# US 10,766,014 B2 · Systems with anti-fouling control and methods for controlling fouling within a channel of a plug flow crystallizer

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- Number: US 10,766,014 B2
- Document ID: US10766014B2
- Status: Granted
- Kind: B2
- Application number: 15/496,355
- Filed: 2017-04-25
- Published: 2017-11-02
- Granted: 2020-09-08
- Earliest claimed: 2016-04-29
- Assignees: Purdue Research Foundation
- Applicants: Purdue Research Foundation
- Inventors: Andy Koswara; Zoltan Kalman Nagy
- Web page: https://patentgrep.com/patent/US10766014B2

## CPC

- B01J 19/0013: {Controlling the temperature of the process}
- B01D 9/0013: {by indirect heat exchange}
- B01D 9/0036: {Crystallisation on to a bed of product crystals; Seeding}
- B01D 9/0054: {Use of anti-solvent}
- B01D 9/0059: {General arrangements of crystallisation plant, e.g. flow sheets}
- B01D 9/0063: {Control or regulation (control per se G05)}
- B08B 7/0064: {by temperature changes}
- B08B 17/00: Methods preventing fouling {(preventing accumulation of deposits in pneumatic conveyors B65G53/521)}
- C07C 227/42: Crystallisation
- C07C 231/24: Separation; Purification
- C30B 7/08: by cooling of the solution
- C30B 29/54: Organic compounds
- B01D 9/0072: {Crystallisation in microfluidic devices}
- B01D 9/0077: {Screening for crystallisation conditions or for crystal forms}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B08B: CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR

## Abstract

The invention generally relates to systems with anti-fouling control and methods for controlling fouling within a channel of a plug flow crystallizer. In certain aspects, the invention provides a system that includes a plug flow crystallizer having a channel, one or more heating/cooling elements, each operably associated with a different segment of the channel, and a controller. The controller is operably coupled to the one or more heating/cooling elements and configured to implement a temperature profile within the channel of the plug flow crystallizer that grows crystals in a plug of fluid that flows through a first segment of the channel and dissolves encrust in a second segment of the channel while having minimal impact on crystal growth in the plug of fluid in the second segment of the channel. In certain embodiments, these segments may be cyclically alternated, in that the segment in which crystal grows in one cycle becomes the segment in which crystal dissolves in the next cycle and vice versa, to realize a fully continuous crystallization process.

## Claims

### Claim 1

A system with anti-fouling control, the system comprising:
a plug flow crystallizer comprising a channel;
one or more heating/cooling elements, each operably associated with a different segment of the channel; and
a controller operably coupled to the one or more heating/cooling elements and configured to implement, via an algorithm, a temperature profile within the channel of the plug flow crystallizer that grows crystals in a plug of fluid that flows through a first segment of the channel and dissolves encrust in a second segment of the channel while having minimal impact on crystal growth in the plug of fluid in the second segment of the channel, wherein the algorithm accounts for existence of a boundary layer between the encrust and the channel such that there exists a temperature gradient between the encrust and the channel so that during cooling, a film temperature is lower than that of the channel, while during heating it is higher such that supersaturation in a growth phase and under saturation in a dissolution phase are stronger for encrust dynamics relative to that of crystallization.

### Claim 2 (depends on 1)

The system according to claim 1, wherein the first segment of the channel has a same length as the second segment of the channel.

### Claim 3 (depends on 2)

The system according to claim 2, wherein the temperature profile in the first segment is configured for cooling the one or more plugs of fluid that flow in the first segment to thereby cause crystal growth.

### Claim 4 (depends on 3)

The system according to claim 3, wherein the temperature profile in the second segment is configured for heating the one or more plugs of fluid that flow in the second segment to thereby cause encrust dissolution while having minimal impact on crystal growth in the one or more plugs of fluid in the second segment of the channel.

### Claim 5 (depends on 1)

The system according to claim 1, wherein the controller is further configured to calculate the temperature profile based on encrust kinetics and crystal growth kinetics for a particular reaction.

### Claim 6 (depends on 1)

The system according to claim 1, further comprising one or more sensors operably coupled to the system.

### Claim 7 (depends on 6)

The system according to claim 6, wherein a first sensor determines a period of output stream collection for as long as flow is within a predetermined product quality range.

### Claim 8 (depends on 7)

The system according to claim 7, wherein the first sensor operably communicates to the controller, which manipulates a valve based on data received from the first sensor, to control collection of the one or more plugs of fluid.

### Claim 9 (depends on 6)

The system according to claim 6, wherein a second sensor monitors encrust within the channel.

### Claim 10 (depends on 9)

The system according to claim 9, wherein the second sensor operably communicates to the controller, which manipulates the temperature within the channel, via the one or more heating/cooling elements, based on data received from the second sensor.

### Claim 11

A method for controlling fouling within a channel of a plug flow crystallizer, the method comprising:
flowing one or more plugs of fluid through a channel of a plug flow crystallizer; and
implementing, via an algorithm running on a controller operably coupled to the plug flow crystallizer, a temperature profile within the channel of the plug flow crystallizer that grows crystals in the one or more plugs of fluid that are flowing through a first segment of the channel and dissolves encrust in a second segment of the channel while having minimal impact on crystal growth in the plugs of fluid in the second segment of the channel, wherein the algorithm accounts for existence of a boundary layer between the encrust and the channel such that there exists a
temperature gradient between the encrust and the channel so that during cooling, a film temperature is lower than that of the channel, while during heating it is higher such that supersaturation in a growth phase and under saturation in a dissolution phase are stronger for encrust dynamics relative to that of crystallization.

### Claim 12 (depends on 11)

The method according to claim 11, wherein the first segment of the channel has a same length as the second segment of the channel.

### Claim 13 (depends on 12)

The method according to claim 12, wherein the temperature profile in the first segment is configured for cooling the one or more plugs of fluid that flow in the first segment to thereby cause crystal growth.

### Claim 14 (depends on 13)

The method according to claim 13, wherein the temperature profile in the second segment is configured for heating the one or more plugs of fluid that flow in the second segment to thereby cause encrust dissolution while having minimal impact on crystal growth in the one or more plugs of fluid in the second segment of the channel.

### Claim 15 (depends on 11)

The method according to claim 11, wherein the method further comprises calculating, via the controller, the temperature profile based on heat transfer, encrust kinetics and crystal growth kinetics for a particular crystallization reaction.

### Claim 16 (depends on 11)

The method according to claim 11, further comprising monitoring conditions within the channel via one or more sensors operably coupled to the controller.

### Claim 17 (depends on 16)

The method according to claim 16, wherein a first sensor determines a period of output stream collection for as long as flow is within a predetermined product quality range.

### Claim 18 (depends on 17)

The method according to claim 17, wherein the first sensor operably communicates to the controller, which manipulates a valve based on data received from the first sensor, to control collection of the one or more plugs of fluid.

### Claim 19 (depends on 16)

The method according to claim 16, wherein a second sensor monitors encrust within the channel.

### Claim 20 (depends on 19)

The method according to claim 19, wherein the second sensor operably communicates to the controller, which manipulates the temperature within the channel, via one or more heating/cooling elements, based on data received from the second sensor.
