WO1999042544A1 - Middle-temperature grease for high-loaded friction assemblies - Google Patents

Middle-temperature grease for high-loaded friction assemblies Download PDF

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Publication number
WO1999042544A1
WO1999042544A1 PCT/GB1999/000484 GB9900484W WO9942544A1 WO 1999042544 A1 WO1999042544 A1 WO 1999042544A1 GB 9900484 W GB9900484 W GB 9900484W WO 9942544 A1 WO9942544 A1 WO 9942544A1
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WO
WIPO (PCT)
Prior art keywords
grease
additive
oils
organophosphoric
soap
Prior art date
Application number
PCT/GB1999/000484
Other languages
French (fr)
Inventor
Petro Georgiyovych Cherednichenko
Victor Yevgenovych Bukin
Original Assignee
Vedatech Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Vedatech Ltd. filed Critical Vedatech Ltd.
Priority to AU25367/99A priority Critical patent/AU2536799A/en
Publication of WO1999042544A1 publication Critical patent/WO1999042544A1/en

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    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02—Phosphorus compounds
    • C07F9/28—Phosphorus compounds with one or more P—C bonds
    • C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
    • C07F9/40—Esters thereof
    • C07F9/4003—Esters thereof the acid moiety containing a substituent or a structure which is considered as characteristic
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/08—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-nitrogen bonds
    • 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
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/10—Phosphatides, e.g. lecithin, cephalin
    • 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
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • 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
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • 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
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings

Definitions

  • the invention relates to lubricants used in friction assemblies: rolling-element and slide bearings, hinged bearings, threaded joints, cogged and other gears.
  • the lubricant proposed by the invention is ideally for use under maximum temperatures of up to 200-250°C, it is to be appreciated that the lubricant may be used under a variety of different operating conditions.
  • the known all-purpose grease " Litol-24” is based on naphthenic oil mixtures thickened with a 12- hydroxystearic acid lithium soap.
  • the grease has the following composition (GOST 21150-75), %:
  • the grease has satisfactory anti-scuffing properties, but in many instances it is insufficient for normal plant operation.
  • Fatty acid-based alkyl phosphates are used as additives.
  • the grease is prepared by mixing the constituents at high temperature.
  • the aim of the invention is to produce such a middle-temperature grease for heavily loaded friction assemblies based on soap oils, introducing a new organophosphoric additive into its composition and thereby improving its operating characteristics, such as anti-wear and anti-scuff properties, as applied to the severe operating conditions of various friction assemblies, as well as extending the retention time of the grease on a surface.
  • the problem is resolved by a grease based on soap-thickened oils, containing an organophosphoric additive, and graphite and/or molybdenum disulphide characterised in that the organophosphoric additive essentially comprises a mixture of isomers being the product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine.
  • the soap thickened oils are preferably a mixture of Ca-stearate or Li-12-hydroxystearate with heavy petroleum oils (MC20 oil).
  • the preferable composition of the grease in % by mass is as follows:
  • Molybdenum disulphide - 5-8 Product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine - 1-3
  • Heavy petroleum oils (MC20 oil) - up to 100
  • the Ca-stearate or Li-12-hydroxystearate form part of the grease as thickeners, but when their content is under 8% by mass the grease becomes liquid and is not retained in an open friction assembly; whereas when the content is over 20% the grease's internal friction with the surface rises, which is undesirable in the operation of bearings, since it leads to a deterioration in the adhesive properties of the grease and an increase in energy consumption.
  • the upper temperature limit for the working efficiency of the grease is raised to 150-180°C, and in conjunction with fillers - graphite and molybdenum disulphide - up to 200°C and possibly greater.
  • the organophosphoric additive comprises a mixture of isomers, obtained through the interaction of diethyl phosphite and N-arylsulphonylquinonimine according to the reaction:
  • the additive is obtained by the following method: 1 mole of arylsulphonylquinonimine is added to 1.25 mole of diethyl phosphite while mixing at a temperature of 125°C in batches. The mixture is allowed to stand for four hours at a temperature of 105°C, from which the mixture of isomers of formula (1) is obtained.
  • the additive was tested using friction machines at critical loads by a method of comparing with industrial oils as a reference standard.
  • Table 1 shows the relationship of the grease characteristics to the load on the friction assembly.
  • Table 3 gives the physico-chemical properties of the suggested and known greases: dropping point temperature, penetration, colloidal stability.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Lubricants (AREA)

