Process for preparing pure barium nitrate crystals

• US 3,947,553 A
• Filed: 06/07/1974
• Issued: 03/30/1976
• Est. Priority Date: 06/07/1974
• Status: Expired due to Term

• Current Assignee: Solan Technologies, Inc.
• Original Assignee: The Harshaw Chemical Company
• Inventors: Spicuzza, William F., Moss, Robert H.
• Primary Examiner(s): Stern, Edward
• Application Number:
  US05/477,508
• Time in Patent Office: 662 Days
• Field of Search: 423/395, 423/397, 423/398, 423/399, 23/304, 23/303, 23/300 R
• US Class Current: 423/395
• CPC Class Codes: C01F 11/22 Fluorides
• CPC Class Codes: C01F 11/36 Nitrates

Abstract

A malleable or press-forgeable ingot of barium fluoride, for use as an optical body, may be grown from an ultra-pure precipitate of barium fluoride which contains less than 10 parts per million (ppm) of strontium or calcium. A process is disclosed for crystallizing barium nitrate crystals in the presence of nitric acid, reacting barium nitrate with ammonium carbonate to form barium carbonate, recovering barium carbonate crystals, suspending the barium carbonate crystals in water and precipitating barium fluoride with hydrofluoric acid. The barium fluoride crystals are recovered, dried and then calcined in the presence of ammonium fluoride or bifluoride. Barium fluoride (BaF₂) crystals obtained by the process of this invention contain less than 10 ppm of each strontium and calcium.

Crystals of an alkaline earth metal fluoride which have been calcined in the presence of a fluoride of ammonium are unexpectedly densified, and are particularly suited for melt-growth of an ingot in a known manner. A maximum concentration of 10 ppm of strontium and calcium in a BaF₂ ingot has been found to be the critical demarcation between a frangible prior art BaF₂ ingot and an ingot of BaF₂ which does not unpredictably shatter when cut, and, which may be reliably press-forged into an optical body.

Claims

1. A wet process for preparing essentially pure barium nitrate from relatively pure barium nitrate having a salt of calcium or strontium element present as an impurity, said relatively pure barium nitrate being at least 99.5 per cent pure, comprising, forming an aqueous solution of said relatively pure barium nitrate, adding concentrated nitric acid to said aqueous solution to yield an acid solution having an acid concentration in the range from about 10 to about 15 percent HNO₃ by weight, maintaining said acid solution at a sufficiently low temperature at about room temperature or below, and recovering said essentially pure barium nitrate in which either calcium or strontium element is coprecipitated as a salt in a concentration smaller than the concentration of either calcium or strontium element present in the mother liquor separated from said essentially pure crystals, by a reduction factor in the range from about 5 to about 500.

3. The process of claim 1 wherein said relatively pure barium nitrate contains less than about 500 parts calcium and less than about 500 parts strontium, present as a salt, per million parts by weight based on total solids.

6. The process of claim 1 wherein the element coprecipitated is strontium and said reduction factor for strontium is in the range from about 5 to about 50.

2. A wet process for preparing essentially pure barium nitrate from a relatively pure barium salt convertible to relatively pure barium nitrate having a salt of calcium or strontium elment present as an impurity, said relatively pure barium nitrate being at least 99.5 per cent pure, comprising, forming an aqueous solution of said relatively pure barium nitrate, adding concentrated nitric acid to said aqueous solution to yield an acid solution having an acid concentration in the range from about 10 to about 15 percent HNO₃ by weight, maintaining said acid solution at a sufficiently low temperature at about room temperature or below, and recovering said essentially pure barium nitrate in which either calcium or strontium element is coprecipitated as a salt in a concentration smaller than the concentration of either calcium or strontium element present in the mother liquor separated from said essentially pure crystals, by a reduction factor in the range from about 5 to about 500.

4. The process of claim 2 wherein said relatively pure barium salt contains less than about 500 parts calcium and less than about 500 parts strontium, present as a salt, per million parts by weight based on total solids.

5. The process of claim 2 wherein the element coprecipitated is strontium and said reduction factor for strontium is in the range from about 5 to about 50.