IP Library Granted Patent US 9,764,963
Granted Patent B2
US 9,764,963 · App. 14/696,652 · Granted Sep 19, 2017

Method for the production of free flowing synthetic calcium fluoride and use thereof

Inventors: Tilman Zipplies (Burghausen, DE); Klaus Hintzer (Kastl, DE); Thorsten Gerdes (Eckersdorf, DE); Achim Schmidt-Rodenkirchen (Bayreuth, DE); Sebastian Seidl (Neumarkt i.d.OPf., DE); Thomas Berger (Hirschau, DE)
Assignee: 3M INNOVATIVE PROPERTIES COMPANY
C01F11/22C01B7/191C01B7/192C01P2004/61C01P2006/12C01P2006/20C01P2006/80
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 9,764,963
App. No.
14/696,652
Granted
Sep 19, 2017
Kind
B2
Abstract

The invention relates to a process for producing free-flowing calcium fluoride particles from a diluted aqueous solution of hydrogen fluoride comprising the step of reacting the diluted aqueous solution of hydrogen fluoride with calcium carbonate particles at a temperature of less than 50° C. The invention further relates to the use of the free-flowing calcium fluoride particles for the manufacturing of anhydrous hydrogen fluoride.

Claims (13)

1. A process for producing free-flowing calcium fluoride particles from an aqueous solution of hydrogen fluoride comprising the step of reacting the aqueous solution of hydrogen fluoride with calcium carbonate particles at a temperature of less than 50° C., further wherein the aqueous solution of hydrogen fluoride has a concentration of hydrogen fluoride of from 0.5 to 40% and the calcium carbonate particles have a mean particle size (d 50 ) of from more than 30 to less than 50 μm.

2. The process of claim 1 , wherein the diluted aqueous solution of hydrogen fluoride has a concentration of hydrogen fluoride of from 1 to 30%.

3. The process of claim 1 , wherein the specific surface area (BET) of the calcium carbonate particles is ≦10 m 2 /g.

4. The process of claim 1 , wherein the diluted aqueous solution of hydrogen fluoride and the calcium carbonate particles are reacted for from 1 to 10 hours.

5. The process of claim 1 , wherein the reaction temperature is in the range of from 20° C. to less than 50° C.

6. The process of claim 1 , wherein the calcium fluoride content of the free-flowing calcium fluoride particles is at least 88%.

7. The process of claim 1 , wherein the content of calcium carbonate in the free-flowing calcium fluoride particles is 12% or less.

8. The process of claim 1 , wherein the mean particle size (d 50 ) of the free-flowing calcium fluoride particles is from more than 30 to less than 50 μm.

9. The process of claim 1 , wherein the specific surface area (BET) of the calcium fluoride particles is from 40 to 80 m 2 /g.

10. The process of claim 1 , further comprising a neutralization step for unreacted hydrofluoric acid.

11. The process of claim 1 , further comprising the step of adding calcium sulfate.

12. The process of claim 1 , wherein the step of reacting the diluted aqueous solution of hydrogen fluoride with calcium carbonate particles is a continuous flow process.

13. The process of claim 1 , wherein the step of reacting the diluted aqueous solution of hydrogen fluoride with calcium carbonate particles is a batch process.

Assignments (7)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: GERDES, THORSTEN; SEIDL, SEBASTIAN
To: UNIVERSITY OF BAYREUTH
Reel/Frame 038384/0298 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: SCHMIDT-RODENKIRCHEN, ACHIM
To: INVERTEC E. V.
Reel/Frame 038384/0619 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: UNIVERSITY OF BAYREUTH
To: 3M INNOVATIVE PROPERTIES COMPANY
Reel/Frame 038384/0957 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: INVERTEC E. V.
To: 3M INNOVATIVE PROPERTIES COMPANY
Reel/Frame 038385/0101 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: BERGER, THOMAS
To: FLUORCHEMIE STULLN GMBH
Reel/Frame 038385/0165 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: FLUORCHEMIE STULLN GMBH
To: 3M INNOVATIVE PROPERTIES COMPANY
Reel/Frame 038385/0257 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2016
From: ZIPPLIES, TILMAN; HINTZER, KLAUS
To: 3M INNOVATIVE PROPERTIES COMPANY
Reel/Frame 038385/0731 →
Priority Claims (1)
EP 14171262 · Jun 5, 2014 · regional
Continuity (1)
Related Publication 20150353372A1 · Dec 10, 2015