Abstract

The invention relates to lubricants used in friction assemblies: rolling-element and slide bearings, hinged bearings, threaded joints, cogged and other gears under maximum temperatures up to 200-250°. The proposed middle-temperature grease based on soap-thickened oils contains an organophosphoric additive, graphite and molybdenum disulphide. As an organophosphoric additive it contains a mixture of isomers - a product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine, and as soap-thickened oils - a mixture of Ca-stearate or Li-12-hydroxystearate with heavy petroleum oils (MC20 oil). The proposed grease is far superior to known greases in terms of operating characteristics: anti-wear and anti-scuff properties under severe operating conditions, as well the grease having the property of increased retention time on friction surfaces. Under conditions of high temperature, ingress of water and slag, friction assemblies, bearings in particular, with the grease applied, operate for 200 twenty-four-hour periods and more.

Description

1 MIDDLE-TEMPERATURE GREASE FOR HIGH-LOADED FRICTION ASSEMBLIES
The invention relates to lubricants used in friction assemblies: rolling-element and slide bearings, hinged bearings, threaded joints, cogged and other gears.
Although the lubricant proposed by the invention is ideally for use under maximum temperatures of up to 200-250°C, it is to be appreciated that the lubricant may be used under a variety of different operating conditions.
The known all-purpose grease " Litol-24" is based on naphthenic oil mixtures thickened with a 12- hydroxystearic acid lithium soap. The grease has the following composition (GOST 21150-75), %:
Thickener -12-hydroxystearic acid lithium soap - 13
Additives - antioxidant - diphenylamine - 0.5 or Neozone-phenylnapthylamine - 0.7 - viscosity - polyisobutylene - 4
Dispersion medium -mixture of axle and industrial oils (1 :3) or residual distillate oils from Western Siberian petrololeum - up to 100
The grease has satisfactory anti-scuffing properties, but in many instances it is insufficient for normal plant operation.
The nearest to the proposed grease is grease for heavily loaded rolling-element and slide friction assemblies (Ukrainian patent No. 12341 A, 1996), having the following composition, % by mass: Graphite - 6-20
Molybdenum disulphide - 3-9
Organophosphoric additive - 0.5-5
Figure imgf000004_0001
Soap thickened oils - 63-91.5
Fatty acid-based alkyl phosphates are used as additives. The grease is prepared by mixing the constituents at high temperature.
However, the grease does not ensure the reliable operation of friction assemblies on which heavy loads and high temperatures act simultaneously, since many of its characteristics are unsuited to such operating conditions.
The aim of the invention is to produce such a middle-temperature grease for heavily loaded friction assemblies based on soap oils, introducing a new organophosphoric additive into its composition and thereby improving its operating characteristics, such as anti-wear and anti-scuff properties, as applied to the severe operating conditions of various friction assemblies, as well as extending the retention time of the grease on a surface.
The problem is resolved by a grease based on soap-thickened oils, containing an organophosphoric additive, and graphite and/or molybdenum disulphide characterised in that the organophosphoric additive essentially comprises a mixture of isomers being the product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine.
The soap thickened oils are preferably a mixture of Ca-stearate or Li-12-hydroxystearate with heavy petroleum oils (MC20 oil).
The preferable composition of the grease in % by mass is as follows:
Ca-stearate or Li-hydroxystearate - 8-20 Graphite - 10-18
Molybdenum disulphide - 5-8 Product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine - 1-3
Heavy petroleum oils (MC20 oil) - up to 100
The Ca-stearate or Li-12-hydroxystearate form part of the grease as thickeners, but when their content is under 8% by mass the grease becomes liquid and is not retained in an open friction assembly; whereas when the content is over 20% the grease's internal friction with the surface rises, which is undesirable in the operation of bearings, since it leads to a deterioration in the adhesive properties of the grease and an increase in energy consumption.
