EP3921392A1 - Clean-burning gasoline additive to eliminate valve seat recession and toxic deposits - Google Patents
Clean-burning gasoline additive to eliminate valve seat recession and toxic depositsInfo
- Publication number
- EP3921392A1 EP3921392A1 EP19888587.3A EP19888587A EP3921392A1 EP 3921392 A1 EP3921392 A1 EP 3921392A1 EP 19888587 A EP19888587 A EP 19888587A EP 3921392 A1 EP3921392 A1 EP 3921392A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fuel
- calcium
- additive
- sulfonates
- aviation gasoline
- Prior art date
- Legal status (The legal status 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 status listed.)
- Pending
Links
Classifications
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/10—Liquid carbonaceous fuels containing additives
- C10L1/14—Organic compounds
- C10L1/24—Organic compounds containing sulfur, selenium and/or tellurium
- C10L1/2493—Organic compounds containing sulfur, selenium and/or tellurium compounds of uncertain formula; reactions of organic compounds (hydrocarbons, acids, esters) with sulfur or sulfur containing compounds
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- C10L1/183—Organic compounds containing oxygen containing hydroxy groups; Salts thereof at least one hydroxy group bound to an aromatic carbon atom
- C10L1/1832—Organic compounds containing oxygen containing hydroxy groups; Salts thereof at least one hydroxy group bound to an aromatic carbon atom mono-hydroxy
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- C10L1/00—Liquid carbonaceous fuels
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- C10L1/2431—Organic compounds containing sulfur, selenium and/or tellurium sulfur bond to oxygen, e.g. sulfones, sulfoxides
- C10L1/2437—Sulfonic acids; Derivatives thereof, e.g. sulfonamides, sulfosuccinic acid esters
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- C10L2200/00—Components of fuel compositions
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- C10L2200/0204—Metals or alloys
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Definitions
- VSR Valve Seat Recession
- Combustion of gasoline products in the combustion chamber of a piston engine often results in residue and deposits forming around the intake valve and exhaust port and around the cylinder and piston head.
- the composition of gasoline typically comprises C7 - C1 0 aromatic hydrocarbons and C4 - C12 aliphatic compounds that upon incomplete combustion result in engine deposits and combustion residue.
- these fuels may utilize specific compounds known as octane boosters, e.g. aromatic amines, organometallic compounds, or >5% (m/m) aromatic hydrocarbons.
- Typical high-octane compounds used to boost octane rating in gasoline engines, but that often result in heavier engine, sparkplug and valve-seat deposits may include any of the following: aromatic hydrocarbons (e.g., toluene, xylenes, and tri- methylbenzenes); aromatic amines (e.g., aniline, m-toluidine and Cumidine); and organometallic compounds (e.g. tetraethyllead (TEL), MMT (Methylcyclopentadienyl manganese tricarbonyl and ferrocene).
- aromatic hydrocarbons e.g., toluene, xylenes, and tri- methylbenzenes
- aromatic amines e.g., ani
- the octane boosters increase octane ratings of the fuel but tend to cause dirty build-up of deposits and grime in the combustion chamber. This can create a physical barrier, primarily around the exhaust port, which serves to resist valve seat recession. However, this type of build-up can become excessive, leading to loss of compression in the combustion chamber or even engine shut-down - thus such excessive deposits require frequent servicing and diligent cleaning of the spark plugs, often every 25 to 50 hours of engine operation in certain engine applications.
- VSR additives in gasoline to prevent or minimize valve seat recession.
- additives have focused for decades on the use of phosphorous-based compounds, potassium, sodium and manganese organometallic chemistries (see Technical Committee on Petroleum Additive Manufacturers in Europe - (ATC) document 113 published in September 2013).
- TEL Trigger-Edge gasoline
- Fuel additives determine much about the useful nature of any gasoline. TEL is toxic and although it is present in small amounts ( ⁇ 2.1g Pb /gallon), it has a large impact on airborne and municipal water toxicity levels across the nation.
- Aviation gasoline is one type of premium-quality gasoline for somewhat lower-compression piston engines that has historically contained TEL, which tends to create what is sometimes referred to as a lubricity effect which serves to prevent valve seat recession.
