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Publication numberUS3531410 A
Publication typeGrant
Publication dateSep 29, 1970
Filing dateMar 14, 1968
Priority dateMar 14, 1968
Publication numberUS 3531410 A, US 3531410A, US-A-3531410, US3531410 A, US3531410A
InventorsWarren L Taylor
Original AssigneeTitan Products Co
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Titaniferous biotite lubricant
US 3531410 A
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Description  (OCR text may contain errors)

United States Patent Int. Cl. C10m /02 US. Cl. 252-28 9 Claims ABSTRACT OF THE DISCLOSURE A method for converting titaniferous biotite ore into a lubricating composition by grinding the ore into small particles, expanding the particles by heating to 1000 to 1400 F., cooling the particles, treating the particles with nitric acid at least 5 N, washing the ore particles with an alkaline solution, and heating the particles below 1400 F. until dry. In preferred embodiments, a second acid treatment with phosphoric acid at least 1 N is used after nitric acid treatment; the alkaline solution is a sodium hydroxide solution; the ore is ground to 0.5 to 400 microns; and the expansion and drying steps are carried out below 1250 F.

This invention relates to a method of making lubricating compositions.

The object of this invention is to provide a simple and economical method for preparing an effective, low-cost, solid, particulate lubricating composition from raw titaniferous biotite ore, a relatively rare boitite ore which is unusually rich in titanium and aluminum.

The invention features converting titaniferous biotite ore, having a total silicon, potassium and magnesium content of at least 50% by weight, a total sodium, iron and phosphorus content of at least but less than 50% by Weight, a total manganese, aluminum, strontium, titanium, copper and calcium content of at least 1% but less than 10% by weight, and less than a total 1% by weight of trace elements including nickel, to a lubricating composition by grinding the ore into particles of a preselected size, heating the ore particles to 1000 to 1400 F. to expand the particles, cooling the particles, treating the ore particles with an acid solution comprising nitric acid at least 5 N, washing the ore particles with an alkaline solution, and heating the ore particles at a temperature below 1400 F. until dry. In preferred embodiments, the ore particles are treated with a second acid solution comprising at least 1 N phosphoric acid following the nitric acid treatment and before the alkaline washing; the acid solutions are 5 to 7 N nitric acid and 1 to 3 N phosphoric acid; the alkaline solution is dilute (e.g., 0.2 N) sodium hydroxide; the heating and drying are both carried out below 1250 F.; the acid treatment is carried out at about 100 F.; the ore particles are washed, after nitric acid and alkali treatment, with softened water; and the ore is ground to particle sizes ranging from 0.5 to at least about 400 microns.

Other objects, features and advantages will appear from the following description.

The initial heating (which expands or exfoliates the ore) and the final drying should be carried out at temperatures high enough to effect expansion or drying, but below the roasting or scorching temperature of the ore (usually above 1400 F.). Where temperatures near this upper limit are used, the heating should not be carried on for an excessively long period (e.g., not more than minutes at 1400 F.). The nitric acid used should preferably be about 5 to 7 N for the most efiicient removal of constituents undesirable in lubricating compositions, such as iron and lead salts, as well as dirt and other unwanted materials. Although it is possible to produce an Patented Sept. 29, 1970 'ice effective additive by using only nitric acid, an improved product results if the second phosphoric acid treatment is also used. About 1 to 3 N phosphoric acid is preferred. About A pint acid to one pound ore is presently preferred. Sodium hydroxide is one example of a strong base which may be used for the purposes of neutralizing acid left in the ore sample after aqueous washings but the others may also be used. A 0.2 N solution is presently preferred to effectively neutalize the unwanted remaining acid with- .out introducing an equally undesirable alkalinity into the ore.

The size to which the ore is initially ground, as well as the amounts of ore to be added to lubricants such as greases, depends on the use to be made of the particulate ore composition or of the overall lubricating mixture. In general, the particulate ore composition of the present invention may be used in sizes and amounts comparable to those in which other solid lubricating compositions, such as molybdenum disulfide, are used; preferred particle sizes range from about 0.25 to 400 microns, and preferred amounts range from 0.1 to 70% by total weight of lubricating composition. Among the additive uses for which the particulate ore composition of the present invention is particularly effective are: gear and bearing greases (especially, oscillating bearing lubrication), dryfilm lubrication, for incorporation into plastic parts which require lubrication, and wherever high temperature greases are required; alone, the composition may be used, e.g., as a sealed lubricant for sealed bearings.

