GB2326424A - Two-stroke motorcycle lubricant - Google Patents

Two-stroke motorcycle lubricant Download PDF

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Publication number
GB2326424A
GB2326424A GB9809096A GB9809096A GB2326424A GB 2326424 A GB2326424 A GB 2326424A GB 9809096 A GB9809096 A GB 9809096A GB 9809096 A GB9809096 A GB 9809096A GB 2326424 A GB2326424 A GB 2326424A
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United Kingdom
Prior art keywords
oil
lubricant
stroke motorcycle
stroke
base oil
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Granted
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GB9809096A
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GB2326424B (en
GB9809096D0 (en
Inventor
Yas Tanaka
Paul Fritz-Johnson
Howard Bernard Silver
David James Atkinson
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Castrol Ltd
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Castrol Ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02Petroleum fractions
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04Mixtures of base-materials and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102Aliphatic fractions
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2215/042Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/062Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups bound to the aromatic ring
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01Physico-chemical properties
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/25Internal-combustion engines
    • C10N2040/255Gasoline engines
    • C10N2040/26Two-strokes or two-cycle engines

Abstract

A two-stroke motorcycle lubricant comprising a base oil having a viscosity at 100 C of less than 8 cSt and a pour point below -30 C, preferably below -39 C. The two-stroke motorcycle lubricant further comprises a detergent system based on an ashless, oil-soluble amine. Thetwo-stroke motorcycle lubricant exhibits high levels of cleanliness and low levels of exhaust smoke, whilst maintaining high load carrying capacity. The two-stroke motorcycle lubricant may be dyed.

