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US4100264A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the preparation of calcium carbonate for use in fluorescent lamp phosphors

Assignee: Philips North America LLC
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Filing: 1976-12-23
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Granted: 1978-07-11
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Expires: 1996-12-23
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Abstract

Abstract A method of producing finely-divided phosphor grade calcium carbonate having a calcite crystalline structure and a very low sodium content. The calcium carbonate is produced from calcium chloride having a high sodium impurity content, such as calcium chloride which is a by-product of the Solvay process for producing soda ash.

Inventors

  • 👤 Herman R. Heytmeijer
  • 👤 Larry P. Rusch
  • 👤 Giuseppe Grasso

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 04:25
CPC Classifications
C; C01; C01F; C01F11/00; C01F11/18; C01F11/185

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 157 words
The method of producing finely-divided phosphor grade calcium carbonate having a calcite crystalline structure and a very low sodium content from calcium chloride having a high sodium impurity content such as 1.6% sodium chloride, which method comprises: (a) forming finely-divided meta-stable vaterite on a continuous basis by continuously adding to an agitated precipitating tank aqueous solutions of calcium chloride and diammonium carbonate in such respective concentrations as to stoichiometrically produce calcium carbonate precipitate and ammonium chloride; (b) separating the resulting meta-stable vaterite precipitate from the mother liquor, and then resuspending the separated vaterite in an aqueous medium; (c) heating the resuspended vaterite to a temperature of at least 80° C for a sufficient period of time to cause the crystal structure of said vaterite to completely convert to calcite; and (d) recovering the resulting calcite, which has a sodium impurity content in the range of from about 10 to 35 ppm, for use in preparing phosphor materials.
Claim 2
Independent Claim 157 words
The method of producing finely-divided phosphor grade calcium carbonate having a calcite crystalline structure and a very low sodium content from calcium chloride having a high sodium impurity content such as 1.6% sodium chloride, which method comprises: (a) forming finely-divided meta-stable vaterite on a continuous basis by continuously adding to an agitated precipitating tank aqueous solutions of calcium chloride and diammonium carbonate in such respective concentrations as to stoichiometrically produce calcium carbonate precipitate and ammonium chloride; (b) separating the resulting meta-stable vaterite precipitate from the mother liquor, and then resuspending the separated vaterite in an aqueous medium; (c) heating the resuspended vaterite to a temperature of at least 80° C for a sufficient period of time to cause the crystal structure of said vaterite to completely convert to calcite; and (d) recovering the resulting calcite, which has a sodium impurity content in the range of from about 10 to 35 ppm, for use in preparing phosphor materials.
Claim 3
Dependent Claim 23 words
The method of claim 1, wherein the concentration of said ammonium carbonate solution and calcium chloride solution is maintained at about 2.5 molar.
Claim 4
Dependent Claim 22 words
The method of claim 1, wherein the pH of the calcium chloride solution is within the range from about 3 to 10.
Claim 5
Dependent Claim 15 words
The method of claim 3, wherein the pH of the calcium chloride solution is 3.5.
Claim 6
Dependent Claim 16 words
The method of claim 1, wherein said vaterite is separated from its mother liquor by filtration.
Claim 7
Dependent Claim 21 words
The method of claim 1, wherein said calcite has a particle size in the range from about 7 to 11 microns.
Claim 8
Dependent Claim 31 words
The method of claim 1, wherein the resuspended vaterite is heated to a temperature of about 85° C to cause the crystal structure of said vaterite to completely convert to calcite.
Claim 9
Dependent Claim 40 words
The method of claim 1, wherein after said meta-stable vaterite precipitate is separated from said mother liquor, said separated meta-stable vaterite is resuspended without water washing in an aqueous medium prior to said heating to effect conversion thereof to calcite.

References Cited (Backward Citations)

US3321269A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-07-10 1982-01-09 1982-07-11 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-07-10 1986-01-09 1986-07-11 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-07-10 1990-01-09 1990-07-11 $7700.00 Window Closed / Lapsed

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