- a fuel additive is provided to limit valve seat recession in piston engines.
- the additive provides calcium sulfonates in an amount in fuel formulation effective to limit VSR in engines using the fuel formulation.
- the calcium sulfonates preferably comprise calcium petroleum sulfonates, and the fuel additive may also include detergents, antioxidants and anti-microbial agents.
- the additives find particular use with clean burning aircraft fuels. Also provided are methods for treating vale seat recession in engines by combining the fuel additives to the fuel used by such engines. Further provided are fuel formulations containing calcium sulfonates, and optionally detergents and other components, which result in limited valve seat recession in the engines using such fuels.
- VSR valve seat recession
- This invention utilizes a new technology - a specialized gasoline additive - to limit valve seat recession (VSR), including when using a clean -burning gasoline, preferably an unleaded gasoline.
- VSR valve seat recession
- gasolines particularly clean-burning gasolines, using this invention result in far less corrosion in the engine and oil system (typically caused by the presence of organometallics) leading to longer engine life and longer time between engine overhauls.
- a preferred embodiment is a high-octane premium-quality aviation gasoline comprised of aliphatic hydrocarbons and oxygenates with no or very low levels of aromatics, amines or metals as outlined herein.
- This invention uses a special formulation of components blended in solution as a fuel Additive (the "Additive”) which is added at a specified treat rate to appropriate gasoline or aviation gasoline compositions.
- Additive a fuel Additive
- This invention provides a unique and novel approach to anti-VSR additives, resulting in a soft, easy-to-clean, non-toxic thin residue film which coats the combustion area of the cylinder, piston head, intake and exhaust port areas, thereby treating VSR (wear-and-tear) to the mechanical parts.
- the Additive of the present invention is tailored to work with any gasoline, but also finds particular advantage in use with clean-burning gasoline to treat VSR. Without being bound to any particular mechanism of action, it appears that the VSR Additive produces a very thin layer of a soft, easy to clean, non-toxic residue which accumulates and then stabilizes in the combustion chamber. This produces a minimal but useful buildup of soft, white residue in and around the intake and exhaust ports during the combustion process. The result is a thin, soft residue that serves as a barrier to treat valve seat recession and to leave the combustion chamber with virtually no wear-and- tear on the valve seat and with freedom from harmful deposits.
- the Additive is useful limiting VSR.
- VSR is meant to include a reduction of VSR as compared to operation of the engine with the same fuel formulation, but without the Additive. This reduction may include, for example, a reduction in VSR of at least 10%, preferably at least 25%, and most preferably at least 50%.
- the Additive is effective to substantially eliminate VSR, meaning that VSR is reduced by at least 90%.
- use of the Additive eliminates VSR.
- the Additive package is free of an octane booster and/or a chemical scavenger, and in an aspect the final fuel formulation including the Additive is free, and preferably substantially free, of an octane booster and/or a chemical scavenger. Being substantially free refers to the final fuel formulation constituting less than 1 wt % of octane booster and/or chemical scavenger.
- the inventive Additive includes one or more fuel-soluble calcium sulfonates.
- the calcium sulfonates preferably comprise calcium petroleum sulfonates.
- the calcium is provide to provide a low treat rate ranging from about 5 to about 100 ppm (as Ca 2+ ), alternatively at least 5 or 10 ppm, in the fuel formulation.
- Sulfonates can be derived from petroleum fractions, from lignin, and from fatty oils.
- Natural petroleum sulfonates are defined as those manufactured by sulfonation of crude oil, crude distillates, or any portion of these distillates in which hydrocarbons present are not substantially different from their state in the original crude oil.
- Calcium petroleum sulfonate is calcium salt of sulfonic acid made by processing heavy alkaline benzene of suitable fraction with sulfuric acid or sulfur trioxide and refining by liquid extraction by using suitable alcoholic solvent and precipitating insoluble salts by control of PH and centrifuging.
- Petroleum sulfonate is mainly obtained by treating high-boiling petroleum fractions in a stirred tank reactor (STR) or in a falling- film reactor (FFR). Synthesis of petroleum sulfonate surfactant may be made with ultra-low interfacial tension in a rotating packed bed reactor.
