# US 12,005,405 B2 · Apparatus and process for continuous adsorption

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- Number: US 12,005,405 B2
- Document ID: US12005405B2
- Status: Granted
- Kind: B2
- Application number: 17/257,701
- Filed: 2019-07-12
- Published: 2021-09-23
- Granted: 2024-06-11
- Earliest claimed: 2018-07-12
- Assignees: Dsm IP Assets B.V.
- Applicants: Dsm IP Assets B.V.
- Inventors: Peter Riebel; Kai Urban
- Web page: https://patentgrep.com/patent/US12005405B2

## CPC

- B01F 23/53: using driven stirrers
- B01J 20/3204: {Inorganic carriers, supports or substrates}
- B01F 23/511: {characterised by the composition of the liquids or solids}
- B01F 23/54: {wetting solids}
- B01F 27/2123: Shafts with both stirring means and feeding or discharging means
- B01F 27/231: with a variable orientation during mixing operation, e.g. with tiltable rotor axis
- B01F 27/61: about an inclined axis
- B01F 27/62: {comprising liquid feeding, e.g. spraying means}
- B01F 27/70: with paddles, blades or arms
- B01J 20/103: {comprising silica}
- B01J 20/165: {Natural alumino-silicates, e.g. zeolites}
- B01J 20/20: comprising free carbon; comprising carbon obtained by carbonising processes
- B01F 2101/22: Mixing of ingredients for pharmaceutical or medical compositions
- B01F: MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING (mixing paints B44D3/06)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

The invention relates to an apparatus for the continuous production of a particulate adsorption product, the apparatus comprising: a mixing drum having an elongated cavity for receiving a particulate adsorbent material, an adsorbent inlet and a product outlet, wherein the mixing drum is arranged such that the cavity is inclined in flow direction of the particulate material, and wherein the cavity comprises an initial transport zone adjacent to the inlet and a mixing zone following the initial transport zone; a rotating member extending through the cavity in a longitudinal direction, wherein the rotating member comprises a helical conveying blade at longitudinal positions corresponding to the initial transport zone and mixing instruments at longitudinal positions corresponding to the mixing zone; and one or more injection nozzles for injecting a liquid adsorbate to the mixing zone. The invention further relates to a process for the continuous production of a particulate adsorption product using such apparatus.

## Claims

### Claim 1

A process for the continuous production of a particulate adsorption product using an apparatus comprising:
a mixing drum having an elongated cavity for receiving a particulate adsorbent material, an adsorbent inlet and a product outlet, wherein
the mixing drum is arranged such that the cavity is inclined in flow direction of the particulate material, and the cavity comprises an initial transport zone adjacent to the inlet and a mixing zone following the initial transport zone;
a rotating member extending through the cavity in a longitudinal direction, wherein the rotating member comprises a helical conveying blade at longitudinal positions corresponding to the initial transport zone and mixing instruments at longitudinal positions corresponding to the mixing zone; and
one or more injection nozzles for injecting a liquid adsorbate to the mixing zone, the process comprising the steps of:
continuously feeding a flowable particulate adsorbent material into the initial transport zone of the cavity through the inlet, wherein the particulate adsorbent material is a silica, charcoal, or zeolite material;
continuously injecting a liquid adsorbate into the mixing zone of the cavity through the nozzles, wherein the liquid adsorbate is a pure liquid active or a liquid solution or dispersion of an active, with the active being a biologically active component; and
continuously operating the rotating member to propagate the adsorbent through the initial transport zone to the mixing zone and to agitate the adsorbent and the adsorbate in the mixing zone.

### Claim 2 (depends on 1)

The process of claim 1, wherein the rotating member is operated at a rotational speed such that the peripheral speed of the helical conveying blade and the mixing instruments is 1 m/s or less.

### Claim 3 (depends on 1)

The process of claim 1, wherein the particulate adsorbent materials is a porous material having a specific surface area of at least 100 m2/g.

### Claim 4 (depends on 1)

The process of claim 1, wherein the feed rate of particulate adsorbent material and the rotational speed of the rotating member are adjusted such that the average residence time of the particulate material is between 2 and 20 minutes.

### Claim 5 (depends on 4)

The process of claim 4, wherein the feed rate of particulate adsorbent material and the rotational speed of the rotating member are adjusted such that the average residence time of the particulate material is between 5 and 10 minutes.

### Claim 6 (depends on 1)

The process of claim 1, wherein the cavity volume unoccupied by the particulate material is filled with ambient air.

### Claim 7 (depends on 1)

The process of claim 1, wherein the mixing instruments comprise mixing paddles.

### Claim 8 (depends on 7)

The process of claim 7, wherein the operative surfaces of the paddles are slanted backwards.

### Claim 9 (depends on 1)

The process of claim 1, wherein the cavity further comprises a terminal transport zone adjacent to the outlet and, at longitudinal positions corresponding to the terminal transport zone, the rotating member comprises a further helical conveyor blade.

### Claim 10 (depends on 1)

The process of claim 1, wherein the cavity further comprises a resting zone following the mixing zone and at longitudinal positions corresponding to the resting zone, the rotating member is devoid of mixing instruments or conveyor blades.

### Claim 11 (depends on 10)

The process of claim 10, wherein the cavity further comprises an intermediate transport zone between the mixing zone and the resting zone, or within the mixing zone, and, at longitudinal positions corresponding to the intermediate transport zone, the rotating member comprises another helical conveyor blade.

### Claim 12 (depends on 11)

The process of claim 11, wherein the resting zone extends over at least 10% of the length of the cavity and/or has a longitudinal extension that is equal or greater than the longitudinal extension of the initial transport zone, the terminal transport zone, the intermediate transport zone, or one of the mixing zones.

### Claim 13 (depends on 1)

The process of claim 1, wherein the incline angle is between 15 and 45° and/or wherein the L/D ratio of the cavity is between 2 and 10.

### Claim 14 (depends on 1)

The process of claim 1, wherein the incline angle and the length and diameter of the mixing zone are such that there are longitudinal positions within the mixing zone whose entire cross-section remains below the level of product removal.

### Claim 15 (depends on 14)

The process of claim 14, wherein the incline angle, the length of the mixing zone and the positions of the injection nozzles are such that all injection nozzles are located below the level of product removal.

### Claim 16 (depends on 1)

The process of claim 1, wherein the apparatus comprises a lifting device for adjusting the incline of the cavity.

### Claim 17 (depends on 16)

The process of claim 16, wherein the lifting device comprises one or more hydraulic cylinders.

### Claim 18 (depends on 12)

The process of claim 12, wherein the resting zone extends over at least 15% of the length of the cavity.

### Claim 19 (depends on 18)

The process of claim 18, wherein the resting zone extends over at least 20% of the length of the cavity.

### Claim 20 (depends on 13)

The process of claim 13, wherein the L/D ratio of the cavity is between 3 and 7.

### Claim 21 (depends on 7)

The process of claim 7, wherein the mixing paddles are distributed over the length of the mixing zone.

### Claim 22 (depends on 14)

The process of claim 14, wherein longitudinal positions whose entire cross-section remains below the level of product removal, account for at least 30% of all longitudinal positions within the mixing zone.