EP0151825B1 - Process for the continuous manufacture of a lubricating grease - Google Patents
Process for the continuous manufacture of a lubricating grease Download PDFInfo
- Publication number
- EP0151825B1 EP0151825B1 EP84201821A EP84201821A EP0151825B1 EP 0151825 B1 EP0151825 B1 EP 0151825B1 EP 84201821 A EP84201821 A EP 84201821A EP 84201821 A EP84201821 A EP 84201821A EP 0151825 B1 EP0151825 B1 EP 0151825B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- process according
- lithium hydroxide
- grease
- monohydrate
- mixers
- 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.)
- Expired
Links
Classifications
-
- 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
- C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
- C10M117/02—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
- C10M117/04—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen containing hydroxy groups
-
- 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
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
-
- 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
Definitions
- This invention relates to a process for the continuous manufacture of a lubricating grease and in particular of a base grease which serves as a basis for the manufacture of a wide variety of lubricating grease formulations containing one or more additives.
- the present invention relates to a process for the continuous manufacture of a lubricating grease comprising blending feed materials and lubricating oil and pumping the resulting blend through at least one motionless mixer which is heated to such a temperature that soap formation takes place and a resultant grease is formed.
- Suitable feed materials are the usual thickening or gelling agents which in the case of soaps are often made in situ in at least part of the lubricating oil from saponifiable material, saponification agents and optionally complexing agents.
- Suitable saponifiable materials are long chain fatty esters, especially glycerides, in particular where the fatty group contains a hydroxy radical, such as ricinoleyl (castor oil) or hydrogenated ricinoleyl (hydrogenated castor oil).
- Another method of soap formation is to neutralize fatty acids or hydroxy fatty acids in mineral oil with alkali metal or alkaline earth metal hydroxides (or mixtures of both) or hydrates thereof - in particular lithium hydroxide monohydrate (LiOH.H 2 0).
- alkali metal or alkaline earth metal hydroxides or mixtures of both
- hydrates thereof in particular lithium hydroxide monohydrate (LiOH.H 2 0).
- hydrogenated fatty acids or hydrogenated hydroxy fatty acids are commonly used in the neutralization.
- Suitable saponification agents are alkali metal or alkaline earth metal hydroxides (or mixtures of both), in particular lithium hydroxide, or hydrates thereof. Therefore, the feed materials preferably comprise
- Suitable complexing agents are short chain fatty acids, such as acetic acid, dicarboxylic acids, such as azelaic acid, hydroxy aromatic acids such as salicyclic acid, boric acid, aluminium compounds, etc. If such complexing agents are used the proportion of saponification agents is usually increased with about the stoichiometric quantity of the complexing agent.
- thickening agents are clays, including coated clays, silica gels, polymers, polyureas, carbon black, dyes, etc.
- Suitable lubricating oils are mineral oils, including hydrogenated mineral oils, synthetic oils, such as ester oils, polyolefin oils, silicon oils, phosphate esters, polyphenyl ethers, etc.
- Suitable mineral lubricating oils include HVI, paraffinic MVI, naphthenic MVI and LVI oils.
- lubricating oil and additives such as antioxidants, antirust, anti-wear and extreme pressure agents, pour point depressants, metal deactivators etc.
- Suitable laboratory-type motionless or static mixers have the form of a cylinder or tube having a length of 65.5 to 66.5 cm and a diameter of 3.3 to 3.6 cm. They are provided with an insulated heating jacket, using e.g. electric tape having a heating capacity of e.g. 400 watt per mixer, or a heating medium as the heating source.
- the inside of the cylinder is provided with e.g. corrugated plates, perforated plates, intermeshing and intersecting bars and similar fixed mechanical obstacles causing mixing and heat exchange.
- a suitable motionless mixer containing perforated plates is described in e.g. GB-A-2086249, but other types may be used as well.
- Suitable mixers are: the Sulzer motionless mixer SMX type which is 655 mm long x 36 mm internal diameter and the Sulzer motionless heat exchanger SMXL type which is 665 mm long x 32.8 mm internal diameter.
- the base grease-making ingredients are preferably blended at room temperature in a container from which they are pumped through at least one motionless mixer, preferably several motionless mixers, preferably longitudinally connected. They may also be, or additionally be, connected in a parallel manner.
- the average velocity of the mixture in the mixers may be 3 kg to 50 kg/h, preferably 7 to 30 kg/h, the flow preferably being laminar.