Description

A Two-Stroke Motorcvcle Lubricant This invention concems a two-stroke motorcycle lubricant.
The function of a lubricant in a two-stroke motorcycle engine is to lubricate and cool moving parts. In a two-stroke motorcycle engine lubricant is burnt along with a fuel charge, which leaves deposits of burnt products in the exhaust, the exhaust port, the combustion chamber and on the piston. These deposits lead to a decrease in the engine performance and they reduce the total working life of the engine, and the exhaust.
Modern two-stroke lubricants usually comprise a balance of additives in a base oil, with a thickener and solvent.
The additives are normally detergents, dispersants and antioxidants. The detergents are oil soluble metallic soaps such as sulphonates or phenates. An example of a detergent that could be used is Hitec 614, which is available from The Ethyl Corporation. Fully formulated additive packages such as Lubrizol 600, which is available from The Lubrizol Corporation, are also used. Lubrizol 600 contains a phenate soap detergent and a succinimide dispersant. The detergents or formulated additive packages are added to lubricants to minimise the build up of deposits.
The base oils are carriers for the additives and they aid in the load carrying capability of the lubricant. The base oils are normally mineral based having a pour point of greater than -120C. A lubricant cannot just comprise a mineral base oil and additives because it would not pass the JASO smoke test FC level (see later for details of the test). In order to pass the JASO smoke test FC level, a polyisobutene (PIB) thickener is added. Polyisobutene has a very low smoke level relative to mineral oil which enables the lubricant to pass the test. The PIB is usually required in a concentration of greater than 20%. Finally, if a high viscosity base oil is used in the lubricant, a hydrocarbon solvent, such as white spirit, is required to aid miscibility with the fuel. Typically the concentration of the solvent is around 20%.
Current lubricants have disadvantages that can affect the longevity of the engine.
Normal detergent additive chemistries are ashcontaining, i.e. they are based on metallic sulphonate or phenate soaps, which can lead to increased deposit formation in the combustion chamber and spark plug whiskering, i.e. a build-up of metallic salts or "ash" on the spark plug electrode. These effects can lead to starting problems, reduced performance and possible engine damage.
The mineral base oils that are routinely chosen for two-stroke lubricants lead to deposits (i.e. decomposition products) that can block the exhaust port and progressively clog the exhaust. This leads to reduced top speed and increased fuel consumption, giving poor combustion and increased emissions.
The lubricity or load carrying capability of two-stroke lubricants is generally acceptable and seizures are uncommon. However, the adequate lubricity of the lubricant is often offset by relatively poor detergency. A good two-stroke lubricant needs all round performance.
These effects described above can occur in less than 5000 km, causing decreased engine performance and possibly even causing damage to the motorcycle engine.
A further disadvantage for the lubricant manufacturer is the dark colour of finished two-stroke lubricants comprising mineral base oils and metallic soap detergents.
Dark coloured lubricants may be perceived by the consumer to be of a lower quality or to contain used oils. It is difficult for the manufacturer to dye dark oils.
The aim of the present invention is to provide further detergents and base oils for a two-stroke motorcycle lubricant.
It is a further aim of the present invention to provide a detergent that will not block exhausts and catalysts, and will maintain excellent levels of cleanliness and very low levels of exhaust smoke, whilst maintaining high load carrying capacity.
In accordance with the present invention there is provided a two-stroke motorcycle lubricant comprising a base oil having a viscosity at 1000C of less than 8 cSt and a pour point below -300C, preferably below -390C.
In accordance with the present invention there is also provided use of an ashless, oil-soluble amine as a detergent in a two-stroke motorcycle lubricant.
The oil-soluble amine is referred to as an ashless, oil-soluble amine because it does not contain any metallic functionality.
The viscosity of the base oil at 1 000C is preferably below 6 cSt, more preferably below 4 cSt, and even more preferably around 2 cSt. The base oil is preferably a mineral oil derived from a naphthenic crude source or a polyalphaolefin.
The ashless, oil-soluble amine preferably has a molecular weight of at least 450, more preferably in the range 900-1500. The ashless, oil-soluble amine is preferably: a polyisobutene-amine; a polyisobutene-phenolamine; a polyetheramine; or a combination thereof.
