EP3004298B1 - Procédé de fabrication de polymère-graisse - Google Patents
Procédé de fabrication de polymère-graisse Download PDFInfo
- Publication number
- EP3004298B1 EP3004298B1 EP14728889.8A EP14728889A EP3004298B1 EP 3004298 B1 EP3004298 B1 EP 3004298B1 EP 14728889 A EP14728889 A EP 14728889A EP 3004298 B1 EP3004298 B1 EP 3004298B1
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- EP
- European Patent Office
- Prior art keywords
- shear
- liquid composition
- process according
- mixing
- temperature
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- 239000004519 grease Substances 0.000 title claims description 56
- 229920000642 polymer Polymers 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000203 mixture Substances 0.000 claims description 84
- 239000007788 liquid Substances 0.000 claims description 53
- 238000000034 method Methods 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 44
- 230000008569 process Effects 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 25
- 239000010687 lubricating oil Substances 0.000 claims description 18
- 230000008719 thickening Effects 0.000 claims description 16
- 230000001050 lubricating effect Effects 0.000 claims description 13
- 230000003068 static effect Effects 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 5
- 235000019198 oils Nutrition 0.000 claims description 5
- 238000012546 transfer Methods 0.000 claims description 5
- 229920002678 cellulose Polymers 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
- 239000002480 mineral oil Substances 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 239000010696 ester oil Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 238000010791 quenching Methods 0.000 description 14
- 239000000314 lubricant Substances 0.000 description 12
- 239000002562 thickening agent Substances 0.000 description 12
- 230000000171 quenching effect Effects 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000002199 base oil Substances 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000010008 shearing Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 239000008240 homogeneous mixture Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000012080 ambient air Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010689 synthetic lubricating oil Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
Images
Classifications
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
-
- 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
- C10M169/00—Lubricating 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
- C10M169/02—Mixtures of base-materials and thickeners
-
- 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/003—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions used as base material
-
- 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
-
- 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/024—Propene
-
- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/2805—Esters used as base material
-
- 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/102—Polyesters
-
- 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
-
- 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
-
- 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
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2217/044—Polyamides
-
- 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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
-
- 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
-
- 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—Semi-solids; greasy
-
- 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
- C10N2070/00—Specific manufacturing methods for lubricant compositions
Definitions
- the present invention relates to the field of polymer greases and methods for the manufacture thereof.
- Greases are used in a variety of engineering applications to maintain a lubricant between moving machine surfaces, such as found, for example, in bearings.
- a grease exhibits shear-thinning rheological properties, which means that the viscosity of the grease reduces under shear.
- a grease typically comprises a lubricant, such as a lubricating mineral oil, and a thickener substance. Under non-shear conditions, the thickener acts as a sponge-like matrix that holds the lubricating oil. As a result, the grease exhibits the characteristics of a solid or semi-solid.
- the lubricating oil may be released from the matrix both under static or dynamic conditions. In particular, when a shear force is applied, the lubricating oil separates from the thickener matrix and results in the grease exhibiting lubricating properties.
- the properties of the lubricating oil are important in determining the lubricating properties of the grease.
- the interaction of the lubricating oil and the thickener is important in determining, for example, the longevity of a grease when used as a lubricant.
- the oil replenishing characteristics of the grease are critical to ensure that the lubricating oil is reabsorbed into the matrix once the shear is removed from the lubricated system.
- Lubricant greases for bearings are described in EP 0700986 , EP 0795597 and EP 0795598 .
- a polymer is used as the thickener in a grease composition.
- the lubricating oil is chosen to be a conventional synthetic lubricating oil, such as a mineral oil, a synthetic hydrocarbon oil or an ester oil.
- a typical method for the manufacture of a grease is to form a homogeneous mixture of the desired lubricating oil and thickener, and then to rapidly cool or quench it. This is generally achieved by pouring the composition onto a cooling table.
- the present invention aims to address at least some of the problems associated with the prior art or at least to provide a commercially useful alternative thereto.
- a process for the manufacture of a lubricating grease composition comprising the steps of: providing a liquid composition comprising a mixture of lubricating oil and a thickening polymer, wherein the mixture is essentially homogenous such that it does not have any domains of separate thickening polymers within the lubricating oil or vice versa, flowing the liquid composition through a shear-mixing device to mix and cool the liquid composition to form a lubricating grease composition, wherein the thickening polymer forms from 5 to 20 wt% of the essentially homogeneous liquid composition, and wherein the liquid composition flows through the shear-mixing device along a flow-path provided with one or more temperature-controlled portions to each heat and/or cool the liquid composition, and wherein the shear-mixing device comprises one or more pairs of heat-transfer plates between which the liquid composition is flowed, wherein the surface of at least one plate is provided with surface features in the flow path of the liquid composition which are surface textures that act as baffles for the
- the present invention provides a process for the manufacture of a lubricating grease composition, the process comprising the steps of:
- the present inventors found that a number of problems associated with the prior art could be addressed by using the new method disclosed herein.
