# US 11,027,250 B2 · Packed bed emulsification

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- Number: US 11,027,250 B2
- Document ID: US11027250B2
- Status: Granted
- Kind: B2
- Application number: 16/328,129
- Filed: 2017-09-04
- Published: 2019-06-20
- Granted: 2021-06-08
- Earliest claimed: 2016-09-06
- Assignees: Cytiva BioProcess R&D AB
- Applicants: Cytiva BioProcess R&D AB
- Inventors: Jimmy Hedin Dahlstrom; Jonas Bengtsson; Per Erik Emilsson; Maranda Fordham; Eva Holmgren; Ronnie Palmgren; Fernando Polanco
- Web page: https://patentgrep.com/patent/US11027250B2

## CPC

- B01J 2/06: in a liquid medium
- B01F 23/4105: {Methods of emulsifying}
- B01F 25/45241: {through a bed of balls}
- B01F 23/4143: {Microemulsions}
- B01F 23/4145: {Emulsions of oils, e.g. fuel, and water}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01F: MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING (mixing paints B44D3/06)

## Abstract

A system and method for producing fine droplets of polysaccharide from a premixed water-in-oil emulsion uses a packed bed (5) comprising hydrophilic beads (7).

## Claims

### Claim 1

A system for the production of polysaccharide droplets from a water-in-oil emulsion comprising, at least one chamber comprising an inlet side connectable to a source of water-in-oil emulsion containing droplets of an aqueous solution of a polysaccharide in an oil-based continuous phase, an outlet side, a packed bed of beads between the inlet side and the outlet side, and flow-producing means for providing a flow of water-in-oil emulsion through the packed bed to an outlet port, wherein the beads are hydrophilic beads, and a bed height of the packed bed is 10-70 mm.

### Claim 2 (depends on 1)

The system of claim 1, wherein the hydrophilic beads are made of glass.

### Claim 3 (depends on 2)

The system of claim 2, wherein the hydrophilic beads are made of glass with a hydrophilic surface coating.

### Claim 4 (depends on 1)

The system of claim 1, wherein the hydrophilic beads are made of stainless steel.

### Claim 5 (depends on 1)

The system of claim 1, wherein the hydrophilic beads have a weight average diameter of 0.1-2 mm.

### Claim 6 (depends on 1)

The system of claim 1, wherein the diameter of each bead is D and the packed bed is supported on a bed support comprising a plurality of through holes which each have at least one dimension W which is smaller than the diameter D of the beads in order to prevent the beads from passing through the holes.

### Claim 7 (depends on 6)

The system of claim 6, wherein said dimension W of the through holes is equal to or greater than 0.3 times the diameter D of the beads and less than or equal to 0.9 times the diameter D of the beads.

### Claim 8 (depends on 1)

The system of claim 1, which is provided with a channel for the recirculation of droplets from said outlet port to the inlet of the chamber.

### Claim 9 (depends on 1)

The system of claim 1, wherein at least the chamber is provided with heating means.

### Claim 10 (depends on 1)

The system of claim 1, comprising a plurality of serially coupled chambers with packed beds, optionally with flow-producing means between the chambers.

### Claim 11

A method for producing fine droplets of polysaccharide material from a water-in-oil premixed emulsion characterized in that it comprises the following steps:
providing a chamber with a packed bed of hydrophilic beads, wherein a bed height of the packed bed is 10-70 mm;
passing a water-in-oil premixed emulsion comprising coarse droplets of aqueous polysaccharide solution in an oil through the packed bed to form fine droplets; and,
optionally recirculating the fine droplets through the packed bed.

### Claim 12 (depends on 11)

The method of claim 11, wherein the polysaccharide solution comprises native or derivatized agar or agarose.

### Claim 13 (depends on 12)

The method of claim 12, wherein the agar or agarose concentration in the polysaccharide solution is 2-15 wt. %.

### Claim 14 (depends on 11)

The method of claim 11, further comprising a step of heating the chamber(s) to a temperature which is greater or equal to 55° C. and less than or equal to 90° C.

### Claim 15 (depends on 11)

The method of claim 11, further comprising a step of heating the chamber(s) to a temperature which is greater or equal to 60° C. and less than or equal to 80° C.

### Claim 16 (depends on 11)

The method of claim 11, wherein the system comprises one or more pressure sensors capable of measuring the pressure drop over the chamber(s), and wherein the pressure drop is controlled in order to keep the size of the droplets within a predetermined interval.

### Claim 17 (depends on 11)

The method of claim 11, wherein said premixed emulsion comprises an oil-soluble polymer and wherein a water-in-oil emulsifier is added to said premixed emulsion before passage through said chamber(s).

### Claim 18 (depends on 11)

The method of claim 11, wherein the volume-weighted median diameter (d50) of the droplets in said premixed emulsion is 100-500 μm.

### Claim 19 (depends on 11)

The method of claim 11, wherein the pressure drop over said chamber(s) is 0.1-3 bar.

### Claim 20 (depends on 19)

The method of claim 19, wherein the pressure drop is 0.1-0.5 bar.

### Claim 21 (depends on 19)

The method of claim 19, wherein the pressure drop is 0.5-2 bar.

### Claim 22 (depends on 11)

The method of claim 11, wherein the volume-weighted median diameter (d50) of the fine droplets is 5-100 μm.

### Claim 23 (depends on 11)

The method of claim 11, comprising 2-10 passages of the emulsion through the packed bed(s).

### Claim 24 (depends on 11)

The method of claim 11, wherein the fine droplets produced are solidified to form solid beads by cooling.

### Claim 25 (depends on 24)

The method of claim 24, wherein the solidified beads are cross-linked and/or derivatized in subsequent operations.