- the pressure at the entrance of the first mixer may be between 1 and 30 bar, preferably between 1 and 15 bar.
- the mixers are heated to a suitable high temperature, e.g. at least 120°C, preferably between 120 and 250°C, preferably up to a maximum temperature between 180 and 230°C, so that a grease structure is formed on cooling.
- a suitable high temperature e.g. at least 120°C, preferably between 120 and 250°C, preferably up to a maximum temperature between 180 and 230°C, so that a grease structure is formed on cooling.
- a suitable high temperature e.g. at least 120°C, preferably between 120 and 250°C, preferably up to a maximum temperature between 180 and 230°C, so that a grease structure is formed on cooling.
- a suitable high temperature e.g. at least 120°C, preferably between 120 and 250°C, preferably up to a maximum temperature between 180 and 230°C
- Thermocouples may be placed between the mixers for temperature control.
- part of the finished grease may be recycled.
- the pump at the entrance of the first mixer may be provided with a recycling circuit.
- the subsequent removal of water can be accomplished by simply dumping the resulting grease in an open vessel, whereafter any further lubricating oil and any desired additives can be added.
- the base grease together with additional lubricating oil and additives is pumped through a heat exchanger tube for mixing and cooling to obtain the desired consistency.
- Homogenisation of the grease if necessary, is carried out using e.g. a Manton Gaulin homogeniser at 3000 psig (20.7 MPa), a mill or a rolling device etc.
- the finished grease is obtained at the outlet and cooled in a jacketed SULZER MONOTUBE HEAT EXCHANGER which consists of 2 units each 1540 mm long x 32.8 mm internal diameter. Each unit contains 1 SMXL type heat exchanger.
- the unworked/worked penetration at 25°C was 262/273 dmm (ASTM D217-82). (1 dmm corresponds with 0.1 mm) and the dropping point was 197°C. (Worked penetration is the penetration at 25°C after 60 double strokes in a standard grease worker).
- the first two Sulzer mixers were of the type SMX DN32, having a length of 655 mm and an internal diameter of 36 mm and the last two were of the type SMXL DN32 (heat exchanger type for boosting the heat transfer during warming up of the viscous mixture), having a length of 665 mm and an internal diameter of 32.8 mm.
- Examples 2-6 are carried out in the arrangement of Example 1, but the flow rate is changed, resulting in different outlet temperatures, penetrations and dropping points (see Table A).
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Description
- This invention relates to a process for the continuous manufacture of a lubricating grease and in particular of a base grease which serves as a basis for the manufacture of a wide variety of lubricating grease formulations containing one or more additives. By first making a base grease a great flexibility is obtained in making a great variety of grease formulations using the same grease manufacturing basic unit.
- From European patent application 0072184 a process for the continuous manufacture of a lubricating grease, which process shows a great flexibility, is already known. According to this process a rotating screw process unit is used.
- It has now been found that such processes, which enable the manufacture of a great variety of greases, such as the greases described in said European patent application, can be carried out in a simpler way without the use of moving parts, namely by using motionless mixers, which are readily commercially available.
- Therefore the present invention relates to a process for the continuous manufacture of a lubricating grease comprising blending feed materials and lubricating oil and pumping the resulting blend through at least one motionless mixer which is heated to such a temperature that soap formation takes place and a resultant grease is formed.
- Suitable feed materials are the usual thickening or gelling agents which in the case of soaps are often made in situ in at least part of the lubricating oil from saponifiable material, saponification agents and optionally complexing agents.
- Suitable saponifiable materials are long chain fatty esters, especially glycerides, in particular where the fatty group contains a hydroxy radical, such as ricinoleyl (castor oil) or hydrogenated ricinoleyl (hydrogenated castor oil).
- Another method of soap formation is to neutralize fatty acids or hydroxy fatty acids in mineral oil with alkali metal or alkaline earth metal hydroxides (or mixtures of both) or hydrates thereof - in particular lithium hydroxide monohydrate (LiOH.H20). Alternatively hydrogenated fatty acids or hydrogenated hydroxy fatty acids are commonly used in the neutralization.