- the method avoids pouring large production batches onto a casting table. It provides control over temperature variations, cooling rates and homogeneous heat distribution in the bulk. It further allows for the adjustment of cooling conditions to optimize grease production quality and avoids direct contact with ambient air, resulting in oxidation, contamination, and dust and particle ingress. Importantly, however, it also allows for adjustment of cooling conditions to obtain greases with different properties, either as a result of the cooling profile or because it allows the use of novel materials.
- the present inventors have found that the conventional pouring-and-quenching method is not ideal for processing grease since it does not allow control of the cooling rate, or heat dissipation in the bulk material during cooling. Indeed, in contrast to the present method, such a cooling process cannot be adjusted to modify the grease properties.
- the components forming the liquid composition are essentially homogeneous and typically not visibly discernible in the mixture.
- the mixture preferably does not have any domains of the separate thickening polymers within the lubricating oils or vice versa.
- the liquid composition is homogeneous.
- the essentially homogeneous liquid composition is provided at a temperature of from 150 to 350°C, preferably from 200 to 250°C. These temperatures are generally required to ensure that the components forming the grease are thoroughly mixed and homogeneous. However, the properties of the components selected will determine the minimum temperature required to establish an essential homogeneous liquid composition.
- Lubricating oils and thickening polymers are well known in the field of grease manufacture. The novel method has been found to permit a broader range of materials to be used when forming greases.
- the lubricating oil comprises oils selected from mineral oils, synthetic hydrocarbons, ester oils, vegetable oils, and mixtures of two or more thereof.
- the thickening polymer comprises a polymer selected from polyamides, polyesters, polyethylene oxides, polyethylene, polypropylene, polylactides, cellulose or cellulose derivatives, and mixtures of two or more thereof. The recited polymers are intended to encompass copolymers, as well.
- the ratio of the lubricating oil and the thickening polymer helps to determine the structure of the final grease.
- the inventors have found that it is preferred when the thickening polymer forms from 5 to 20 wt%, preferably 9 to 15 wt% of the essentially homogeneous liquid composition. Working within this range ensures that the lubricating properties can be enhanced while providing a readily producible and stable grease product.
- the liquid composition is flowed through a shear-mixing device to mix and cool the liquid composition to form a lubricating grease composition.
- the shear mixing device is preferably a shear-mixing conduit, preferably having a variable cross-sectional area.
- the use of a shear-mixing conduit is advantageous because it has contact surfaces for controlling the temperature of the liquid composition and it also allows for shear-mixing of the composition as it flows through. This is preferably achieved by the variable cross-section introducing shear into the mixture.
- the shear-mixing device is a closed gas-tight system. This allows for greater control of the grease properties and it also reduces gas contamination of the lubricant. In addition, it reduces oxidation, which is an important factor if the temperature of the lubricant is increased during processing.
- the liquid composition flows through the shear-mixing device along a flow-path provided with one or more static mixing elements.
- Static mixing elements allow for reproducible mixing. Examples of static mixers are well known in the art and include baffles, mixer bars and other obstructions in the flow-path.
- the liquid composition flows through the shear-mixing device along a flow-path provided with a plurality of static mixing elements arranged to provide regions of increased shear mixing.
- the liquid composition flows through the shear-mixing device along a flow-path provided with one or more temperature-controlled portions to each heat or cool the liquid composition. That is, the shear-mixing device can be provided with a plurality of regions having alternative purposes. Some regions may be used to change the temperature of the lubricant flowing there-through, while others may be used to achieve high or low shear mixing. Regions may, of course, be used for temperature-control and/or shear-mixing.
- At least one temperature-controlled portion is provided at a higher temperature than a preceding temperature-controlled portion along the flow-path. This allows for the heating of the lubricant after, for example, an initial cooling step. This can provide a controllable tempering or annealing step, which cannot be achieved using the conventional casting table approach. It therefore can be used to provide novel lubricants having previously unachievable properties.
- the shear-mixing device comprises one or more pairs of heat-transfer plates between which the liquid composition is flowed, wherein the surface of at least one plate is provided with surface features in the flow path of the liquid composition.
- the pair of plates provides both a means for raising, lowering or maintaining a temperature of the lubricant, while the surface features (on one or both of the pair of plates) can work the grease to shear-mix it.
- the temperature of the heat-transfer plates is controlled with water cooling. This is a cheap and effective way of controlling the temperature.