Using heavy petroleum oils as the base, the upper temperature limit for the working efficiency of the grease is raised to 150-180°C, and in conjunction with fillers - graphite and molybdenum disulphide - up to 200°C and possibly greater.
The organophosphoric additive comprises a mixture of isomers, obtained through the interaction of diethyl phosphite and N-arylsulphonylquinonimine according to the reaction:
Figure imgf000006_0001
■SO; — + (C5Il,O^L=o
Figure imgf000006_0002
H,c~ ~s°r -N; W
(CJHJOJJP— OH
The additive is obtained by the following method: 1 mole of arylsulphonylquinonimine is added to 1.25 mole of diethyl phosphite while mixing at a temperature of 125°C in batches. The mixture is allowed to stand for four hours at a temperature of 105°C, from which the mixture of isomers of formula (1) is obtained.
The additive was tested using friction machines at critical loads by a method of comparing with industrial oils as a reference standard.
An experiment was conducted until the destruction of the test-pieces as a result of seizure of the friction surfaces. Table 1 shows the relationship of the grease characteristics to the load on the friction assembly.
Table 1
Load (kgf/cm ) 10 15 20 25 30-35 40 45 50
Clean industrial 8.42 9.94 11.76 15.25 20.55 24.34 - - oil (kg cm)
1% Additive 8.38 10.3 12.4 15.75 20.34 23.6 28.38 -
2% Additive 8.46 10.65 12.85 16.12 20.41 23.36 27.87 32.61
3% Additive 8.44 11.01 13.6 16.8 20.25 23.31 27.29 32.58
Figure imgf000006_0003
4% Additive 8.41 11.61 14.49 17.52 20.58 23.28 27.37 32.53
The use of the proposed additive increases the load under which the destruction of the test-pieces takes place. It can be seen from table 1 that on introducing a quantity of 1% additive into the oil, the friction assembly ?s critical load rises by 15%, and on increasing the additive concentration up to 4%, the critical load rises by 30%. The grease is prepared by mixing while heating up to 100°C. The data on the composition of the grease are given in table 2.
Table 2
Grease Contents of constituents, by % mass constituents: sample 1 sample 2 sample 3 sample 4
1. Ca-stearate 20 15 - -
2. Li-12-hydroxystearate - - 8 12
3. Graphite 10 16 18 16
4. Mo disulphide 5 6 8 6
5. Additive 2 1 3 2
Figure imgf000007_0001
6. MC20 oil up to 100 up to 100 up to 100 up to 100
Table 3 gives the physico-chemical properties of the suggested and known greases: dropping point temperature, penetration, colloidal stability.
Table 3
Description of grease compositions property
1 2 3 4 prototype
Penetration
25°C 250 300 240 260 210
Dropping point temperature °C 190 210 195 220 180
Colloidal stability, % of separated oil 11 9 12 8 12
Figure imgf000007_0002
It can be seen from table 3 that the grease composition samples 1-4 with respect to the prototype relate to a single class of lubricating grease according to rheological characteristics (similar penetration properties), whilst according to working characteristics they are far superior to the prototype grease. As a higher dropping point characterizes the thermal stability of the grease - it is higher than the known one - the colloidal stability of the proposed grease is also 1-1.5 times higher.
Grease prepared according to the procedure described above, was tested at the Novolipetsk metallurgical plant in a sheet rolling mill on the output roller conveyor of the " 2000 " mill's continuous furnaces. The grease was placed in assemblies that had been washed with kerosene and air-blown, disconnected from the centralized grease supply. The tests showed that under conditions of high temperature (300-350°C), ingress of water and slag, the assemblies operated without attention for 200 twenty-four-hour periods. Similar assemblies, operating on known greases (in particular, on IP-1 greases of the firm "Mobil plex" , required grease being pumped by the centralized systems at hourly intervals. After opening up the bearings of the assemblies, it was found that after 200 twenty-four-hour periods of continuous operation the quality of the grease had not altered, the quantity of grease remained as before, and on examining the bearings no defects were detected.