- Sulfonation may be defined as any chemical process by which the sulfonic acid group (SO2OH) or the corresponding salt or sulfonyl halide group (e.g. -SO2CI) is introduced into an organic compound.
- SO2OH sulfonic acid group
- -SO2CI sulfonyl halide group
- the calcium compound is preferably formulated in a compatible, low-toxicity carrier suitable for use in combination with gasoline fuels.
- a compatible, low-toxicity carrier suitable for use in combination with gasoline fuels.
- such carriers include, for example, C7 to C9 arene hydrocarbons.
- the Additive further may comprise one or more detergents.
- the detergents typically comprise, for example, from 50 to 200 ppm of the Additive.
- a polyolefin alkyl phenol alkyl amine is a suitable detergent.
- Detergents leave the intake clean, while the calcium forms a soft white film during combustion which is easily cleaned by a light brush or rinsed with water and air dried. This is dramatically easier to clean than removing TEL or MMT organometallic deposits which form once fuel is combusted and caked onto engine parts - requiring frequent and excessive physical effort to clean off the spark plugs.
- a detergent will depend on the nature of the fuel. For clean-burning fuels there will be less need for a detergent, whereas fuels which are not clean-burning may benefit from addition of a detergent. This is demonstrated in the examples provided hereafter. The determination of the use of a detergent, and the amount, is within the ordinary skill in the art based on assessment of the results of using the calcium sulfonate with a given fuel.
- the detergent is used with the calcium sulfonates for addition to a fuel formulation requiring the detergent to make the calcium sulfonates effective to limit VSR.
- certain fuels benefit from the combination of calcium sulfonates and detergents in order to enhance the effect of either alone in limiting VSR.
- the calcium sulfonates and the detergents are used in amounts and proportions that increase the VSR limiting effect of the calcium sulfonates.
- the combination of the one or more calcium sulfonates and the one or more detergents provides enhanced limiting of VSR that is at least 25%, preferably at least 50%, better than use of the calcium sulfonates alone for a given fuel and engine. For example, if the calcium sulfonates limit VSR to 12%, then the addition of the detergent results in a limitation of VSR to at most 9%, or at most 6%.
- An additional component may comprise an antioxidant, suitable for use with fuel formulations.
- An example of a suitable antioxidant is 2,6-ditertiaiy butyl-4- methylphenol. The determination of the use of an antioxidant, and the amount, is within the ordinary skill in the art based on assessment of the results of using the calcium sulfonate with a given fuel.
- an anti-microbial agent such as 4,4,6-trimethyl-l,3,2- dioxaborolane
- an anti-microbial agent such as 4,4,6-trimethyl-l,3,2- dioxaborolane
- a color dye for example Blue (1,4-dialkylaminoanthraquinone), or Red (alkylazobenzene-4-azo-2- naphthol) dyes, or possibly other colors.
- the addition of such coloring agent may be prescribed by international fuel regulatory organizations (e.g. ASTM International) for quality control and color calibration when used in aviation gasolines.
- This invention is a specially designed Additive uniquely tailored to work with specific fuels, particularly clean -burning aviation gasolines that combust with very little or no organometallic, amines or hydrocarbon deposits - i.e. those fuels comprised of
- This Additive can be applied to any gasoline formulation for use in a piston engine, no matter the formulation, but is particularly useful when used in very clean burning unleaded gasoline blends comprised of aliphatic hydrocarbons or any combination of aliphatic hydrocarbons and oxygenates as described herein.
- the cleanest burning high-octane gasoline preferred an oxygenate compound.
- Our scientists tested various known high-octane aviation gasolines (100LL, 100-octane with MMT, 100-octane with aniline) were tested.
- 100R the cleanest burning oxygenated aviation gasoline, which in various embodiments contained > 80% Ethyl Tert-Butyl Ether and ideally > 95% ETBE, however some combination of other ethers (MTBE, TAME, THME, Diisopropyl Ether, etc.) and trace amount of alcohols (methanol, ethanol, etc.) in the fuel as acceptable within industry limits on water solubility.
- a further aspect of this invention is the Additive formulation in a clean-burning fuel eliminates the use of harmful chemicals that can cause acidity, corrosion, organometallic deposits and sparkplug fouling, and sludge build-up that by their chemical nature can cause unwanted wear-and-tear throughout the piston engine.