The inventor has found that if he uses a detergent comprising an ashless, oil-soluble amine in combination with base oils having low viscosity (i.e. less than 8 cSt at 1000C) and low pour point (i.e. below -30 "C) in a two-stroke motorcycle lubricant, the two-stroke motorcycle lubricant exhibits excellent detergency, there is a reduction in the blocking of exhausts and catalysts, and very low levels of smoke are produced. Furthermore, the lubricants are extremely light in colour, they are attractive to the consumer, and they are capable of being dyed different colours by the manufacturer.
The two-stroke motorcycle lubricant may also include a thickener. The thickener is preferably a polyisobutene, preferably having a molecular weight of greater than 450, more preferably greater than 950. The thickener is more preferably a reactive polyisobutene, preferably having a molecular weight of greater than 450, more preferably greater than 950. A reactive polyisobutene differs from a standard polyisobutene in that at least 80% of the terminal unsaturation is in the alpha position. Suitable conventional polyisobutenes are Hyvis 07 and Hyvis 10, and suitable reactive polyisobutenes are Ultravis 5 and Ultravis 10, all of which are available from BP Chemicals. The polyisobutene thickener is added to the two-stroke lubricant to increase the viscosity without having a detrimental effect on smoke and deposit formation. High viscosity mineral base oils may be used to increase a lubricant's viscosity, but they have a negative effect on smoke and deposit formation.
The invention will now be described with reference to the following examples: Examples The base oils used in the examples are described in the following table:
Base oil type Viscosity Pour point /"C @1000C1cSt ASTM D445 ASTM D97 BP 60 Spindle, Naphthenic 2.3 typical A0 max available from BP Oils Nynas T9, Naphthenic 2.0 typical -57 available from Nynas Nynas NS100, Naphthenic 8.4 typical -24 typical available from Nynas PAO 2, Polyalphaolefin 1.6-1.8 -60 available from Mobil PAO 8, Polyalphaolefin 7.7-8.2 -54 available from Mobil BP 500 SN, Solvent neutral 10.8 typical -9 max available from BP mineral Oils The additives used in the examples are described in the following table:
ADX 3866, Detergent package containing 38 % of polyether, and 14 % of available ADX251 C polyisobutene-amine (see below) from Adibis ADX 2510, Polyisobutene-amine (PIB-amine) available from Adibis ADX 4009, Polyisobutene-phenolamine (PIB phenol-amine) available from Adibis Lubrizol Conventional 2 stroke additive package containing calcium 600, phenate detergent and polyisobutene-succinimide dispersant available from The Lubrizol Corporation Paratemps 8 Conventional 2 stroke additive package containing calcium available detergent and polyisobutene-succinic anhydride based dispersant from Paramins The lubricants were blended by adding the base oil to a suitable blending vessel, and adding the thickener. The mixture was agitated using either a mixer or blown air, and the mixture was warmed to 650C. The mixture was then cooled to below 300C and the ashless detergent system was added. The conventional additives such as Lubrizol 600 or Paratemps 8 were blended in at 65"C.
Example 1 Two-stroke motorcycle lubricants were prepared and their performance was tested.
The performance of the lubricant was determined using the JASO standards and an ISO detergency standard that are currently used on commercially available two-stroke motorcycle lubricants. There are four levels of performance: JASO FA; FB; FC; and ISO EGD. JASO FA is the lowest standard and ISO EGD is the highest standard.
The performance criteria that determine the quality of a two-stroke motorcycle lubricant are set out in the JASO engine test sequences, details of which are available from the Japanese Automotive Standards Organisation. A short summary on each test is given below. The tests determine the two-stroke motorcycle lubricant's performance in comparison to a reference two-stroke motorcycle lubricant of known quality, and they give the result as an index number. The parameters that are measured are: JASO Exhaust svstem blocking test (JASO M- 343-92) This test determines the two-stroke motorcycle lubricant's potential for the breakdown products on combustion to build up to such a degree that they affect the engines performance, possibly causing failure, more likely reducing top speed and increasing fuel consumption.
This is referred to as Blocking index (B IX). The minimum index result for JASO FC standard is 90 and the minimum index result for JASO FB standard is 45.
JASO Deteraencv test (JASO M- 341-92) This test determines the high temperature detergency of the two-stroke motorcycle lubricant. The two-stroke motorcycle lubricant's ability to control deposits on the piston, focusing on the piston ring grooves, is also evaluated.
This is referred to as the Detergency index (DIX). The minimum index result for JASO FC standard is 95 and the minimum index result for JASO FB standard is 85.
JASO Smoke test (JASO M- 342-92) This test determines the amount of smoke formed when the two-stroke motorcycle lubricant is burnt.
This is referred to as the Smoke index (SIX). The minimum index result for JASO FC standard is 95 and the minimum index result for JASO FB standard is 45.
JASO Lubricity test (JASO M- 340-92) The lubricity test determines the load carrying capability of the two-stroke motorcycle lubricant at elevated temperatures.
