Asbestiform crystalline calcium sodium or lithium phosphate, preparation and compositions

• US 4,346,028 A
• Filed: 11/24/1980
• Issued: 08/24/1982
• Est. Priority Date: 12/14/1979
• Status: Expired due to Term

• Current Assignee: Solutia Incorporated (Eastman Chemical Company)
• Original Assignee: Monsanto Company (Bayer AG)
• Inventors: Griffith, Edward J.
• Primary Examiner(s): Thomas, Earl C.
• Assistant Examiner(s): Langel, Wayne A.
• Application Number:
  US06/209,221
• Time in Patent Office: 638 Days
• Field of Search: 423/306, 423/314, 106/193 J, 260/37 N, 260/37 EP, 260/37 R, 260/39 R, 260/40 R, 260/42.46, 260/42.47, 260/42.49, 260/42.52
• US Class Current: 524/417
• CPC Class Codes: B01D 39/2082 the material being filamentary or fibrous
• CPC Class Codes: C01B 25/45 containing plural metal, or metal and ammonium
• CPC Class Codes: C04B 14/38 Fibrous materials; Whiskers
• CPC Class Codes: C04B 26/02 Macromolecular compounds
• CPC Class Codes: C08K 3/32 Phosphorus-containing compounds
• CPC Class Codes: C08K 7/08 Oxygen-containing compounds
• CPC Class Codes: C10M 103/00 Lubricating compositions characterised by the base-material being an inorganic material containing more than 10% water C10M173/00
• CPC Class Codes: C10M 107/50 containing silicon
• CPC Class Codes: C10M 111/00 Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
• CPC Class Codes: C10M 2201/003 used as base material
• CPC Class Codes: C10M 2201/0403 used as base material
• CPC Class Codes: C10M 2201/0433 used as base material
• CPC Class Codes: C10M 2201/0606 used as thickening agents
• CPC Class Codes: C10M 2201/0616 used as thickening agents
• CPC Class Codes: C10M 2201/0626 used as thickening agents
• CPC Class Codes: C10M 2201/0656 used as thickening agents
• CPC Class Codes: C10M 2201/0666 used as thickening agents
• CPC Class Codes: C10M 2201/0806 used as thickening agent
• CPC Class Codes: C10M 2201/085 Phosphorus oxides, acids or salts
• CPC Class Codes: C10M 2201/0856 used as thickening agent
• CPC Class Codes: C10M 2201/0866 : used as thickening agent
• CPC Class Codes: C10M 2201/0876 : used as thickening agent
• CPC Class Codes: C10M 2201/1013 : used as thickening agents
• CPC Class Codes: C10M 2201/1026 : used as thickening agents
• CPC Class Codes: C10M 2229/02 : Unspecified siloxanes; Silicones
• CPC Class Codes: C10M 2229/025 : used as base material
• CPC Class Codes: C10M 2229/0405 : used as base material
• CPC Class Codes: C10M 2229/0415 : used as base material
• CPC Class Codes: C10M 2229/0425 : used as base material
• CPC Class Codes: C10M 2229/0435 : used as base material
• CPC Class Codes: C10M 2229/0445 : used as base material
• CPC Class Codes: C10M 2229/0455 : used as base material
• CPC Class Codes: C10M 2229/0465 : used as base material
• CPC Class Codes: C10M 2229/0475 : used as base material
• CPC Class Codes: C10M 2229/0485 : used as base material
• CPC Class Codes: C10M 2229/05 : containing atoms other than silicon, hydrogen, oxygen or carbon
• CPC Class Codes: C10M 2229/0505 : used as base material
• CPC Class Codes: C10M 2229/0515 : used as base material
• CPC Class Codes: C10M 2229/0525 : used as base material
• CPC Class Codes: C10M 2229/0535 : used as base material
• CPC Class Codes: C10M 2229/0545 : used as base material
• CPC Class Codes: C10M 7/00 : Solid or semi-solid compositions essentially based on lubricating components other than mineral lubricating oils or fatty oils and their use as lubricants; Use as lubricants of single solid or semi-solid substances compositions in general essentially based on macromolecular compounds C08L
• CPC Class Codes: C10N 2050/08 : Solids
• CPC Class Codes: C10N 2050/10 : Semi-solids; greasy
• CPC Class Codes: D21H 13/36 : Inorganic fibres or flakes
• CPC Class Codes: D21H 5/18 : of inorganic fibres with or without cellulose fibres

