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Arkema : Patent Issued for Hydrochloric Acid Purification Process (USPTO 9828314)

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12/07/2017 | 08:08pm CET

By a News Reporter-Staff News Editor at Journal of Engineering -- According to news reporting originating from Alexandria, Virginia, by VerticalNews journalists, a patent by the inventors Collier, Bertrand (Saint-genis-laval, FR); Deur-Bert, Dominique (Charly, FR); Lacambra, Joaquin (Vernaison, FR); Pigamo, Anne (Francheville, FR), filed on November 10, 2014, was published online on November 28, 2017.

The assignee for this patent, patent number 9828314, is Arkema France (Colombes, FR).

Reporters obtained the following quote from the background information supplied by the inventors: "It is known to produce fluorinated compounds, such as hydrofluorocarbons, by fluorination of chlorinated compounds, such as hydrochlorocarbons in particular. This fluorination is generally a catalytic fluorination using hydrofluoric acid (HF) as fluorinating agent.

"During this type of reaction, hydrochloric acid (HCl) is coproduced. It is known to separate the HCl from the other gases produced via a distillation column and then to absorb the HCl in an adiabatic absorption column in order to generate an HCl solution of commercial type.

"The document FR 1507252 describes stages of treatment on active charcoal, at high temperature and in the presence of water, and of washing with concentrated aqueous hydrochloric acid.

"The document U.S. Pat. No. 3,353,911 describes the purification of an HF/HCl gas mixture by bringing into contact with an absorbent solution which is a saturated boric acid solution.

"However, the known techniques for the purification of hydrochloric acid do not make it possible, in some cases, to achieve the required HCl purity.

"There thus exists a need to provide an improved process for the purification of hydrochloric acid in a gas stream."

In addition to obtaining background information on this patent, VerticalNews editors also obtained the inventors' summary information for this patent: "The invention relates first to a process for the treatment of a gas stream comprising hydrochloric acid, hydrofluoric acid and fluorinated-oxygenated compounds, in which the gas stream is successively subjected to: a stage of catalytic hydrolysis; a stage of washing with an acid solution; a stage of adsorption of impurities by active charcoal; a stage of adiabatic or isothermal absorption of the hydrochloric acid in an aqueous solution, making it possible to collect hydrochloric acid solution.

"According to one embodiment, the stage of catalytic hydrolysis is carried out on a bed of active charcoal.

"According to one embodiment, the acid solution used during the washing stage is a hydrochloric acid solution and preferably originates from the hydrochloric acid solution collected on conclusion of the adiabatic or isothermal absorption stage.

"According to one embodiment, the process additionally comprises: a stage of bringing the hydrochloric acid solution into contact with a silica gel.

"According to one embodiment, the fluorinated-oxygenated compounds comprise carbonyl difluoride, carbonyl chloride fluoride, trifluoroacetyl fluoride and/or trifluoroacetic acid and, preferably, the gas stream comprises at least 50 mg/l, in particular at least 100 mg/l, indeed even at least 200 mg/l, of trifluoroacetyl fluoride and/or trifluoroacetic acid.

"According to one embodiment, boric acid is added to the acid solution used for the washing stage.

"According to one embodiment, the gas stream is a stream resulting from a catalytic fluorination reaction of at least one chlorinated compound to give at least one fluorinated compound, said stream preferably being collected at the outlet of a distillation of a stream of products from the catalytic fluorination reaction.

"According to one embodiment, the catalytic fluorination reaction is carried out in the presence of oxygen.

"According to one embodiment: the chlorinated compound is a chlorocarbon, a hydrochlorocarbon, a chlorofluorocarbon, a hydrochlorofluorocarbon, a chloroolefin, a hydrochloroolefin, a chlorofluoroolefin or a hydrochlorofluoroolefin and the fluorinated compound is a fluorocarbon, a hydrofluorocarbon, a chlorofluorocarbon, a hydrochlorofluorocarbon, a fluoroolefin, a hydrofluoroolefin, a chlorofluoroolefin or a hydrochlorofluoroolefin; preferably, the chlorinated compound is chosen from 1,1,2-trichloroethane, 1,1,1,2,3-pentachloropropane, 1,1,1,3,3-pentachloropropane, 1,1,2,2,3-pentachloropropane, 2,3-dichloro-1,1,1-trifluoropropane, perchloroethylene, 1,2-dichloroethylene, 1,1,2,3-tetrachloropropene, 2,3,3,3-tetrachloropropene, 1,1,3,3-tetrachloropropene, 1,3,3,3-tetrachloropropene, 2-chloro-3,3,3-trifluoropropene, 1-chloro-3,3,3-trifluoropropene and their mixtures; and preferably, the fluorinated compound is chosen from pentafluoroethane, 1-chloro-2,2-difluoroethane, 1,3,3,3-tetrafluoropropene, 2,3,3,3-tetrafluoropropene, 2-chloro-3,3,3-trifluoropropene, 1-chloro-3,3,3-trifluoropropene and their mixtures.

