# US 11,897,833 B2 · Removing organic acids in monoethylene glycol recovery

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- Number: US 11,897,833 B2
- Document ID: US11897833B2
- Status: Granted
- Kind: B2
- Application number: 17/658,739
- Filed: 2022-04-11
- Published: 2022-12-01
- Granted: 2024-02-13
- Earliest claimed: 2019-09-13
- Assignees: Cameron International Corporation
- Applicants: Cameron International Corporation
- Inventors: Steven Langley
- Web page: https://patentgrep.com/patent/US11897833B2

## CPC

- C07C 29/80: by distillation
- B01D 1/0082: {Regulation; Control}
- B01D 3/06: Flash distillation
- B01D 3/143: {by two or more of a fractionation, separation or rectification step}
- B01D 3/322: {Reboiler specifications}
- C07C 29/84: by extractive distillation
- C07C 29/88: by treatment giving rise to a chemical modification of at least one compound (chemisorption C07C29/76)
- B01D 3/009: {in combination with chemical reactions}
- C07C 31/202: {Ethylene glycol}
- Y02P 20/10: Process efficiency
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Embodiments described herein provide a method, comprising reducing pH of a glycol vaporization separator purge stream to form an acid stream; distilling the acid stream to form an overhead stream and a bottoms stream; and recycling the bottoms stream to the vaporization separator.

## Claims

### Claim 1

A method for removing organic acid salts in monoethylene glycol recovery, comprising:
controlling a purge stream from a vaporization separator based on a physical property indicating buildup of organic salts in monoethylene glycol that circulates through the vaporization separator, wherein the physical property comprises a viscosity or a density;
reducing pH of the purge stream to form an acid stream;
distilling the acid stream to form an overhead stream and a bottoms stream; and
recycling the bottoms stream to the vaporization separator.

### Claim 2 (depends on 1)

The method of claim 1, wherein distilling the acid stream comprises providing the acid stream to a distillation column having a packing, and refluxing and reboiling the distillation column.

### Claim 3 (depends on 2)

The method of claim 2, wherein the acid stream is charged to the distillation column at a location between the packing and a bottom of the distillation column.

### Claim 4 (depends on 2)

The method of claim 2, wherein the acid stream is charged to a feed point of the distillation column, a reboiled bottoms stream is returned to the distillation column at a return point, and the feed point is between the packing and the return point.

### Claim 5 (depends on 1)

The method of claim 1, wherein reducing pH of the purge stream comprises injecting an aqueous acid solution into the purge stream to form an acid mixture and flowing the acid mixture through a vessel.

### Claim 6 (depends on 5)

The method of claim 5, further comprising detecting pH of the acid stream and adjusting a flow rate of the aqueous acid solution based on the detected pH.

### Claim 7 (depends on 1)

The method of claim 1, wherein the purge stream is obtained from a pumparound stream of the vaporization separator, and further comprising:
comparing the physical property of the pumparound stream to a first threshold value indicating organic salts in the pumparound stream need treatment;
comparing the physical property of the pumparound stream to a second threshold value indicating the organic salts in the pumparound stream do not need treatment;
commencing the reducing pH if the physical property reaches the first threshold value; and
discontinuing the reducing pH if the physical property reaches the second threshold value.

### Claim 8 (depends on 1)

The method of claim 1, wherein recycling the bottoms stream to the vaporization separator includes routing the bottoms stream to a feed stream of the vaporization separator.

### Claim 9 (depends on 1)

The method of claim 1, wherein the physical property comprises the viscosity.

### Claim 10

A method for removing organic acid salts in monoethylene glycol recovery, comprising:
detecting a physical property indicating buildup of organic salts in a pumparound stream of a glycol vaporization separator, wherein the physical property comprises a viscosity or a density;
comparing the physical property to a first threshold value indicating the organic salts in the pumparound stream need treatment;
withdrawing a purge stream from the pumparound stream if the physical property reaches the first threshold value;
reducing pH of the purge stream to form an acid stream;
distilling the acid stream to form an overhead stream and a bottoms stream; and
recycling the bottoms stream to the glycol vaporization separator.

### Claim 11 (depends on 10)

The method of claim 10, wherein distilling the acid stream comprises providing the acid stream to a distillation column having a packing, and refluxing and reboiling the distillation column.

### Claim 12 (depends on 11)

The method of claim 11, wherein the acid stream is charged to a feed point of the distillation column, a bottoms stream of the distillation column is reboiled and returned to the distillation column at a return point, and the feed point is between the packing and the return point.

### Claim 13 (depends on 10)

The method of claim 10, wherein the physical property comprises the viscosity.

### Claim 14 (depends on 10)

The method of claim 10, wherein the physical property is compared to the first threshold value and to a second threshold value indicating the organic salts in the pumparound stream do not need treatment, withdrawal of the purge stream from the pumparound stream is commenced if the physical property reaches the first threshold value, and withdrawal of the purge stream is discontinued if the physical property reaches the second threshold value.

### Claim 15 (depends on 10)

The method of claim 10, further comprising removing divalent species from the bottoms stream.

### Claim 16 (depends on 10)

The method of claim 10, wherein reducing pH of the purge stream to form the acid stream comprises:
adding an aqueous acid treatment to the purge stream at an acid treatment rate;
mixing the purge stream with the acid treatment stream in an acid treatment vessel;
detecting a pH of the acid stream; and
controlling the acid treatment rate based on the pH.

### Claim 17 (depends on 16)

The method of claim 16, further comprising controlling conversion of the organic acid salts to organic acids using a pH target for the acid stream.

### Claim 18

A method for removing organic acid salts in monoethylene glycol recovery, comprising:
withdrawing a purge stream from a liquid volume of a glycol vaporization separator based on a physical property of the liquid volume indicating buildup of organic salts in the liquid volume wherein the physical property comprises a viscosity or a density;
mixing an aqueous acid with the purge stream to form an acid stream at a rate of the aqueous acid that is based on a pH of the acid stream;
providing the acid stream to a packed distillation column at a location below a packing inside the packed distillation column;
distilling the acid stream to form an overhead stream and a bottoms stream; and
recycling the bottoms stream to the glycol vaporization separator.

### Claim 19 (depends on 18)

The method of claim 18, wherein recycling the bottoms stream to the glycol vaporization separator comprises removing divalent species from the bottoms stream.

### Claim 20 (depends on 18)

The method of claim 18, wherein the physical property comprises the viscosity.