- Using this special Additive with clean-burning gasoline results in less frequent and less extensive engine maintenance requirements, conducted at longer time intervals between servicing, thereby creating an economic benefit to operators of aircraft piston engines.
- the present invention provides an Additive package suited for addition to an existing fuel formulation. This addition could occur at any point in the preparation and use of a given fuel formulation.
- the calcium sulfonate may be added to the other fuel components.
- the calcium sulfonate may be provided by itself, or it may be in combination with other intended fuel components.
- the calcium sulfonate forms a components of an Additive package that includes other components intended to work in combination with the calcium sulfonates, such as those described herein including detergents and/or antioxidants.
- the Additive package may then also comprise a carrier effective to suspend or otherwise support, including by solution, the calcium sulfonates
- the Additive package is configured to be used for addition to a fuel formulation as provided to an end user.
- the Additive package may be separately contained and added directly to the fuel in a storage receptacle or in the fuel tank of an aircraft or the like.
- the Additive package may be specifically supplied with a combination of related components, e.g., the calcium sulfonates and other components such as carrier, detergent, antioxidant, dye, etc.
- the present invention further includes a method of treating VSR using the Additive.
- the method comprises adding the Additive to a fuel formulation to provide the calcium sulfonates at a level to provide the concentrations of calcium in the final fuel formulation as set forth herein.
- the method may comprise adding the Additive during the blending of the fuel formulation.
- the method may also comprise adding the
- Additive to the fuel formulation as it is received from the producer This may occur by way of adding the Additive to the fuel while in storage or as present in a fuel tank, such as the tank of an aircraft.
- An aviation gasoline blend comprising at least one C4 - C10 aliphatic hydrocarbon and at least one oxygenated compound, with less than 5% arene hydrocarbons and no amines or organometallic compounds, having a motor octane of at least 99.6 MON was tested without any anti-VSR additive.
- the result was an excessive level of valve recession as the fuel combustion ran "too clean" and the metal-on-metal impact of the valves undesirably eroded the facing edge of the valves with the valve seat making the valve seat, out-of-tolerance after the 250 hours test of engine operation.
- Aviation gasoline blend comprising at least one C4 - C10 aliphatic hydrocarbon and at least one oxygenated compound, with less than 5% arene hydrocarbons and no amines or organometallic compounds, having a motor octane of at least 99.6 MON was tested with a phosphorous-based anti-VSR additive. The result was a limited level of valve recession, still within tolerance, but sludge and grime were excessive and difficult to remove.
- Aviation gasoline blend comprising at least one C4 - C10 aliphatic hydrocarbon and at least one oxygenated compound, with less than 5% arene hydrocarbons and no amines or organometallic compounds, having a motor octane of at least 99.6 MON was tested with a potassium -based anti-VSR additive.
- the result was a limited level of valve recession, still within tolerance, but sludge and grime were excessive and difficult to remove. Potassium tends to cake-up and form chunks of debris which can be dangerous when dislodged in the combustion or exhaust chamber.
- Aviation gasoline blend comprising at least one C4 - C10 aliphatic hydrocarbon and at least one oxygenated compound, with less than 5% arene hydrocarbons and no amines or organometallic compounds, having a motor octane of at least 99.6 MON was tested with a manganese-based anti-VSR additive (MMT).
- MMT manganese-based anti-VSR additive
- the result was a limited level of valve recession, but sludge and grime were excessive. Spark plug deposits shut down the engine between regular cleaning intervals. MMT tends to cake-up and form chunks of debris which can be dangerous when dislodged in the combustion chamber.
- MMT manganese-based anti-VSR additive
- the response of the Additive package of this invention was tested in several different test engine runs using SAE standard testing for the response of the Additive package.
- the standard calls for a 250-hour test, with the engine under full load. In total, 13 of these test engines were run the full 250 hours to evaluate additive response.
- This test was conducted on a nominal blend of 100R, a clean-burning aviation gasoline with 75% aliphatic hydrocarbons and 25% oxygenates (m/m) with the maximum treat rate prescribed by the SPEC-lOOR-18 specification.
