 19/18 Stationary reactors having moving elements inside B01J19/08, B01J19/26 take precedence
• CPC Class Codes: B01J 19/185 of the pulsating type
• CPC Class Codes: B01J 2/06 in a liquid medium
• CPC Class Codes: B01J 2/12 in rotating drums
• CPC Class Codes: B01J 4/004 Sparger-type elements
• CPC Class Codes: B01J 4/007 provided with moving parts
• CPC Class Codes: C08F 2/01 characterised by special features of the polymerisation apparatus used

Abstract

Speriodal polymer beads having a uniform size are prepared by polymerizing uniformly sized monomer droplets formed by dispersing a polymerizable monomer phase over double-walled cylindrical cross-flow membrane into an aqueous phase. A shear force is provided at a point of egression of the polymerizable monomer phase into the aqueous phase, the direction of shear substantially perpendicular to the direction of egression of the monomer phase. The polymer beads can be employed in applications where beads having uniform diameters of 10 to 200 μm are useful.

Claims

1. A method for preparing spheroidal polymer beads having a volume average particle diameter of about 5 to about 300 μ

m, the method comprising;

providing an apparatus comprising a cylindrical-shaped double-walled chamber comprising;

an outer cylindrical component with a continuous side wall;

an inner cylindrical component with a continuous side wall, wherein the side wall of the inner component is spaced inwardly from the side wall of the outer component and the inner component includes a constant diameter throughout the height of the outer wall;

wherein the side wall of the inner component and the side wall of the outer component include continuous upper and bottom rims and the rims are joined to form an air tight compartment between the inner and outer components, the side wall of the outer component and the side wall of the inner component comprise a membrane comprising a plurality of pores wherein a first volume is in contact with a first side of the membrane located in the compartment between the inner and outer components of the double-walled chamber and a second volume is in contact with a second side of the membrane located outside of the double-walled chamber, the first volume comprising a polymerizable monomer phase, the second volume comprising an aqueous liquid immiscible with the polymerizable monomer phase;

dispersing the first volume through the pores into the second volume under conditions sufficient to form a plurality of monomer droplets comprising the polymerizable monomer, wherein a shear force is provided at a point of egression of the first volume into the second volume, the direction of shear substantially perpendicular to the direction of egression of the first volume; and

polymerizing the droplets dispersed in the second volume.

2. The method according to claim 1, wherein the membrane comprises from about 200 to about 2,000 pores per cm² of the membrane.

3. The method according to claim 2, wherein the membrane comprises from about 1,000 to about 2,000 pores per cm² of the membrane.

4. The method according to claim 1, wherein the pores have a diameter in the range of about 1 μ

m to about 100 μ

m.

5. The method according to claim 4, wherein the pores have a diameter in the range of about 20 μ

m to about 60 μ

m.

6. The method according to claim 1, wherein the plurality of pores are positioned from each other at a distance of at least about 20 times the diameter of each pore when the distance is measured from the center of each pore.

7. The method according to claim 1, wherein the monomer phase is dispersed through the pores into the second volume at a rate of about 1 to about 50 cm/s.

8. The method according to claim 7, wherein the monomer phase is dispersed through the pores into the second volume at a rate of about 40 cm/s.

9. The method according to claim 1, wherein the beads have a particle size distribution having a uniformity coefficient of less than 1.2.

10. The method according to claim 1, wherein the shear at the point of egression of the first volume is provided by displacing the membrane relative to the second volume.

11. The method according to claim 10, wherein the displacing is rotating, pulsing, or oscillating movement.

12. The method according to claim 1, wherein the first volume is dispersed into the second volume by applying pressure to the first volume.

13. The method according to claim 1, wherein monomer phase is directed into the aqueous liquid by pumping the first volume through the membrane.

14. The method according to claim 1, wherein the membrane is substantially metallic.

15. The method according to claim 14, wherein the membrane is wholly metallic.

16. The method according to claim 15, wherein the membrane comprises nickel

17. The method according to claim 16, wherein the membrane is nickel-plated.

18. The method according to claim 1, wherein the plurality of pores are conical shaped.

19. The method according to claim 1, wherein the pores are in the shape of a slot, with an aspect ratio of slot width to slot length of at least 1:

2.

20. The method according to claim 1, wherein the polymerizable monomer phase comprises at least one monomer selected from styrene, divinylbenzene, and methacrylate.

21. The method according to claim 1, wherein the polymerizable monomer phase comprises divinylbenzene.

22. The method according to claim 1, wherein the dispersed phase comprises agarose or other gel forming compounds.

23. The method according to claim 1, wherein the polymerizable monomer phase comprises a porogen.

24. The method according to claim 23, wherein the porogen is an aliphatic alcohol.

25. The method according to claim 24, wherein the aliphatic alcohol is isobutyl alcohol.

26. The method according to claim 1, wherein the membrane comprises nickel, the monomer phase comprises styrene and divinylbenzene and the aqueous liquid comprises polyvinylalcohol.