- Suitable saponification agents are alkali metal or alkaline earth metal hydroxides (or mixtures of both), in particular lithium hydroxide, or hydrates thereof. Therefore, the feed materials preferably comprise
- a) hydrogenated castor oil (HCO) and lithium hydroxide or lithium hydroxide monohydrate;
- b) HCO and lithium hydroxide (or monohydrate) or calcium hydroxide;
- c) Hydrogenated castor oil -fatty acid (HCOFA) and lithium hydroxide or lithium hydroxide monohydrate; and/or
- d) HCOFA and lithium hydroxide (or monohydrate) or calcium hydroxide.
- Suitable complexing agents are short chain fatty acids, such as acetic acid, dicarboxylic acids, such as azelaic acid, hydroxy aromatic acids such as salicyclic acid, boric acid, aluminium compounds, etc. If such complexing agents are used the proportion of saponification agents is usually increased with about the stoichiometric quantity of the complexing agent.
- Other suitable thickening agents are clays, including coated clays, silica gels, polymers, polyureas, carbon black, dyes, etc.
- Suitable lubricating oils are mineral oils, including hydrogenated mineral oils, synthetic oils, such as ester oils, polyolefin oils, silicon oils, phosphate esters, polyphenyl ethers, etc. Suitable mineral lubricating oils include HVI, paraffinic MVI, naphthenic MVI and LVI oils.
- To the base greases may be added additional lubricating oil and additives, such as antioxidants, antirust, anti-wear and extreme pressure agents, pour point depressants, metal deactivators etc.
- Suitable laboratory-type motionless or static mixers have the form of a cylinder or tube having a length of 65.5 to 66.5 cm and a diameter of 3.3 to 3.6 cm. They are provided with an insulated heating jacket, using e.g. electric tape having a heating capacity of e.g. 400 watt per mixer, or a heating medium as the heating source. The inside of the cylinder is provided with e.g. corrugated plates, perforated plates, intermeshing and intersecting bars and similar fixed mechanical obstacles causing mixing and heat exchange. A suitable motionless mixer containing perforated plates is described in e.g. GB-A-2086249, but other types may be used as well.
- Suitable mixers are: the Sulzer motionless mixer SMX type which is 655 mm long x 36 mm internal diameter and the Sulzer motionless heat exchanger SMXL type which is 665 mm long x 32.8 mm internal diameter.
- For commercial production the sizes of the mixers require scaling up.
- According to the present process the base grease-making ingredients are preferably blended at room temperature in a container from which they are pumped through at least one motionless mixer, preferably several motionless mixers, preferably longitudinally connected. They may also be, or additionally be, connected in a parallel manner.
- The average velocity of the mixture in the mixers may be 3 kg to 50 kg/h, preferably 7 to 30 kg/h, the flow preferably being laminar.
- The pressure at the entrance of the first mixer may be between 1 and 30 bar, preferably between 1 and 15 bar.
- The mixers are heated to a suitable high temperature, e.g. at least 120°C, preferably between 120 and 250°C, preferably up to a maximum temperature between 180 and 230°C, so that a grease structure is formed on cooling. Preferably the temperature of each of the heated mixers is higher than that of the preceding mixer and so on.
- Thermocouples may be placed between the mixers for temperature control.
- If desired part of the finished grease may be recycled. Also the pump at the entrance of the first mixer may be provided with a recycling circuit.
- The subsequent removal of water can be accomplished by simply dumping the resulting grease in an open vessel, whereafter any further lubricating oil and any desired additives can be added.
- Due to condensation some water may be present in the open vessel. If required complete dehydration may be accomplished using conventional flash vacuum equipment.
- Preferably the base grease together with additional lubricating oil and additives is pumped through a heat exchanger tube for mixing and cooling to obtain the desired consistency.
- Homogenisation of the grease, if necessary, is carried out using e.g. a Manton Gaulin homogeniser at 3000 psig (20.7 MPa), a mill or a rolling device etc.
- The invention is illustrated by the following Examples.
- 1.3 kg feed containing: 12 %w hydrogenated castor oil, 1.7 %w LiOH.H20, 86.3 %w mineral lubricating oil (HVI, viscosity 10.7-11.8 cSt at 100°C, VI = 96 (min), and 3 %2 (= 39 g) water is mixed at room temperature for at least 10 minutes in a container and then pumped at a flow rate of 8.3 kg/h once through a series of 4 Sulzer motionless mixers (each unit containing 2 mixing elements) which are beforehand adjusted to temperatures of 130,170,190 and 230°C, respectively, by 4 200 watt electric heaters per mixer.