The minimum index result for JASO FC standard is 95 and the minimum index result for JASO FB standard is 95.
CEO ISO EGD Deternencv test (CEC L479-X-94) This test is an extension of the JASO detergency test, however, it is more severe and has higher pass limits. Details of this test are available from the Co-ordinating European Council (CEC).
This is referred to as the EGD detergency index, and piston skirt cleanliness index (EGD DIX and PIX). The ISO standard is 125 minimum DIX and 95 minimum PIX.
Description Formulation Comparative Formulation 1 2 ADX 3866 Ashless 30% detergent package Ultravis 10 Thickener 33% 60 Spindle 2 cSt 37% Naphthenic base oil Paratemps 8 Conventional 4.5% two-stroke detergentidis persant package Brightstock Base oil 10% 500 Solvent Base oil 75.5% Neutral White Spirit Solvent 10% Test results Blocking Index ; 342 75 ISO EGD 144 Detergency index
JASO 114 85 Detergency Index The minimum performance for JASO FC in the blocking index test is 90; and the minimum performance for JASO FB is 45. The minimum performance in the detergency test is 95 for FC level and 85 for FB level. Comparative Formulation 2 is classed as a JASO FB oil. Formulation 1 greatly exceeds the limits for JASO FC.
Example 2 The following two-stroke motorcycle lubricants show the advantage of using a low viscosity, low pour point base oil in place of standard mineral solvent neutral stocks:
Description Formulation 3 Comparative Formulation 4 ADX 251C PIB-amine 4.2 % 4.2 % ADX 4009 PlB-phenolamine 1.54 % 1.54 % Nynas T9 2 cSt naphthenic 61.26 % base oil SN 500 Solvent neutral 61.26 % mineral base oil Ultravis 10 PIB thickener 33 % 33 % Test Results Lubricity index 115 91 Blocking index 236 ; 224 Smoke index 199 50 ISO EGD detergent index 152 101 Piston Skirt index 104 100 Comparing the JASO test results for Formulation 3 with Comparative Formulation 4, the results show that by replacing a standard solvent neutral mineral stock with a naphthenic base oil having low pour point and low viscosity, the performance in the JASO tests can be improved.
Example 3 The following two-stroke motorcycle lubricants show the benefit of using low viscositv base oils:
Description Formulation 5 Formulation 6 ADX 251 C PIB-amine 4.2 % 4.2 % ADX 4009 PlB-phenolamine 1.54 % 1.54 % Nynas NS100 8 cSt naphthenic 61.26 % base oil Nynas T9 2 cSt naphthenic 61.26 % base oil Ultravis 10 PIB thickener 33 % 33 % Test results Lubricity index 96 115 Blocking index 163 236 Smoke index 48 199 ISO EGD detergency index 142 152 Piston Skirt index 104 104 The results for Formulation 6 clearly show the advantages of using a 2 cSt base oil in the JASO tests when compared to Formulation 5 which uses an 8 cSt base oil.
Example 4 The following two-stroke motorcycle lubricants show the benefit of low viscosity base oils:
Description Formulation 7 Formulation 8 ADX 251C PIB-amine 4.2 % 4.2 % ADX 4009 PlB-Dhenolamine 1.54 % 1.54 % PAO 8 8 cSt polyalpha- 61.26 % olefin base oil PAO 2 2 cSt polyalpha- 61.26 % olefin base oil Ultravis 10 PIB thickener 33 % 33 or Test results Lubricity index 107 111 Blocking index 328 344 Smoke index 66 183 ISO EGD detergent index 133 132 Piston Skirt index 97 107 Again, the results for Formulation 8 clearly show the advantages of using a low viscosity (2 cSt) base oil in the JASO tests when compared to Formulation 7 which uses an 8 cSt base oil.
Example 5 The following two-stroke motorcycle lubricants show the advantage of using the ashless, oil-soluble amine detergent in place of a conventional two-stroke detergent system:
Description Formulation 9 Comparative Formulation 10 ADX 251C PIB-amine 4.2 % ADX 4009 PlB-phenolamine 1.54 % Lubrizol 600 Conventional 4.2 % two-stroke additive PAO 2 2 cSt polyalpha- 61.26% 62.8 % olefin base oil Ultravis 10 PIB thickener 33 % 33 % Test result Blocking index 344 312 Description Formulation 11 Comparative Formulation 12 ADX 251 C PIB-amine 4.2 % ADX 4009 PlB-phenolamine 1.54 % Lubrizol 600 Conventional 4.2 % two-stroke additive PAO 8 8 cSt polyalpha- 61.26 % 62.8 % olefin base oil Ultravis 10 PIB thickener 33 % 33 % Test result Blocking index 328 256 The results show that blocking performance can be improved by the use of the ash less, oil-soluble amine detergent in place of a conventional two-stroke detergent package.
Example 6 The following two-stroke motorcycle lubricants show the advantage in lubricant colour of using a highly refined base oil with an ashless, oil-soluble amine detergent over a conventional two-stroke lubricant:
Description Formulation 13 Comparative Formulation 14 ADX 3866 Formulated 30 % detergent package BP 60 SPindle Naphthenic base oil 37 % Ultravis 5 PIB thickener 33 % Paratemps 8 Conventional 4.5 % two-stroke additive package Brightstock Mineral base oil 10% BP 500 SN Mineral solvent 75.5 % neutral base oil White spirit Hydrocarbon solvent 10 ASTM Colour test ASTM Do 500 Less than 1.0 3 The colour of the Formulation 13 using the ash less, oil-soluble amine as a detergent is much lighter than the conventional lubricant (Comparative Formulation 14) as measured in the ASTM colour test.