- the lubricating grease composition can be continuously extruded using the method of the present invention.
- This has numerous advantages for packaging the grease compared to the conventional pouring-and-quenching method. Furthermore, it allows for greater control of the residency time of the grease within the system.
- the shear-mixing is controlled by altering the flow rate of the liquid composition.
- This can be controlled, for example, by varying the gas pressure applied to a reservoir of the substantially homogeneous composition.
- the flow rate may be decreased or stopped during the shear-mixing process, such that alternating dynamic and static quenching may occur.
- the shear rate and shear stress imposed on the grease are varied in the shear-mixing process such that properties of the final grease can be accurately controlled.
- the shear rate is regulated by adjusting flow rate and geometry of the flow channels or flow plates. Especially, by narrowing the distance between plates, the shear rate can be increased to accommodate a higher shear stress and a more severe grease working process.
- the shear stress is controlled by adjusting flow rate and temperature in each zone.
- this will enable grease working of quenched liquids of different rheological properties, in particular quenched liquids that possess a high degree of stiffness.
- the shear rate experienced by the homogeneous liquid during quenching, as well as during grease working, in the shear-mixing conduit, varies from 0 to 107 s -1 .
- the thickening composition forms from shear rate varying from 10 -1 to 10 5 s -1 .
- the thickening composition forms from shear stress varying from 1 to 10 7 Pa.
- one or more additives are added to the liquid composition in the shear-mixing device. These additives can be used to fine-tune the properties of the final grease.
- a small amount e.g. 0.1 - 1.0%) of a co-solvent such as ethanol or water is added to the hot mixture of polymer + base oil.
- the co-solvent is added in order to change the solubility of the polymer in the base oil, and thus influence, e.g. the quenching temperature or thickener structure.
- the process described herein provides for polymer grease synthesis whereby a hot polymer/base oil mixture is pumped through different temperature zones.
- This can be achieved by using a system of, for example, temperature-controlled parallel plates. These may be connected to a reactor resulting in a (semicontinuous, closed synthesis process.
- the polymer/base oil mixture is pumped between the plates by, for example, applying over-pressure in the reactor, resulting in a process of combined cooling and grease working.
- conditions may be varied to adjust the properties of the polymer grease. Adjustment of cooling and grease-working may be achieved by, for example, adjusting one or more of pumping pressure and speed, gap size between the plates, shape and profile of the shape adjusted, and number of temperature zones.
- the process therefore replaces the standard quenching method by combined cooling and grease working in an accurately controlled step.
- This allows grease synthesis with a wider range of properties and higher degree of reproducibility.
- the working of the grease may include shearing, straining, extrusion, rolling, forced flow and/or compression.
- the formation of a grease can occur in several steps.
- the four slides, A - D show the microstructures of the grease during its formation.
- the hot liquid composition or "solution”
- slide B following quenching, there is a liquid-liquid separation.
- slide C there is some solidification as the thickener structure forms. With on-going working of the grease, a more stable structure is formed in slide D.
- Figure 2 shows an example of an apparatus for executing the method of the invention.
- a reservoir is provided for the hot solution comprising the oil and the thickener as a substantially homogeneous liquid composition.
- the reservoir has an outlet in fluid communication with a plurality of pairs of cooling/shearing plates.
- the reservoir is gas-tight and in contact with a source of pressurised gas, by which the solution can be driven through the cooling/shearing plates.
- the apparatus has three pairs of cooling/shearing plates. These each can be used to hold the liquid composition at a different temperature
- the flow-path between pairs of parallel plates allows for working of the liquid composition.
- the internal surface texture of the plates acts as baffles for the flow of the liquid composition, causing shear-mixing.
- Means may be provided to heat and/or cool one or more of the sets of plates. Cooling may be achieved by water-cooling. Heating may be achieved by the uses of electrical heating elements. One set of plates may comprise both cooling means and heating means.
- Figure 4 shows a graph over time of the temperature (degrees Celsius) and the shear (Pa) applied in the formation of the grease in Example 1.
- the liquid composition of the base oil and thickener are held at a high temperature and then cooled step-wise.
- the shear level is controlled so that is peaks during a second quenching step.
- the shear changes stepwise as the composition moves from each set of parallel plates, but the rate of temperature change is more finely controlled, with a fast rate of cooling in the first quenching step and a slower rate at the grease is equilibrated.
- a homogeneous mixture comprising a synthetic hydrocarbon/ester mixture as the base oil and the thickening polymer comprising a propylene polymer or co-polymer having a weight average molecular weight of from 50,000 to 100,000.
