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(12) United States Patent (10) Patent No.: US 6,635,231 B2 Smith Et Al

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(12) United States Patent (10) Patent No.: US 6,635,231 B2 Smith Et Al USOO663.5231B2 (12) United States Patent (10) Patent No.: US 6,635,231 B2 Smith et al. (45) Date of Patent: Oct. 21, 2003 (54) PREPARATION OF ARSENIC (56) References Cited PENTAFLUORIDE U.S. PATENT DOCUMENTS (75) Inventors: W. Novis Smith, Philadelphia, PA (US); Joel McCloskey, Phildelphia, PA (US) 2.952,514 A 9/1960 Smith ......................... 423/489 3,875.292 A * 4/1975 Wiesboecket al. ......... 423/472 (73) Assignee: Lithdyne International, Anaheim, CA 4,034,069 A 7/1977 Curtis ........................ 423/489 (US) (*) Notice: Subject to any disclaimer,- the term of this * cited by examiner patent is extended or adjusted under 35 U.S.C. 154(b) by 343 days. Primary Examiner Ngoc-Yen Nguyen (74) Attorney, Agent, or Firm John LeZdey & Associates (21) Appl. No.: 09/799,964 (57) ABSTRACT (22) Filed: Mar. 6, 2001 A process for the preparation of high purity arsenic pen (65) Prior Publication Data tafluoride in high yield. The process uses Sulfur trioxide or oleum and an excess of hydrogen fluoride to react arsenic US 2002/0127174 A1 Sep. 12, 2002 acid or arsenic pentoxide- in0 a reaction medium containing an (51) Int. Cl. .................................................. C01B 9/08 excess of hydrogen fluoride to yield high purity arsenic (52) U.S. Cl. ........................ 423/489; 423/491; 423/522 pentafluoride as a gas. (58) Field of Search ................................. 423/489, 491, 423/522 13 Claims, No Drawings US 6,635,231 B2 1 2 PREPARATION OF ARSENIC c) recovering the pure arsenic pentafluoride and hydrof PENTAFLUORIDE luoric acid by distillation. Optionally, the recovered hydrofluoric acid may be recycled by being added to Supplement the amount of BACKGROUND FOR THE INVENTION hydrogen fluoride to be used in the next preparation batch in 1. Field of the Invention the first Step of the process. This invention relates to the preparation of anhydrous Alternatively, in another preferred embodiment, hexafluo high purity arsenic pentafluoride in high yield. roarsenic acid can be used as the Starting material and 2. Description of the Prior Art effectively reacted with a Stoichiometric amount oleum or SO in a reaction medium of hydrogen fluoride to produce Known processes for the production of arsenic pentafluo high purity arsenic pentafluoride in high yield which is ride include: recovered by distillation. 1. The fluorination of arsenic fluoride, It is, therefore, an object of the present invention to As F+F->AS Fs provide an improved process for the preparation of high 15 purity arsenic pentafluoride in high yield. 2. Fluorination of arsenic, Another related object of the present invention is to 2 AS+5 F->2 ASFs provide a process which is highly efficient and economical U.S. Pat. No. 3,875,292 to Wiesboeck et al. discloses the in preparing arsenic pentafluoride. preparation of Arsenic pentafluoride and fluoroarsenic acids A further object of the present invention is to provide a by fluorinating an arsenic Source Selected from arsenic acid process which produces a minimum amount of hydrofluoric and monofluoroarsenic acid. acid by-product. Therefore, there exists a need to provide high purity Further objects and embodiments of the process of this arsenic pentafluoride in a simple and economical procedure invention will be more readily apparent from the following without the need for extensive fractionation or high-pressure detailed description. equipment and not to have extensive acid gases present that 25 require Special disposal. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS SUMMARY OF THE INVENTION In accordance with the present invention, high purity The present invention is applicable to a process for the arsenic pentafluoride can be produced in high yield without production of arsenic pentafluoride which involves resorting to complex process operations. The critical feature hexafluoroarsenic acid either as a Starting reactant or as an of the present invention is affecting the reaction of arsenic intermediate. The invention is first described in the context acid or arsenic pentoxide in a reaction medium comprising of a preferred proceSS for Such production in which the hydrogen fluoride to form high purity arsenic pentafluoride hexafluoroarsenic acid is produced as an intermediate. in yields of 65 to 100 weight percent (based on contained This embodiment of the present process comprises two arsenic). The yield based on fluoride content is also calcu 35 essential reaction Steps: The first reaction Step involves the lated to be about 90 to 99 percent. Preferably the process is formation of a more concentrated hexafluoroarsenic acid and conducted under a dry atmosphere, at autogenous pressures the Second reaction Step relates to the production of high and moderate temperatures. purity arsenic pentafluoride. In one preferred embodiment the proceSS involves a two 40 The theoretically required quantity of hydrogen fluoride Step process: first preparing hexafluoroarsenic