- 8 other full runs were conducted with decreasing amounts of the Additive package in this invention.
- the piston engines were purchased new, fully dimensionally measured, and reassembled before the run. Oil was changed initially at 25 hours and thereafter every 50 hours. For comparison of data, 100LL avgas with tetraethyllead and ethanol-free automotive gasoline were each run on a full additive test engine. At the completion of each run, the test engine was torn down and completely measured, evaluated, and photographed.
- VSR pass / fail was only one criteria of the test:
- 100LL avgas created lead deposits which allowed the fuel to meet valve seat recession requirements.
- the lead deposits required 25- to 50-hour inspections and cleaning.
- Autogas typically has up to 50% aromatics and high boiling compounds which impact the heavy exhaust valve deposits; autogas detergents may clean the intake.
- the 100R baseline fuel with no additives was spotless on both valve seats, but regrettably the amount of valve seat wear was "high” due to the metal-on-metal impact (i.e., without appropriate additives the fuel burns "too clean", with no deposits).
- Table 3 reports the results of using very clean-burning unleaded avgas 100R (second column), and using small amounts of calcium (2.5 ppm, 5 ppm and 7.5 ppm) from calcium petroleum sulfonate, with 10 mg/L of antioxidant (2, 6-ditertiary butyl-4- methylphenol).
- the use of 7.5 ppm of Ca for test blend TA 402 yielded a passing result with respect to VSR.
- Addition of 50 ppm of detergent for test blend TA 401 helped clean the intake on TA401 and provided passing results.
- organometallic compounds provided passing results using an Additive containing at least lOppm calcium petroleum sulfonates plus anti-oxidants to result in no valve seat recession.
- an aviation gasoline blend comprising at least one C4 - C10 aliphatic hydrocarbon and at least oxygenated compound, with less than 5% arene hydrocarbons and no amines or organometallic compounds, having a motor octane of at least 99.6 MON was tested with the calcium-based anti-VSR Additive.
- the result was a level of valve recession of zero wear - like new.
- the calcium component of the additive formed a thin white layer of soft film which prevented the valve seat from wearing during the 250-hour engine test. Additional testing found that the addition of detergents kept the intake clear from any deposits and dirt buildup.
- the antioxidant reduced the impact of any gum-forming compounds.
- the anti-microbial agent reduced the risk of microbial growth in unleaded fuels that might be exposed to growth propagating conditions.
- Anti-VSR Calcium petroleum sulfonates
- Anti-Oxidant 2,6-ditertiary butyl-4-methylphenol
- Anti-microbial 4, 4, 6 - trimethyl- 1, 3, 2-dioxaborinane (Optional)
- Blue Dye 1,4-dialkylaminoanthraquinone (Optional)
- Red Dye alkylazobenzene-4-azo-2-naphthol (Optional)
- the present invention has many aspects. These further include the following.
- the fuel Additive may be comprised of at least 10 ppm of calcium petroleum sulfonates in solution with a liquid carrier (an C7 to C9 arene hydrocarbon), blended with any gasoline composition, which upon combustion prevents valve seat recession, intake coking, and reduces post-combustion deposits in the exhaust chamber.
- a liquid carrier an C7 to C9 arene hydrocarbon
- the fuel Additive in the first aspect may be blended
- the fuel Additive of the first or second aspect may be combined with 50 to 250 ppm of detergent - such as Polyolefin alkyl phenol alkyl amine.
- the fuel Additive of the first or second aspect may be combined with up to 20 mg/L of antioxidant - 2,6-ditertiary butyl-4-methylphenol.
- the fuel Additive of the first or second aspect may be combined with up to 40 mg/L of an anti-microbial agent - 4, 4, 6 - trimethyl- 1, 3, 2-dioxaborinane.
- the fuel Additive of the first or second aspect may be combined with any approved dyes for quality control and color calibration for fuel safety.
- a fuel Additive may be comprised of at least 10 ppm of calcium petroleum sulfonates in solution with a liquid carrier (an C7 to C9 arene hydrocarbon), blended with any clean-burning aviation gasoline with at least a 99.6 MON octane rating, comprised of at least one C4 to C8 aliphatic hydrocarbon and at least one oxygenated-compound and with no more than 5% aromatic hydrocarbons, and no amines or organometallic compounds, which upon combustion prevents valve seat recession, intake coking, and reduces post-combustion deposits in the exhaust chamber.