Claims

CLAIMS:
1. A grease based on soap-thickened oils, containing an organophosphoric additive, and graphite and/or molybdenum disulphide characterised in that the organophosphoric additive essentially comprises a mixture of isomers being the product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine.
2. A grease according to claim 1 characterised in that the soap thickened oils are a mixture of Ca-stearate or Li-12-hydroxystearate with heavy petroleum oils (MC20 oil).
3. A grease according to either of the preceding claims characterised in that the composition of the grease in % by mass is as follows::
Ca-stearate or Li-hydroxystearate - 8-20
Graphite - 10-18
Molybdenum disulphide - 5-8 Product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine - 1-3
Heavy petroleum oils (MC20 oil) - up to 100
4. A middle-temperature grease for high-loaded friction assemblies based on soap-thickened oils, containing an organophosphoric additive, graphite and molybdenum disulphide, characterised in that as an organophosphoric additive it contains a mixture of isomers - the product of the interaction between diethyl phosphite and N- arylsulphonylquinonimine, and as soap-thickened oils - a mixture of Ca-stearate or Li-12-hydroxystearate with heavy petroleum oils (MC20 oil), with the following ratio of constituents, by % mass:
Ca-stearate or Li-hydroxystearate - 8-20
Graphite - 10-18
Molybdenum disulphide - 5-8 Product of the interaction between diethyl phosphite and N-arylsulphonylquinonimine - 1-3
Heavy petroleum oils (MC20 oil) - up to 100
PCT/GB1999/000484 1998-02-19 1999-02-19 Middle-temperature grease for high-loaded friction assemblies WO1999042544A1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1967572A1 (en) * 2007-02-27 2008-09-10 Setral Chemie GMBH Lubricant additive
JP2012225440A (en) * 2011-04-20 2012-11-15 Ntn Corp Grease-sealed bearing for motor
RU2647118C1 (en) * 2017-03-21 2018-03-14 Общество с ограниченной ответственностью "РОМБ" (ООО "РОМБ") Lubricating electroducing composition for mobile electrical connections

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2635112A (en) * 1949-07-28 1953-04-14 Research Corp Process for producing aminomethylphosphonic acid compounds
WO1994011470A1 (en) * 1992-11-14 1994-05-26 Gkn Technology Limited Greases

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2635112A (en) * 1949-07-28 1953-04-14 Research Corp Process for producing aminomethylphosphonic acid compounds
WO1994011470A1 (en) * 1992-11-14 1994-05-26 Gkn Technology Limited Greases

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 118, no. 19, 10 May 1993, Columbus, Ohio, US; abstract no. 191843q, AVDEENKO A P: "Reaction of N-arylsulfonyl-p-quinonimines with dialkyl phosphites and dialkylsilyl phosphites" page 969; column 1; XP002102957 *
ZH. OBSHCH. KHIM., vol. 62, no. 4, 1992, pages 815 - 821 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1967572A1 (en) * 2007-02-27 2008-09-10 Setral Chemie GMBH Lubricant additive
JP2012225440A (en) * 2011-04-20 2012-11-15 Ntn Corp Grease-sealed bearing for motor
RU2647118C1 (en) * 2017-03-21 2018-03-14 Общество с ограниченной ответственностью "РОМБ" (ООО "РОМБ") Lubricating electroducing composition for mobile electrical connections

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