# US 10,500,524 B2 · Separation systems and methods of using them

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- Number: US 10,500,524 B2
- Document ID: US10500524B2
- Status: Granted
- Kind: B2
- Application number: 15/469,990
- Filed: 2017-03-27
- Published: 2018-02-15
- Granted: 2019-12-10
- Earliest claimed: 2012-07-31
- Assignees: Quinlan Properties, LLC
- Applicants: George L Quinlan
- Inventors: George L Quinlan
- Web page: https://patentgrep.com/patent/US10500524B2

## CPC

- B01D 3/40: Extractive distillation
- B01D 3/36: Azeotropic distillation
- B01D 11/0203: {with a supercritical fluid}
- B01D 11/0403: {with a supercritical fluid}
- B01D 11/0407: {the supercritical fluid acting as solvent for the solute}
- H10P 70/80: {Cleaning only by supercritical fluids}
- B01D 3/14: Fractional distillation {or use of a fractionation or rectification column}
- B01D 3/16: Fractionating columns in which vapour bubbles through liquid (packing elements B01J19/30, B01J19/32)
- B01D 3/26: Fractionating columns in which vapour and liquid flow past each other, or in which the fluid is sprayed into the vapour, or in which a two-phase mixture is passed in one direction
- B01D 3/30: Fractionating columns with movable parts or in which centrifugal movement is caused
- B01J 3/008: {Processes carried out under supercritical conditions}
- C07C 45/82: by distillation
- C07C 49/395: of a five-membered ring
- 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)
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS

## Abstract

Certain embodiments described herein are directed to separation systems and methods effective to separate two or more solvents in a solvent mixture. In certain examples, a system effective to separate two or more azeotrope forming solvents is provided. In some embodiments, the system can be effective to remove at least about 95% of one of the solvents from the solvent mixture.

## Claims

### Claim 1

A method of removing at least about 75% by weight or by volume of NMP, based on the total weight of a solvent mixture or based on the total volume of the solvent mixture respectively, from the solvent mixture comprising NMP and ethylene glycol in a chamber, the method comprising:
exposing the solvent mixture comprising the NMP and the ethylene glycol to a supercritical fluid stream of carbon dioxide at an effective temperature and pressure to remove at least about 75% by weight or by volume of the NMP, based on the total weight of the solvent mixture or based on the total volume of the solvent mixture respectively, from the solvent mixture comprising the NMP and ethylene glycol; and
collecting the removed NMP in the supercritical fluid stream of carbon dioxide exiting the chamber.

### Claim 2 (depends on 1)

The method of claim 1, comprising providing the supercritical fluid stream at an effective pressure to be miscible with the NMP.

### Claim 3 (depends on 1)

The method of claim 1, further comprising depressurizing the removed NMP in the supercritical fluid stream to collect the removed NMP.

### Claim 4 (depends on 3)

The method of claim 3, further comprising collecting the removed NMP in a closed vessel.

### Claim 5 (depends on 3)

The method of claim 3, further comprising collecting the removed NMP in an open vessel.

### Claim 6 (depends on 1)

The method of claim 1, further comprising recycling the supercritical fluid stream.

### Claim 7 (depends on 6)

The method of claim 6, further comprising providing the recycled supercritical fluid stream to additional solvent mixture.

### Claim 8 (depends on 7)

The method of claim 7, further comprising removing additional amounts of the NMP from the solvent mixture to remove a total of at least 99% by weight or by volume of the NMP from the solvent mixture.

### Claim 9 (depends on 6)

The method of claim 6, exposing the collected NMP to the recycled supercritical fluid stream.

### Claim 10 (depends on 1)

The method of claim 1, further comprising reusing the supercritical fluid stream to separate solvent mixture.

### Claim 11 (depends on 1)

The method of claim 1, further comprising adding a carrier to the supercritical fluid stream to increase the amount of the NMP recovered compared to the amount of NMP recovered using the same supercritical fluid without the carrier.

### Claim 12 (depends on 1)

The method of claim 1, further comprising detecting the NMP in the supercritical fluid stream.

### Claim 13 (depends on 1)

The method of claim 1, further comprising drying the supercritical fluid after collecting the NMP.

### Claim 14 (depends on 13)

The method of claim 13, further comprising providing the dried supercritical fluid back to the chamber.

### Claim 15 (depends on 1)

The method of claim 1, further comprising configuring the supercritical fluid stream to be supercritical carbon dioxide at a pressure and temperature effective to be miscible with the NMP and the ethylene glycol.