- a liquid carrier an C7 to C9 arene hydrocarbon
- the fuel Additive of the third aspect may be combined with 50 to 250 ppm of detergent - such as Polyolefin alkyl phenol alkyl amine.
- the fuel Additive of the third aspect may be combined with up to 20 mg/L of antioxidant - such as 2,6-ditertiary butyl-4-methylphenol.
- the fuel Additive of the third aspect may be combined with up to 40 mg/L of an anti-microbial agent - such as 4, 4, 6 - trimethyl-1, 3, 2-dioxaborinane.
- an anti-microbial agent - such as 4, 4, 6 - trimethyl-1, 3, 2-dioxaborinane.
- the fuel Additive of the third aspect may be combined with any approved dyes for quality control and color calibration for fuel safety - such as Blue Dye: 1,4- dialkylaminoanthraquinone and Red Dye: alkylazobenzene-4-azo-2-naphthol.
- the fuel Additive of any of the first, second or third aspects may comprise at least 10 ppm of calcium petroleum sulfonates in a liquid carrier (an C7 to C9 arene hydrocarbon), blended with any combination of specified detergents, anti oxidants, anti-microbial agents and dyes and subsequently blended with any gasoline composition or aviation gasoline composition, which upon combustion prevents valve seat recession, intake coking, and reduces post-combustion deposits in the exhaust chamber.
- a method of treating VSR in a fuel formulation may comprise addition of a fuel Additive of the first, second or third aspects to yield a fuel formulation having the indicated amounts of calcium sulfonates in the final fuel.
- a fuel formulation comprising calcium sulfonates and other components, as disclosed herein, at amounts operative to limit, or eliminate, VSR for the engine in which the fuel formulation is used.
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Abstract
Description
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US201862771292P | 2018-11-26 | 2018-11-26 | |
PCT/US2019/063353 WO2020112842A1 (en) | 2018-11-26 | 2019-11-26 | Clean-burning gasoline additive to eliminate valve seat recession and toxic deposits |
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EP3921392A1 true EP3921392A1 (en) | 2021-12-15 |
EP3921392A4 EP3921392A4 (en) | 2023-01-11 |
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US (2) | US20200165534A1 (en) |
EP (1) | EP3921392A4 (en) |
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Family Cites Families (9)
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US4718919A (en) * | 1986-10-01 | 1988-01-12 | Ppg Industries, Inc. | Fuel additive |
US5160350A (en) * | 1988-01-27 | 1992-11-03 | The Lubrizol Corporation | Fuel compositions |
US5407453A (en) * | 1993-03-19 | 1995-04-18 | The Lubrizol Corporation | Deposit cleaning composition for internal combustion engines |
ES2248887T3 (en) * | 1997-02-03 | 2006-03-16 | Ciba Specialty Chemicals Holding Inc. | POLYFUNCTIONAL LIQUID ADDITIVES TO IMPROVE FUEL LUBRICITY. |
US7862629B2 (en) * | 2004-04-15 | 2011-01-04 | Exxonmobil Research And Engineering Company | Leaded aviation gasoline |
US20100132253A1 (en) * | 2008-12-03 | 2010-06-03 | Taconic Energy, Inc. | Fuel additives and fuel compositions and methods for making and using the same |
US20100206260A1 (en) * | 2009-02-18 | 2010-08-19 | Chevron Oronite Company Llc | Method for preventing exhaust valve seat recession |
EP3161112B1 (en) * | 2014-06-27 | 2021-08-04 | BP Oil International Limited | Aviation gasoline composition, its preparation and use |
CN107532096A (en) * | 2014-07-14 | 2018-01-02 | 斯威夫特燃料有限责任公司 | For piston-engined unleaded gas preparation |
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2019
- 2019-11-26 CA CA3121161A patent/CA3121161A1/en active Pending
- 2019-11-26 US US16/696,429 patent/US20200165534A1/en not_active Abandoned
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CA3121161A1 (en) | 2020-06-04 |
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