"The invention also relates to a process for the preparation of a fluorinated compound, comprising: the provision of a chlorinated compound and of hydrofluoric acid; the catalytic reaction of the chlorinated compound with the hydrofluoric acid and the collection of a stream of crude products; the separation of the stream of crude products, preferably by distillation, making it possible to recover, on the one hand, a stream of fluorinated compound and, on the other hand, a gas stream mainly comprising hydrochloric acid and also minor amounts of hydrofluoric acid and of fluorinated-oxygenated compounds; the treatment of the gas stream comprising hydrochloric acid, hydrofluoric acid and fluorinated-oxygenated compounds as described above.

"According to one embodiment, the catalytic reaction is carried out in the presence of oxygen.

"According to one embodiment: the chlorinated compound is a chlorocarbon, a hydrochlorocarbon, a chlorofluorocarbon, a hydrochlorofluorocarbon, a chloroolefin, a hydrochloroolefin, a chlorofluoroolefin or a hydrochlorofluoroolefin and the fluorinated compound is a fluorocarbon, a hydrofluorocarbon, a chlorofluorocarbon, a hydrochlorofluorocarbon, a fluoroolefin, a hydrofluoroolefin, a chlorofluoroolefin or a hydrochlorofluoroolefin; preferably, the chlorinated compound is chosen from 1,1,2-trichloroethane, 1,1,1,2,3-pentachloropropane, 1,1,1,3,3-pentachloropropane, 1,1,2,2,3-pentachloropropane, 2,3-dichloro-1,1,1-trifluoropropane, perchloroethylene, 1,2-dichloroethylene, 1,1,2,3-tetrachloropropene, 2,3,3,3-tetrachloropropene, 1,1,3,3-tetrachloropropene, 1,3,3,3-tetrachloropropene, 2-chloro-3,3,3-trifluoropropene, 1-chloro-3,3,3-trifluoropropene and their mixtures; and preferably, the fluorinated compound is chosen from pentafluoroethane, 1-chloro-2,2-difluoroethane, 1,3,3,3-tetrafluoropropene, 2,3,3,3-tetrafluoropropene, 2-chloro-3,3,3-trifluoropropene, 1-chloro-3,3,3-trifluoropropene and their mixtures.

"The invention also relates to a plant for the treatment of a gas stream comprising hydrochloric acid, hydrofluoric acid and fluorinated-oxygenated compounds, comprising: a pipe for introducing a gas stream comprising hydrochloric acid, hydrofluoric acid and fluorinated-oxygenated compounds, feeding a catalytic hydrolysis unit; a washing unit, fed on the one hand by a pipe for collecting the hydrolyzed gas stream resulting from the catalytic hydrolysis unit and on the other hand by a pipe for introducing an acid solution; a unit for adsorption of impurities comprising a bed of active charcoal, which unit is fed by a pipe for collecting the washed gas stream resulting from the washing unit; a unit for adiabatic or isothermal absorption, fed on the one hand by a pipe for collecting the purified or isothermal stream resulting from the adsorption unit and on the other hand by a pipe for introducing an aqueous solution; a pipe for collecting a hydrochloric acid solution at the outlet of the adiabatic or isothermal absorption unit.

"According to one embodiment, the catalytic hydrolysis unit comprises a bed of active charcoal.

"According to one embodiment, the pipe for introducing an acid solution does or does not result directly from the pipe for collecting a hydrochloric acid solution.

"According to one embodiment, the plant additionally comprises: an additional adsorption unit comprising a silica gel, which unit is fed by the pipe for collecting a hydrochloric acid solution; and a pipe for collecting a purified hydrochloric acid solution resulting from the additional adsorption unit.

"According to one embodiment, the plan comprises a contribution of boric acid solution to the washing unit.

"According to one embodiment, the pipe for introducing a gas stream comprising hydrochloric acid, hydrofluoric acid and fluorinated-oxygenated compounds results from a distillation unit, the distillation unit preferably being fed by a pipe for collecting crude products at the outlet of a catalytic reactor.