Abstract

Asbestiform crystalline calcium M phosphate, where M is sodium or lithium, having a length to average diameter ratio of at least 5:1, can be prepared by forming a melt of a source of oxygen, calcium, phosphorus and M having a mole ratio of about 15 percent to about 30 percent M₂ O, about 48 percent to about 60 percent P₂ O₅ and about 20 percent to about 37 percent CaO, cooling the melt within the range of about 500° C. to about 750° C. for a sufficient time to permit blocks of calcium M phosphate to form, and fiberizing the blocks into the asbestiform crystals. Such asbestiform crystalline calcium M phosphates are useful to prepare composites of organic polymeric materials.

Claims

1. Asbestiform, crystalline calcium M phosphate wherein M is sodium or lithium.

2. An asbestiform phosphate of claim 1 wherein M is sodium having characteristic d-spacings at about 5.29, 4.82, 3.39 and 3.15 Angstroms.

3. An asbestiform phosphate of claim 1 wherein M is lithium having characteristic d-spacings at about 4.75, 3.59, 3.40 and 3.054 Angstroms.

4. An asbestiform phosphate of claim 1, 2 or 3 having an aspect ratio of at least 5:

1.

5. An asbestiform phosphate of claim 1, 2 or 3 having an aspect ratio of at least 10:

1.

6. An asbestiform phosphate of claim 1 or 2 having an aspect ratio of at least 50:

1.

7. An asbestiform phosphate of claim 1 or 2 having an aspect ratio of at least 10:

1 and an average diameter between about 0.05 micron and about 1 micron.

8. An asbestiform phosphate of claim 1 or 2 having an aspect ratio of at least 10:

1 and an average diameter between about 0.1 micron and about 0.5 micron.

9. A process for preparing asbestiform crystalline calcium M phosphate wherein M is sodium or lithium which comprises:

(a) bringing together under reaction conditions a source of oxygen, calcium, phosphorus and M wherein the mole ratios are about 15 mole percent to about 30 mole percent M₂ O, about 48 mole percent to about 60 mole percent P₂ O₅, and about 20 mole percent to about 37 mole percent CaO to form a melt of a phosphate salt mixture;

(b) maintaining the phosphate salt mixture at a temperature below about the melting point of the calcium M phosphate for a sufficient time to form blocks of calcium M phosphate; and

(c) fiberizing the blocks into said asbestiform crystalline calcium M phosphate.

10. A process of claim 9 wherein the melt has a mole ratio of about 17 mole percent to about 25 mole percent M₂ O, about 48 mole percent to about 53 mole percent P₂ O₅, and about 25 mole percent to about 32 mole percent CaO.

11. A process of claim 9 wherein the blocks of calcium M phosphate are separated from other salts by contacting the phosphate salt mixture with water after the blocks of calcium M phosphate have formed.

13. A process of claim 9 wherein the phosphate salt mixture is maintained between about 500°

C. and about 780°

C.

14. A process of claim 9 wherein the phosphate salt mixture is maintained between about 550°

C. and about 750°

C.

12. A process for preparing asbestiform cyrstalline calcium M phosphate wherein M is sodium or lithium which comprises:

(a) bringing together under reaction conditions a source of oxygen, calcium phosphorus and M wherein the mole ratios are about 17 mole percent to about 25 mole percent M₂ O, about 48 mole percent to about 53 mole percent P₂ O₅ and about 25 mole percent to about 32 mole percent CaO to form a melt of a phosphate salt mixture;

(b) maintaining the phosphate salt mixture at a temperature below about the melting point of the calcium M phosphate for a sufficient time to form blocks of calcium M phosphate; and

(c) fiberizing the blocks into said asbestiform crystalline calcium M phosphate wherein the source of calcium is calcium carbonate or calcium hydroxide, and the source of phosphorus is a sodium or lithium phosphate, phosphoric acid or mixtures thereof.

15. A composite which comprises from about 1 to about 99 percent by weight asbestiform crystalline calcium M phosphate wherein M is sodium or lithium, having an aspect ratio of at least 10:

1 and from about 1 to about 99 percent by weight organic polymeric materials.