US3725276A - Tungsten disulfide lubricant - Google Patents

Tungsten disulfide lubricant Download PDF

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Publication number
US3725276A
US3725276A US00168550A US3725276DA US3725276A US 3725276 A US3725276 A US 3725276A US 00168550 A US00168550 A US 00168550A US 3725276D A US3725276D A US 3725276DA US 3725276 A US3725276 A US 3725276A
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United States
Prior art keywords
sulfur
tungsten disulfide
tungsten
container
disulfide
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Expired - Lifetime
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US00168550A
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English (en)
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M Ohkage
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Individual
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Individual
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M7/00—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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy

Definitions

  • the invention relates to a novel method of preparing a lubricating crystalline tungsten disulfide by an instantaneous exothermic reaction.
  • natural flake graphite or molybdenite composition, MoS the molybdenum ore
  • MoS the molybdenum ore
  • both natural graphite and molybdenite are well known to contain impurities composed mainly of quartz, various sulfide minerals or mining stones constituting their mineral beds. Therefore, even after effecting various procedures of mineral selection and chemical treatments for refining the ore, the perfect removal of such impurities is looked upon as virtually impossible.
  • the Canadian Pat. 630,830 to Spengler et al. concerns the manufacture of molybdenum disulfide using metallic molybdenum or one of the various molybdenum compounds as the molybdenum source and one of the alkaline earth metals, ammonium hydroxide, sulfides, carbonates, sodium and potassium polysulfides, sodium carbonate or potassium carbonate as the sulfur source. Further, the reference discloses the reaction temperature range to be 300 C. to 500 C. This reference is not concerned with tungsten, or tungsten disulfide. Although there is a relationship between molybdenum and tungsten, their respective characteristics were established for the first time by the present invention.
  • British Pat. 630,042 to International, hydrogenation patent of October 1949 relates to a process for converting oxides of heavy metals in floated and fluid state into sulfides with the aid of hydrogen sulfide.
  • the reference products are sulfides intended for use as catalysts for hydrogenation of organic compounds.
  • S is used in an amount equivalent to more than 2 atoms or 3 atoms per atom of W.
  • metal tungsten be kept sufiiciently in contact with sulfur, and the spacing between both elements be decreased by this operation, thereby enabling air exhaust to be effected and the produced amount 0 S0,, to be decreased during the operation.
  • lubricating agent in a very small size particle, it is easy to carry out a crushing operation and to adjust the degree of particle size for converting the product to particles of less than 1.0 micron.
  • the tungsten disulfide of the present invention shows high heat resistance and will perform up to 500 C. in the air. Since tungsten disulfide of the present invention ensures sufficient pressure resistance and lubricity, it can be used to decrease static electricity by 20-50%, as compared with the use of oil or grease. This advantage is very useful in the planning of national electrical recould be, discharged perfectly from the container in 3 hours while keeping the container at temperatures between 550 and 650 C.
  • the tungsten disulfide thus produced was obtained in the form of perfect flake crystals, about 10 microns in diameter, 0.1-0.5 micron in thickness, and showing a color similar to natural molybden disulfide.
  • the average size of particles was found to be 0.1-0.2 micron, and showing very good lubricity.
  • Example I The results of frictional experiments on Example I quirements or calculation of manufacturing costs of inby a 4-ball coefiicient tester were as follows: dividual industr es and fuel consumption of engmes. Friction coeflicient EXAMPLE I.-METHOD OF PREPARING 5.5 kg. of load (oil pressure) 0.018 TUNGSTEN DISULFIDE 10 kg. of load (oil pressure) 0.012 (A) Metal Tungsten 2
  • T M f 1 As follows: I a e o ana ys1s Percent W percent 99.98 W 74.12 Fe do 0.005 S 25.80 Mo dO 0.005 2 Fe 0.02 N.V.R. do 0.010 Mo 0.0036 Size of particles microns 1.0 As 0.00 1 Percent purity except for 02. Orgamc matter N.V.R. 0.04
  • the mixture consisting of tungsten disulfide of very small size particles (less than 0.1 micron) and sulfur thus melted at the abovementioned temperature was caused to flow by gravity gradually into a container provided with a side pipe for distillate induction, 20 cm. in diameter and 30 cm. in height, said container having been preheated to 550 C. beforehand.
  • the material 7600 grs. initially prepared was poured into the container in 2 hours and then the liberated sulfur A mixture of W8 10%, gear oil and antioxidizing agent 10% was used as the test material.
  • Ball bearings used for practical tests Made by certain leading maker Both surfaces of pillow block provided with oil 1%" seal.
  • the shaft of revolution was supported by ball bearings at both ends thereof and a single ball bearing was disposed between both steel wires attached to said single ball bearmg.
  • This grease was sufficiently applied to said two ball bearings at both ends of the shaft and additional oil supplies of same grease were applied thereto from time to time during the running period of the shaft. Said single bearing for test purposes was used in its original state when purchased and no further supply of grease was made until the end of this test.
  • EXAMPLE II Method of preparing tungsten disulfide of submicron size For lubrication in dry state, high temperature lubrication at 300 to 500 C., or for use together with a high viscosity, high consistency oil or fat such as grease or as a composite bearing material with a metal, or for molding in mixture with plastics; the tungsten disulfide obtained by the method of preparing tungsten disulfide is employed.
  • the WS is in the form of very fine powder. This is generally beyond the existing capacity for mechanical pulverization.
  • the mixture After mixing tungsten 5,000 grs. with sulfur powder 5,200 grs., the mixture was put into a heat-resistant steel container provided with heating means and stirrer and melted at C., stirring the melted mixture at a temperature to 250 C. for four hours. Then, the mixture consisting of tungsten disulfide of very small particles (less than 0.1 micron) and an excess of sulfur melted flowed down gradually into a container provided with a side pipe for distillate of sulfur induction, 20 cm. in diameter and 30 cm. in height, said container having been preheated to 550 C. beforehand.
  • nitrogen gas at the rate of about 200 liters per hour was supplied into the reaction container through 2. provided pipe inserted herein so that it was made to cool the reacted material and carry the evaporated sulfur out of the container.
  • the material 10,200 grs. initially prepared was poured into the container in two hours and then the liberated sulfur could be discharged perfectly from the container in another four hours, while keeping the container at a temperature between 550-650 C.
  • the tungsten disulfide thus produced was obtained in very fine flake crystals.
  • the maximum length of the flake was 0.5 micron and minimum length of the flake was 0.01 micron, showing a blackish-grey color.
  • zinc reduction method of tungsten makes it possible to accomplish the reduction at less than a half of the cost required by the former for the materials and supplies including heat and electricity and at less than one-third of the cost for labor. Also, the submicron particles which are scarcely obtained by the hydrogen reduction method can be easily produced by this method.
  • the method of producing WS from W is industrially very advantageous because, as described in the specification of the present application, the manufacturing cost, net yield, and particle size of the product can be easily controlled.
  • Method of preparing lubricating crystalline tungsten disulfide comprising the steps of:
  • said step of mixing comprising mixing one mole of tungsten metal powder and 4-8 moles of sulfur; said step of reacting comprising heating the mixture to -250 C. for about 2-8 hours; said step of crystallizing comprising pouring the melt into a vessel preheated to 550 -650 C.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
US00168550A 1968-01-26 1971-08-03 Tungsten disulfide lubricant Expired - Lifetime US3725276A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP472168 1968-01-26