"According to one embodiment, the catalytic reactor is fed by a pipe for introducing a chlorinated compound and a pipe for introducing hydrofluoric acid, and the pipe for collecting crude products transports a stream comprising a fluorinated compound, and preferably: the chlorinated compound is a chlorocarbon, a hydrochlorocarbon, a chlorofluorocarbon, a hydrochlorofluorocarbon, a chloroolefin, a hydrochloroolefin, a chlorofluoroolefin or a hydrochlorofluoroolefin and the fluorinated compound is a fluorocarbon, a hydrofluorocarbon, a chlorofluorocarbon, a hydrochlorofluorocarbon, a fluoroolefin, a hydrofluoroolefin, a chlorofluoroolefin or a hydrochlorofluoroolefin; more particularly, the chlorinated compound is chosen from 1,1,2-trichloroethane, 1,1,1,2,3-pentachloropropane, 1,1,1,3,3-pentachloropropane, 1,1,2,2,3-pentachloropropane, 2,3-dichloro-1,1,1-trifluoropropane, perchloroethylene, 1,2-dichloroethylene, 1,1,2,3-tetrachloropropene, 2,3,3,3-tetrachloropropene, 1,1,3,3-tetrachloropropene, 1,3,3,3-tetrachloropropene, 2-chloro-3,3,3-trifluoropropene, 1-chloro-3,3,3-trifluoropropene and their mixtures; and more particularly, the fluorinated compound is chosen from pentafluoroethane, 1-chloro-2,2-difluoroethane, 1,3,3,3-tetrafluoropropene, 2,3,3,3-tetrafluoropropene, 2-chloro-3,3,3-trifluoropropene, 1-chloro-3,3,3-trifluoropropene and their mixtures.

"According to one embodiment, the plant comprises a contribution of oxygen to the catalytic reactor.

"The present invention makes it possible to overcome the disadvantages of the state of the art. It more particularly provides an improved process for the purification of the hydrochloric acid in a gas stream.

"This is accomplished by virtue of the use of three successive stages of treatment of the gas stream, namely a stage of catalytic hydrolysis, a stage of washing and a stage of adsorption on active charcoal, this taking place before the stage of adiabatic or isothermal absorption which generates a concentrated hydrochloric acid solution.

"The invention is based on the identification, by the present inventors, that the gaseous HCl recovered at the distillation column top may be contaminated by a small amount of free HF (entrained due to azotropes with light fluorinated compounds) but also by fluorinated-oxygenated compounds, such as carbonyl difluoride (COF.sub.2), carbonyl chloride fluoride (COFCl) and trifluoroacetyl fluoride (CF.sub.3COF).

"These compounds are generated in particular when the gas stream to be treated results from a fluorination reaction carried out in the presence of oxygen.

"These compounds are highly toxic and are hydrolyzable. They are thus capable of releasing HF, in particular during the stage of adiabatic or isothermal absorption in water, thus contaminating the HCl solution obtained with HF. In addition, the trifluoroacetyl fluoride generates trifluoroacetic acid (or TFA) during its hydrolysis, which compound is harmful.

"The invention makes it possible to separate the HCl from the HF with which it is mixed but also to separate it from the abovementioned fluorinated-oxygenated compounds.

"The invention is also based on the identification, by the present inventors, that the gaseous HCl recovered at the distillation column top may be contaminated by light organic compounds. The invention also makes it possible to satisfactorily remove these light organic compounds during the treatment."

For more information, see this patent: Collier, Bertrand; Deur-Bert, Dominique; Lacambra, Joaquin; Pigamo, Anne. Hydrochloric Acid Purification Process. U.S. Patent Number 9828314, filed November 10, 2014, and published online on November 28, 2017. Patent URL: http://patft.uspto.gov/netacgi/nph-Parser?Sect1=PTO1&Sect2=HITOFF&d=PALL&p=1&u=%2Fnetahtml%2FPTO%2Fsrchnum.htm&r=1&f=G&l=50&s1=9828314.PN.&OS=PN/9828314RS=PN/9828314

Keywords for this news article include: Anions, Charcoal, Chemicals, Fluorides, Chalcogens, Silica Gel, Arkema France, Hydrochloric Acid, Hydrofluoric Acid, Chlorine Compounds, Fluorine Compounds, Chlorofluorocarbons, Noncarboxylic Acids, Chlorinated Hydrocarbons, Fluorinated Hydrocarbons.

Our reports deliver fact-based news of research and discoveries from around the world. Copyright 2017, NewsRx LLC

(c) 2017 NewsRx LLC, source Science Newsletters

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