acid by effec necessary for the complete transformation of a arsenic acid tively reacting arsenic acid or arsenic pentoxide with a or arsenic pentoxide into the hexafluoroarsenic acid HASF Stoichiometric excess of anhydrous hydrogen fluoride and is available when the materials are present in a ratio corre then in the Second step, effectively reacting the So formed sponding to 6 molecules of hydrogen fluorine per atom of hexafluoroarsenic acid with oleum (65% SO) or SO to 45 arsenic. react with the formed water from the first step in a reaction In the first reaction Step an excess of anhydrous hydrogen medium comprising the unreacted exceSS hydrogen fluoride fluoride which may range from 9 to 100% over the stoichio from the first reaction Step to form arsenic pentafluoride. metric amount is reacted with arsenic acid or arsenic pen Then the ASFs is distilled from the mixture. All fluoride toxide to form hexafluoroarsenic acid and a water containing compounds other than the arsenic pentafluoride 50 by-product, as shown by the following equation for arsenic product may be condensed and recycled to the reactor for the pentoxide: next reaction. More Specifically in a preferred embodiment, the proceSS for producing arsenic pentafluoride according to the inven XS-CXCCSS tion comprises the Steps of: 55 a) adding an excess of anhydrous hydrogen fluoride above When arsenic acid is used, the number of moles of water a Stoichiometric amount to arsenic acid or arsenic formed is slightly higher, based on the HASF formed as pentoxide to effect reaction in a preferably dry atmo shown by the equation: Sphere to form hexafluoroarsenic acid in the unreacted excess of hydrogen fluoride; alternatively, the arsenic 60 acid or arsenic pentoxide may be added to the hydrogen The Second reaction Step consists in adding oleum or SO fluoride; to the hexafluoroarsenic acid with the excess of anhydrous b) reacting the formed hexafluoroarsenic acid with oleum hydrogen fluoride present to form arsenic pentafluoride of or SO which reacts with the formed water from the high purity and is illustrated by the following equation: first Step while in contact with the unreacted excess of 65 hydrogen fluoride to form Substantially pure arsenic pentafluoride; and co products US 6,635,231 B2 3 4 (1st rxn) fluorine-containing final product is arsenic pentafluoride. In a preferred operation of Step one of the process, arsenic Thus, the Overall process according to this invention uses pentoxide is mixed in a closed System preferably under a dry only Stoichiometric amounts of hydrogen fluoride and atmosphere, Such as nitrogen, dry air or argon at pressures arsenic pentoxide or arsenic acid while achieving consis less than 10 pounds per Square inch with an excess of 5 tently high yields (80–100%) of arsenic pentafluoride (based anhydrous hydrogen fluoride over the Stoichiometric on arsenic used). There is virtually no waste in the process. amount. It has been found when an excess of anhydrous The resulting purified arsenic pentafluoride was measured hydrogen fluoride is added to a arsenic acid or arsenic pentoxide over the amount theoretically required to form the by trapping in diethyl ether at 0° C. and ambient pressure hexafluoroarsenic acid (HASF), the yield of arsenic pen and weighed. It also can be used directly or condensed into tafluoride increases in the Subsequent reaction Step with gas cylinders for distribution. oleum or SO. The mixing can be achieved by adding The exceSS amount of anhydrous hydrogen fluoride may anhydrous hydrogen fluoride to the arsenic acid or arsenic range from about 7 to 100 weight percent based on the pentoxide with adequate Stirring and cooling. After the amount of hexafluoroarsenic acid, which in turn is based on initial reaction, the arsenic acid or arsenic pentoxide the amount of arsenic pentoxide or arsenic acid used. becomes fluid and the reaction medium is maintained below 15 Preferably, hydrogen fluoride comprises from 20 to about 50 25 C. during the mixing operation to yield the hexafluo percent exceSS over Stoichiometric. roarsenic acid, in the exceSS and unreacted hydrogen fluoride The following example is illustrative of the practice of the and resultant water. method of the present invention. It will be understood, To the resulting liquid hexafluoroarsenic acid and exceSS however, that it is not to be construed in any way limitative and unreacted hydrogen fluoride, in the same reactor a of the full Scope of the invention, Since various changes can Stoichiometric amount of oleum or SO is gradually added be made without departing from the Spirit of the teachings with stirring while maintaining the temperature below 25 contained herein in light of the guiding principles which C. Usually only 80-90% of the theoretical amount of SO is have been set forth above. necessary to accomplish liberation of the ASFs. EXAMPLE The stoichiometric amount of Sulfur trioxide which is 25 added to the heXfluoroarsenic acid is represented by a Into a 1-1 Hastalloy reactor containing 115 g arsenic molecular rate within the range of one molecule of SO for pentoxide (0.5 moles) at 5-10°C.
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