Publications (1)

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US3725276A true US3725276A (en) 1973-04-03

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US00168550A Expired - Lifetime US3725276A (en) 1968-01-26 1971-08-03 Tungsten disulfide lubricant

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US (1) US3725276A (enrdf_load_stackoverflow)
GB (1) GB1250716A (enrdf_load_stackoverflow)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4676970A (en) * 1985-05-14 1987-06-30 Elkem Metals Company Method for producing metal sulfide and the product produced therefrom
US5327998A (en) * 1992-09-18 1994-07-12 The United States Of America As Represented By The Secretary Of The Air Force Lubrication by sublimation
US20060029494A1 (en) * 2003-05-27 2006-02-09 General Electric Company High temperature ceramic lubricant
US20060245676A1 (en) * 2005-04-28 2006-11-02 General Electric Company High temperature rod end bearings

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2614944C (en) * 2001-04-11 2011-03-29 Sumitomo Metal Industries, Ltd. Threaded joint for steel pipe and method for surface treatment of the threaded joint
CN109852458B (zh) * 2019-03-22 2022-06-21 合肥学院 一种二硫化钨/粉煤灰复合物润滑剂及其制备方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4676970A (en) * 1985-05-14 1987-06-30 Elkem Metals Company Method for producing metal sulfide and the product produced therefrom
US5327998A (en) * 1992-09-18 1994-07-12 The United States Of America As Represented By The Secretary Of The Air Force Lubrication by sublimation
US20060029494A1 (en) * 2003-05-27 2006-02-09 General Electric Company High temperature ceramic lubricant
US20060245676A1 (en) * 2005-04-28 2006-11-02 General Electric Company High temperature rod end bearings
US7543992B2 (en) 2005-04-28 2009-06-09 General Electric Company High temperature rod end bearings

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Publication number Publication date
GB1250716A (enrdf_load_stackoverflow) 1971-10-20

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