EXAMPLE Titaniferous biotite ore was ground to particule sizes of about 200 to 400 microns. The ore particles were heated at 1200 F. for 15 minutes. After cooling to room temperature, the ore particles were mixed, with agitation, for one hour with about A pint, per pound of ore, of 6 N nitric acid, at F. The particles were then filtered, Washed at 100 F. for one hour with softened water (the same orezliquid ratio being observed as with the nitric acid), and filtered again. The particles were then similarly mixed with 2 N phosphoric acid, the same amounts and reaction conditions being observed as in the nitric acid treatment. After filtering, washing with softened water, as above, and filtering again, the ore particles were mixed with 0.2 N sodium hydroxide at 70 F. for one hour, the same particle:liquid ratio being observed. The particles were filtered, washed with softened water for /2 hour at 100 F., and filtered again. Finally, the particles were heated in a furnace at 1200 F. until dry.

The dried ore particles were then added, in amounts ranging from 4 to 20% by total weight of mixture, to Arnolith Grease No. 2, a trade designation for a type of pure petroleum grease. It has been heretofore known that titaniferous biotite ore can be made into such an additive. The grease and greasezore mixtures were subjected to a series of standard wear and temperature tests. The grease: ore mixture was found to have improved wear preventive characteristics over the grease alone, and also to be useful at significantly higher temperatures than the pure grease.

Other embodiments will occur to those skilled in the art and are Within the following claims.

What is claimed is:

1. A method for converting titaniferous biotite ore having a total silicon, potassium and magnesium content of at least 50% by weight, a total sodium, iron and phosphorus content of at least 10% but less than 50% by weight, a total manganese, aluminum, strontium, titanium, copper and calcium content of at least 1% but less than 10% by weight, and less than a total 1% by weight of trace elements including nickel, into a lubricating composition, said method comprising the steps of grinding said ore into particles of a preselected size,

heating said ore particles to 1000 to 1400 F. to expand said particles,

cooling said particles,

treating said ore particles with an acid solution comprising at least 5 N nitric acid,

washing said ore particles with an alkaline solution,

and

heating said ore particles at a temperature less than 1400 F. until dry.

2. The method of claim 1 wherein said first acid solution is a 5 to 7 N solution of nitric acid.

3. The method of claim 1 including the step of treating said ore particles with a second acid solution comprising at least 1 N phosphoric acid following said nitric acid treatment and prior to said alkaline washing.

4. The method of claim 3 wherein said second acid solution is a 1 to 3 N solution of phosphoric acid.

5. The method of claim 1 wherein said alkaline solution is a solution of sodium hydroxide.

6. The metod of claim 1 wherein said ore particles are washed with softened water after said acid treatment and after said alkaline treatment.

7. The method of claim 1 wherein said titaniferous biotite ore is ground to particles sized in the range of about 0.5 to 400 microns.

8. The method of claim 1 wherein each said heating is carried out at a temperature below 1250 F.

9. A method for converting raw titaniferous biotite ore having a total silicon, potassium and magnesium content of at least 50% by weight, a total sodium, iron and phosphorus content of at least 10% but less than 50% by weight, a total manganese, aluminum, strontium, titanium, copper and calcium content of at least 1% but less than 10% by weight, and less than a total 1% by weight of trace elements including nickel, into a lubricating composition, said method comprising the steps of grinding said ore into particles of preselected size, heating the ore particles to 1200 F. for one hour, cooling the ore particles, mixing said ore particles with 6 N nitric acid and maintaining said mixture at 100 F. for about one hour while agitating said mixture, washing said ore particles with softened water to remove said nitric acid, mixing said ore particles with 2 N phosphoric acid and maintaining said mixture at 100 F. for one hour while agitating said mixture, washing said ore particles with 0.2 N sodium hydroxide at room temperature for one halt hour to neutralize remaining acids, washing said ore particles with softened water, and heating said particles at a temperature below 1250 F. until dry.

References Cited UNITED STATES PATENTS 11/1963 Gordon 252-28 4/ 1965 Slater et a1. 252-28 U.S. Cl. X.R. 252-378

Patent Citations
Cited PatentFiling datePublication dateApplicantTitle
US3110399 *Jun 16, 1959Nov 12, 1963Cie De St GobainWorking of titaniferous metals
US3180828 *Dec 5, 1961Apr 27, 1965Slater Ian GriffithLubricant for use in the hot extrusion of metals and metal alloys
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US4400297 *Oct 14, 1980Aug 23, 1983Morca, Inc.Modified hydrated magnesium aluminosilicates and method of preparation
US4515633 *Jun 27, 1983May 7, 1985Morca, Inc.Polymeric materials combined with modified hydrated magnesium aluminosilicates
US4952388 *Sep 11, 1989Aug 28, 1990Corning IncorporatedMethod of treating phyllosilicates
Classifications
U.S. Classification508/141, 252/378.00R, 508/110
Cooperative ClassificationC10N2250/10, C10N2240/02, C10M5/00, C10M2201/062
European ClassificationC10M5/00