# US 4,396,591 A · Recovery of hydrogen iodide

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- Number: US 4,396,591 A
- Document ID: US4396591A
- Status: Granted
- Kind: A
- Application number: 06/379,363
- Filed: 1982-05-18
- Granted: 1983-08-02
- Earliest claimed: 1982-05-18
- Assignees: GA Technologies Inc.
- Inventors: John H. Norman
- Web page: https://patentgrep.com/patent/US4396591A

## CPC

- C01B 3/103: the hydrogen being generated from the water as a result of cycles of reactions, e.g. sulfur-iodine cycle
- C01B 7/093: {Hydrogen bromide}
- C01B 7/135: {Hydrogen iodide}
- Y02E 60/36: Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A method of extraction of HI from an aqueous solution of HI and I.sub.2. HBr is added to create a two-phase liquid mixture wherein a dry phase consists essentially of HBr, I and HI and is in equilibrium with a wet phase having a far greater HBr:HI ratio. Using a countercurrent extractor, two solutions can be obtained: a dry HBr--HI--I.sub.2 solution and a wet essentially HBr solution. The dry and wet phases are easily separable, and HI is recovered from the dry phase, after first separating I.sub.2, as by distillation. Alternatively, the HI-HBr liquid mixture is treated to catalytically decompose the HI. HBr is recovered from the wet phase by suitable treatment, including high-pressure distillation, to produce an H.sub.2 O--HBr azeotrope that is not more than 25 mole percent HBr. The azeotrope may be returned for use in an earlier step in the overall process which results in the production of the aqueous solution of HI and I.sub.2 without major detriment because of the presence of HBr.

## Claims

### Claim 1

A method for extracting HI from a solution containing HI and H.sub.2 O, which method comprises the steps of
adding HBr to create two liquid phases:
a dry phase containing HBr and a major portion of the HI from said solution and a wet phase containing a major portion of the H.sub.2 O from said solution and HBr, and
separating said wet and dry phases to obtain HI in a utilizable form.

### Claim 2 (depends on 1)

A method in accordance with claim 1 wherein said dry phase contains substantially all of the HI from said solution and after said separating step is treated to distill HI therefrom.

### Claim 3 (depends on 1)

A method in accordance with claim 1 wherein said solution also contains I.sub.2 which is carried into said dry phase and said dry phase is treated to separate I.sub.2 therefrom leaving a liquid mixture of HI and HBr.

### Claim 4 (depends on 3)

A method in accordance with claim 3 wherein said liquid mixture is subjected to catalytic decomposition to decompose HI and form H.sub.2 and I.sub.2.

### Claim 5 (depends on 1)

A method in accordance with claim 1 wherein said HBr addition to said solution is carried out as a countercurrent extraction step.

### Claim 6 (depends on 1)

A method in accordance with claim 1 wherein said wet phase contains substantially all of the H.sub.2 O from said solution and is subjected to high-pressure distillation to distill HBr therefrom for recovery and reuse and create an HBr--H.sub.2 O azeotrope containing not more than about 8 mole percent HBr.

### Claim 7 (depends on 6)

A method in accordance with claim 6 wherein said high-pressure distillation is carried out at a pressure of at least about 200 atm. and a temperature of at least about 395.degree. C.

### Claim 8

In a process for the production of H.sub.2 from H.sub.2 O using the Bunsen reaction including the steps of
reacting H.sub.2 O, I.sub.2 and SO.sub.2 in a main reaction step under conditions which create first and second distinct liquid phases,
separating said first phase containing HI, I.sub.2, H.sub.2 O and SO.sub.2 from said second phase,
removing SO.sub.2 from said first phase, and
recovering HI from said first phase and decomposing same to create H.sub.2,
the improvement which comprises
adding sufficient HBr to said first phase to again create two liquid phases: a dry phase containing HBr, I.sub.2 and substantially all of the HI and a wet phase containing substantially all of the H.sub.2 O and HBr and
separating said dry phase from said wet phase to obtain HI in a form for said decomposing step.

### Claim 9 (depends on 8)

The invention in accordance with claim 8 wherein I.sub.2 is separated from said dry phase and the remaining HI is catalytically decomposed in the liquid phase in the presence of HBr.

### Claim 10 (depends on 8)

The invention in accordance with claim 8 wherein said wet phase is subjected to high-pressure distillation to distill HBr and leave an azeotrope of water and not more than about 8 mole percent HBr.

### Claim 11 (depends on 10)

The invention in accordance with claim 10 wherein said azeotrope is returned to said main reaction step and at least some of said returned HBr is thereafter included in said first phase.

### Claim 12 (depends on 11)

The invention in accordance with claim 11 wherein the remainder of said returned HBr is carried over in said second liquid phase from said main reaction step along with H.sub.2 SO.sub.4 and H.sub.2 O and wherein this HBr is fractionally distilled from said second phase by treating said second liquid phase with sufficient additional concentrated H.sub.2 SO.sub.4 to break the H.sub.2 O--HBr azeotrope.

### Claim 13 (depends on 11)

The invention in accordance with claim 11 wherein the remainder of said returned HBr is carried over in said second liquid phase and is extracted therefrom by contact with a countercurrently flowing I.sub.2 stream in a step that also serves to increase the H.sub.2 SO.sub.4 concentration of said second liquid phase.