# US 5,707,497 A · Process for the separation of hydrogen fluoride and of difluoromethane

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- Number: US 5,707,497 A
- Document ID: US5707497A
- Status: Granted
- Kind: A
- Application number: 08/394,983
- Filed: 1995-02-27
- Granted: 1998-01-13
- Earliest claimed: 1994-02-28
- Assignees: Elf Atochem S.A.
- Inventors: Jean-Michel Galland; Dominique Rouzies
- Web page: https://patentgrep.com/patent/US5707497A

## CPC

- C07C 17/38: Separation; Purification; Stabilisation; Use of additives
- C01B 7/196: {by distillation}
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A process for the separation of hydrogen fluoride (HF) and of difluoromethane (F32) by fractional distillation and/or condensation, in at least one stage, including in at least one stage obtaining a stream whose HF and F32 contents correspond.

## Claims

### Claim 1

Process for the separation of hydrogen fluoride (HF) and of difluoromethane (F32) by fractional distillation and/or condensation, in at least one stage, consisting essentially of at least one stage obtaining a stream whose HF and F32 contents correspond substantially to those of an azeotropic composition, the at least one stage being performed, as a function of the separation, at a pressure related so that the partial pressure of the HF+F32 mixture of the stream, Pa expressed in bars absolute, and the HF content of the mixture, x in per cent by weight, are linked by the relationship:
Pa=17-22.9(x+0.821)ln(x+0.608)+56.6›ln(x+0.608)!.sup.2 wherein the HF content of the HF-F32 azeotrope decreases when pressure increases.

### Claim 2 (depends on 1)

Process according to claim 1, for the separation of the mixture HF and F32, wherein said mixture is subjected to a first distillation conducted at a pressure above 6 bars absolute.

### Claim 3 (depends on 2)

Process according to claim 2, wherein the HF-F32 azeotrope of low HF content, obtained at the top of the distillation, is subjected to a second distillation conducted at a lower pressure than that of the first distillation and the HF-F32 azeotrope of higher HF content, obtained at the top of the second distillation, is recycled to the first distillation.

### Claim 4 (depends on 3)

Process according to claim 3, wherein the second distillation is performed at a pressure below 10 bars absolute.

### Claim 5 (depends on 2)

Process according to claim 2, wherein the pressure is above 10 bars absolute.

### Claim 6 (depends on 1)

Process according to claim 1, for the separation of a gaseous mixture originating from a reaction for producing F32 by fluorination of methylene chloride with HF in liquid phase, wherein the gaseous mixture containing F32, HF, HCl and by products and reactants of said reaction for producing F32 are subjected to a fractional distillation return or condensation operation at a pressure above 12 bars absolute.

### Claim 7 (depends on 6)

Process according to claim 6, wherein the separation is performed at a pressure of between 16 and 50 bars absolute.

### Claim 8 (depends on 1)

Process according to claim 1, for the separation of a gaseous mixture originating from a reaction for producing F32 by fluorination of methylene chloride with HF in gaseous phase, wherein the gaseous mixture containing F32, HF, HCl and by products and reactants of said reaction for producing F32 is subjected to a fractional distillation and/or condensation at a pressure above 12 bars absolute.

### Claim 9 (depends on 8)

Process according to claim 8, wherein the separation is performed at a pressure of between 16 and 50 bars absolute.