- This was passed through a processing unit having the following temperature and shear profile: Step Zone temperature Shear intensity Process step 1 190°C Homogeneous polymer/base oil solution 2 120°C Low shear 1 st Quenching step : generation of thickener structure, determination of fiber size 3 80 °C High shear 2 nd Quenching step : homogenisation of thickener structure 4 25°C Low shear Equilibration
- the final grease had exemplary performance characteristics and was capable of continuous production.
- the process as described herein is capable of improving the controllability of polymer grease synthesis.
- the process can be exploited to investigate the use of new polymers and/or lubricants.
- the use of a closed system allows the process to be applied beyond what is possible with current batch-production and laboratory-scale synthesis.
- Use of polymer types with high melting points means that temperatures for the starting mixture can be higher than temperatures currently used, which tend to be limited to a maximum of about 250°C. This allows for the development of greases with a higher temperature-limit compared to current polymer greases.
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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)
Claims (12)
- Procédé pour la fabrication d'une composition de graisse lubrifiante, le procédé comprenant les étapes suivantes :la fourniture d'une composition liquide comprenant un mélange d'une huile lubrifiante et d'un polymère épaississant, dans lequel le mélange est pratiquement homogène de telle sorte qu'il ne présente pas de domaines de polymères épaississants séparés dans l'huile lubrifiante ou vice versa,l'écoulement de la composition liquide à travers un dispositif de mélange par cisaillement pour mélanger et refroidir la composition liquide afin de former une composition de graisse lubrifiante,dans lequel le polymère épaississant forme de 5 à 20 % en poids de la composition liquide pratiquement homogène,et dans lequel la composition liquide s'écoule à travers le dispositif de mélange par cisaillement le long d'un chemin d'écoulement pourvu d'une ou de plusieurs parties à température contrôlée pour chauffer et/ou refroidir chacune la composition liquide,et dans lequel le dispositif de mélange par cisaillement comprend une ou plusieurs paires de plaques de transfert de chaleur entre lesquelles la composition liquide s'écoule, dans lequel la surface d'au moins une plaque est pourvue d'éléments de surface dans le chemin d'écoulement de la composition liquide qui sont des textures de surface qui font office de chicanes pour l'écoulement de la composition liquide, provoquant un mélange par cisaillement, dans lequel la composition liquide pratiquement homogène est fournie à une température de 150 à 350 °C, de préférence de 200 à 250 °C.
- Procédé selon la revendication 1, dans lequel l'huile lubrifiante comprend des huiles choisies parmi des huiles minérales, des hydrocarbures de synthèse, des huiles d'esters, des huiles végétales et des mélanges de deux ou plusieurs de ceux-ci.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel le polymère épaississant comprend un polymère choisi parmi des polyamides, des polyesters, des oxydes de polyéthylène, du polyéthylène, du polypropylène, des polylactides, de la cellulose ou des dérivés de cellulose, notamment des copolymères de ceux-ci, et des mélanges de deux ou plusieurs de ceux-ci.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel le dispositif de mélange par cisaillement est un conduit de mélange par cisaillement, de préférence ayant une aire en coupe transversale variable.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel le dispositif de mélange par cisaillement est un système fermé étanche aux gaz.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel la composition liquide s'écoule à travers le dispositif de mélange par cisaillement le long d'un chemin d'écoulement pourvu d'un ou de plusieurs éléments de mélange statiques.
- Procédé selon la revendication 6, dans lequel la composition liquide s'écoule à travers le dispositif de mélange par cisaillement le long d'un chemin d'écoulement pourvu d'une pluralité d'éléments de mélange statiques disposés pour fournir des régions de mélange par cisaillement accru.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel au moins une des parties à température contrôlée est à une température plus élevée qu'une partie à température contrôlée précédente le long du chemin d'écoulement.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel la température des plaques de transfert de chaleur est contrôlée avec un refroidissement à l'eau.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel la composition de graisse lubrifiante est extrudée en continu.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel le mélange par cisaillement est contrôlé en modifiant le débit de la composition liquide.
- Procédé selon l'une quelconque des revendications précédentes, dans lequel un ou plusieurs additifs sont ajoutés à la composition liquide dans le dispositif de mélange par cisaillement.
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EP14728889.8A EP3004298B1 (fr) | 2013-05-30 | 2014-05-28 | Procédé de fabrication de polymère-graisse |
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EP2013061143 | 2013-05-30 | ||
PCT/EP2014/061090 WO2014191470A2 (fr) | 2013-05-30 | 2014-05-28 | Procédé de fabrication de polymère-graisse |
EP14728889.8A EP3004298B1 (fr) | 2013-05-30 | 2014-05-28 | Procédé de fabrication de polymère-graisse |
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EP3004298A2 EP3004298A2 (fr) | 2016-04-13 |
EP3004298B1 true EP3004298B1 (fr) | 2022-07-20 |
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