- The finished grease is obtained at the outlet and cooled in a jacketed SULZER MONOTUBE HEAT EXCHANGER which consists of 2 units each 1540 mm long x 32.8 mm internal diameter. Each unit contains 1 SMXL type heat exchanger. The unworked/worked penetration at 25°C was 262/273 dmm (ASTM D217-82). (1 dmm corresponds with 0.1 mm) and the dropping point was 197°C. (Worked penetration is the penetration at 25°C after 60 double strokes in a standard grease worker).
- The first two Sulzer mixers were of the type SMX DN32, having a length of 655 mm and an internal diameter of 36 mm and the last two were of the type SMXL DN32 (heat exchanger type for boosting the heat transfer during warming up of the viscous mixture), having a length of 665 mm and an internal diameter of 32.8 mm.
- Subsequently the water present in the grease was flashed off.
-
Claims (8)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB8400073 | 1984-01-04 | ||
GB848400073A GB8400073D0 (en) | 1984-01-04 | 1984-01-04 | Lubricating grease |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0151825A2 EP0151825A2 (en) | 1985-08-21 |
EP0151825A3 EP0151825A3 (en) | 1987-05-20 |
EP0151825B1 true EP0151825B1 (en) | 1989-11-02 |
Family
ID=10554517
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP84201821A Expired EP0151825B1 (en) | 1984-01-04 | 1984-12-10 | Process for the continuous manufacture of a lubricating grease |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP0151825B1 (en) |
JP (1) | JPS60192798A (en) |
AU (1) | AU571628B2 (en) |
BR (1) | BR8500001A (en) |
DE (1) | DE3480349D1 (en) |
GB (1) | GB8400073D0 (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6214778B1 (en) | 1995-08-24 | 2001-04-10 | The Lubrizol Corporation | Polyurea-thickened grease composition |
KR100240821B1 (en) * | 1997-12-23 | 2000-01-15 | 허동수 | Process for preparation of grease and filter of the same |
US7829512B2 (en) | 2003-10-17 | 2010-11-09 | Exxonmobil Research And Engineering Company | Method and equipment for making a complex lithium grease |
EP2591080B1 (en) * | 2010-07-05 | 2014-11-26 | Shell Internationale Research Maatschappij B.V. | Process for the manufacture of a grease composition |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB579847A (en) * | 1942-07-31 | 1946-08-19 | Standard Oil Dev Co | An improved manufacture of lubricating greases and apparatus therefor |
GB1508281A (en) * | 1977-02-11 | 1978-04-19 | Exxon Research Engineering Co | Lubricating greases |
DE2927686A1 (en) * | 1979-07-09 | 1981-02-05 | Henkel Kgaa | NEW LITHIUM SOAPS AND THEIR USE AS A THICKENING AGENT IN LUBRICANTS OR. GREASES |
JPS602899B2 (en) * | 1980-10-13 | 1985-01-24 | 三井東圧化学株式会社 | mixing device |
US4392967A (en) * | 1981-08-11 | 1983-07-12 | Exxon Research And Engineering Co. | Process for continuously manufacturing lubricating grease |
DD210299A5 (en) * | 1982-07-05 | 1984-06-06 | Mta Mueszaki Kemiai Kutato Int | METHOD AND DEVICE FOR CONTINUOUS MANUFACTURE OF LUBRICANT |
-
1984
- 1984-01-04 GB GB848400073A patent/GB8400073D0/en active Pending
- 1984-12-10 EP EP84201821A patent/EP0151825B1/en not_active Expired
- 1984-12-10 DE DE8484201821T patent/DE3480349D1/en not_active Expired
- 1984-12-28 JP JP59281841A patent/JPS60192798A/en active Pending
-
1985
- 1985-01-02 BR BR8500001A patent/BR8500001A/en not_active IP Right Cessation
- 1985-01-02 AU AU37255/85A patent/AU571628B2/en not_active Ceased
Also Published As
Publication number | Publication date |
---|---|
EP0151825A2 (en) | 1985-08-21 |
EP0151825A3 (en) | 1987-05-20 |
AU3725585A (en) | 1985-07-18 |
DE3480349D1 (en) | 1989-12-07 |
GB8400073D0 (en) | 1984-02-08 |
BR8500001A (en) | 1985-08-13 |
JPS60192798A (en) | 1985-10-01 |
AU571628B2 (en) | 1988-04-21 |
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