Claims (20)

Claims
1. A two-stroke motorcycle lubricant comprising a base oil having a viscosity at 100 C of less than 8 cSt and a pour point below 30CC, preferably below -39 C.
2. The two-stroke motorcycle lubricant as claimed in claim 1, wherein the viscosity at 1 000C is below 6 cSt, preferably below 4 cSt, and more preferably around 2 cSt.
3. The two-stroke motorcycle lubricant as claimed in claims 1 or 2, wherein the base oil is a mineral oil derived from a naphthenic crude source.
4. The two-stroke motorcycle lubricant as claimed in claims 1 or 2, wherein the base oil is a polyalphaolefin.
5 A two-stroke motorcycle lubricant comprising an ashless, oil-soluble amine as a detergent system.
6. The two-stroke motorcycle lubricant as claimed in claim 5, wherein the ashless, oil-soluble amine has a molecular weight of at least 450, preferably in range 900-1500.
7. The two-stroke motorcycle lubricant as claimed in claims 5 or 6, wherein the ashless, oil-soluble amine is a polyisobutene-amine
8. The two-stroke motorcycle lubricant as claimed in claims 5 or 6, wherein the ash less, oil-soluble amine is a polyisobutene-phenolamine
9. The two-stroke motorcycle lubricant as claimed in claims 5 or 6, wherein the ashless, oil-soluble amine is a polyetheramine.
10. A two-stroke motorcycle lubricant comprising a base oil as defined in any one of claims 1-4 and an ashless, oil-soluble amine as defined in any one of claims 5-9 as a detergent.
11. Use of a base oil having a viscosity at 100 "C of less than 8 cSt and a pour point below -30 "C, preferably less than -39 C, as a base oil in a two-stroke motorcycle lubricant.
12. The use as claimed in claim 11, wherein the base oil has a viscosity at 10000 of below 6 cSt, preferably below 4 cSt, and more preferably around 2 cSt.
13. The use as claimed in claims 11 or 12, wherein the base oil is a mineral oil derived from naphthenic crude source.
14. The use as claimed in claims 11 or 12, wherein the base oil is a polyalphaolefin.
15. Use of an ashless, oil-soluble amine as a detergent in a two-stroke motorcycle lubricant.
16. The use as claimed in claim 15, wherein the ashless, oil-soluble amine has a molecular weight of at least 450, preferably in the range 900-1500.
17. The use as claimed in claims 15 or 16, wherein the ashless, oil-soluble amine is a polyisobutene-amine
18. The use as claimed in claims 15 or 16, wherein the ashless, oil-soluble amine is a polyisobutene-phenolamine
19. The use as claimed in claims 15 or 16, wherein the ashless, oil-soluble amine is a polyetheramine.
20. The two-stroke motorcycle lubricant as claimed in any one of claims 1-10, wherein the lubricant is capable of being dyed.
GB9809096A 1997-04-29 1998-04-29 A two stroke motorcycle lubricant Expired - Fee Related GB2326424B (en)

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GB2326424A true GB2326424A (en) 1998-12-23
GB2326424B GB2326424B (en) 2000-12-13

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EP (1) EP0979264B1 (en)
JP (1) JP2002505694A (en)
KR (1) KR20010020260A (en)
CN (1) CN1098341C (en)
AT (1) ATE286529T1 (en)
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GB (2) GB9708628D0 (en)
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RU2213128C2 (en) 2003-09-27
US6281173B1 (en) 2001-08-28
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EP0979264B1 (en) 2005-01-05
WO1998049254A1 (en) 1998-11-05
KR20010020260A (en) 2001-03-15
GB9708628D0 (en) 1997-06-18
PT979264E (en) 2005-04-29
AU7059998A (en) 1998-11-24
ES2232943T3 (en) 2005-06-01
ATE286529T1 (en) 2005-01-15
JP2002505694A (en) 2002-02-19
AU743132B2 (en) 2002-01-17
BR9809356A (en) 2000-07-04
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GB2326424B (en) 2000-12-13
ID24588A (en) 2000-07-27
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EP0979264A1 (en) 2000-02-16
CN1253579A (en) 2000-05-17
GB9809096D0 (en) 1998-06-24

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