Method of recycling hydrochloric and hydrofluoric acid effluent

Patent metadata

Field	Value
Publication number	US-9783427-B2
Application number	US-201214350195-A
Country	US
Kind code	B2
Filing date	Oct 1, 2012
Priority date	Oct 6, 2011
Publication date	Oct 10, 2017
Grant date	Oct 10, 2017

Abstract

A method of recycling mixtures of hydrochloric and hydrofluoric acid. In particular, a method of recycling hydrofluoric acid and boron fluoride mixtures. A process for upgrading mixtures of fluoroboron compounds contaminated with chlorides as an aqueous solution of boron fluoride hydrates, including a step of vacuum distillation. Also, a method of producing gaseous boron trifluoride.

First claim

The invention claimed is:

1. A process for producing boron trifluoride hydrates, comprising:
(i) at least one step during which at least one boron compound chosen from boric acid (H 3 BO 3 ), metaboric acid (HBO 2 ) and boric anhydride (B 2 O 3 ) is placed in contact with an aqueous solution of hydrochlorofluoric acid at atmospheric pressure to give a mixture of fluoroboron compounds and of hydrochloric acid;
(ii) a distillation step performed at atmospheric pressure to yield a first fraction comprising hydrochloric acid and a second fraction comprising water, residual hydrochloric acid, and a mixture of fluoroboron compounds; and
(iii) a step of vacuum distillation of the second fraction obtained in step (ii) to remove the residual hydrochloric acid and the water, wherein the temperature of the second fraction is increased during the vacuum distillation step so as to give a concentrated aqueous solution of boron trifluoride hydrates, and wherein the absolute pressure of the vacuum distillation step is between 10 and 100 mbar, and the concentrated aqueous solution of boron trifluoride hydrates obtained after step (iii) contains less than 100 mg of chloride per kg of boron trifluoride hydrates.

2. The process as claimed in claim 1 , wherein the aqueous solution of hydrochlorofluoric acid comprises from 0.005% to 38% by weight of hydrochloric acid, from 1% to 65% by weight of hydrofluoric acid and water representing the remainder to 100%.

3. The process as claimed in claim 1 , wherein the temperature of step (i) is between 0 and 120° C.

4. The process as claimed in claim 1 , wherein the temperature of step (ii) is between 25 and 120° C.

5. The process as claimed in claim 1 , wherein the temperature of the vacuum distillation step is between 30 and 90° C.

6. A process for manufacturing gaseous boron trifluoride, wherein after the vacuum distillation step as claimed in claim 1 , the aqueous solution of boron trifluoride hydrate is subjected to a treatment with concentrated sulfuric acid or sulfuric anhydride or with oleum.

7. The process as claimed in claim 6 , wherein the treatment temperature is between 75 and 135° C.

8. The process as claimed in claim 1 , wherein the process is performed in batch, semi-continuous or continuous mode.

Assignees

• Arkema France

Inventors

• Dufour Pascal
• Le Toullec Cyrille

Classifications

• C01B35/06

  Boron halogen compounds · CPC title

• C01B35/065

  Tetrafluoboric acid · CPC title

• C01B7/0712

  by distillation · CPC title

• C01B35/061 Primary

  Halides · CPC title

• C01B35/063

  Tetrafluoboric acid; Salts thereof · CPC title