US2298317A - Manufacture of lubricating greases - Google Patents

Manufacture of lubricating greases Download PDF

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Publication number
US2298317A
US2298317A US354435A US35443540A US2298317A US 2298317 A US2298317 A US 2298317A US 354435 A US354435 A US 354435A US 35443540 A US35443540 A US 35443540A US 2298317 A US2298317 A US 2298317A
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Prior art keywords
grease
kettle
agitator
vacuum
oil
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US354435A
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English (en)
Inventor
Herschel G Smith
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Gulf Oil Corp
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Gulf Oil Corp
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Priority to NL142820D priority Critical patent/NL142820C/xx
Application filed by Gulf Oil Corp filed Critical Gulf Oil Corp
Priority to US354435A priority patent/US2298317A/en
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Publication of US2298317A publication Critical patent/US2298317A/en
Priority to US503152A priority patent/US2367149A/en
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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
    • C10M177/00Special 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/0042Degasification of liquids modifying the liquid flow
    • B01D19/0052Degasification of liquids modifying the liquid flow in rotating vessels, vessels containing movable parts or in which centrifugal movement is caused
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/84Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with two or more stirrers rotating at different speeds or in opposite directions about the same axis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F35/92Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1868Stationary reactors having moving elements inside resulting in a loop-type movement
    • B01J19/1875Stationary reactors having moving elements inside resulting in a loop-type movement internally, i.e. the mixture circulating inside the vessel such that the upwards stream is separated physically from the downwards stream(s)
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/20Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05Stirrers
    • B01F27/09Stirrers characterised by the mounting of the stirrers with respect to the receptacle
    • B01F27/091Stirrers characterised by the mounting of the stirrers with respect to the receptacle with elements co-operating with receptacle wall or bottom, e.g. for scraping the receptacle wall
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05Stirrers
    • B01F27/11Stirrers characterised by the configuration of the stirrers
    • B01F27/15Stirrers with tubes for guiding the material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • B01J2219/00063Temperature measurement of the reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/0009Coils
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/0015Controlling the temperature by thermal insulation means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00245Avoiding undesirable reactions or side-effects
    • B01J2219/00252Formation of deposits other than coke
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02Water
    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/021Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
    • CCHEMISTRY; METALLURGY
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/281Esters of (cyclo)aliphatic monocarboxylic acids
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    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/282Esters of (cyclo)aliphatic oolycarboxylic acids
    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
    • 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/286Esters of polymerised unsaturated acids
    • 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
    • C10M2215/064Di- and triaryl amines
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C10M2219/104Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
    • C10M2219/108Phenothiazine
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • 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
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/02Groups 1 or 11
    • 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
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/04Groups 2 or 12
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/06Groups 3 or 13
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/08Groups 4 or 14
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy
    • CCHEMISTRY; METALLURGY
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    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00Specific manufacturing methods for lubricant compositions

Definitions

  • This invention relates to manufacture of lubrieating greases; and it comprises an improved method of manufacturing lubricating greases of the soap and oil type, in which'the grease constituents are subjected to agitation under vacuum during one or more of the stages of compounding, blending, extending, finishing and drawing the grease, said agitation advantageously being so accomplished that a positive upward axial flow is maintained in a relatively tall, narrow body of grease constituents with a positive downward flow at the periphery of said body and with both flows being disturbed and having a helical component, thus circulating the grease constituents with turbulent flow in a helical path and with the core and peripheral portion thereof flowing in opposite directions while in direct contact at 'their interface; and it also comprises apparatus in which this agitation under vacuum maybe readily effected and in which other steps in the manufacture of lubricating greases may also be effected conveniently and economically, said apparatus advantageously comprising a -relatively' more individual chemical. compounds.
  • Sources of fatty acids suitable for grease manufacture include hard tallow, t'allow oil, stearin, cottonseed oil, fish oil, corn oil, palm oil and various hydrogenated fats.
  • This invention is applicable to the manufactureof many types of greases, including hard greases of high soap content and smooth consistency, such as locomotive driving journal compounds, and also including substantially all types of cup greases, fiber greases and special greases, including universal joint lubricants, wheel bearing greases, brake cylinder compounds, etc.
  • the steps in the complete manufacturing procedure may vary somewhat; but in all cases, there is included the step of agitating under vacuum during one of the later stages of manufacture. This step is one of the features of the improved manufacturing procedure which constitutes a part of this invention.
  • an agitating device which advantageously includes a coaxial pair of conveyors rotating in opposite directions.
  • a bladed conveyor positioned adjacent the casing wall'with as little clearance as may be, and thus capable of producing powerful shearing stresses when rotated.
  • Cooperating with this element and adapted to provide return circulation is an axial agitator and conveyor; and for this element I to be especially advantageous.
  • Elements car- .ried by the two conveyors extend radially, and
  • Fig. l is a vertical sectional view of a vertical columnar type kettle
  • Fig. 2 is a cross sectional view of the kettle, taken on line 22 of Fig. 1;
  • Fig. 3 is an enlarged fragmentary view of a scraper blade, taken on line 3-3 of Fig. 1;
  • Fig. 4 is an enlarged fragmentary view of another portion of the agitator, taken on line 4-4 of Fig. 1;
  • Fig. 5 is a view in elevation of the grease kettle assembled with one form of auxi1iary equipment, including a motor and a separately enclosed gearing for rotating the agitators;
  • Fig. 6 is an enlarged vertical section of the en-. closed gearing shown in Fig. 5;
  • Fig. 7 is a sectional view of another type of I,
  • the kettle is fabricated in any suitable way as by welding.
  • the interior height is advantageously great compared to the diameter, as shown; at least about .1.5 times as great and often 3 or 4 times as great
  • the kettle is conveniently supported on pillars It, by means of lugs l8, as shown.
  • An inlet connection II at the top servesfor introduction of liquid grease ingredients, and means for removal or drainage of the kettle contents is provided by a valved outlet ll at the bottom.
  • the movable part of the valve l8 advantageously includes a plug I! which, in closed position, becomes flush with the interior ofthe kettle bottom as shown, to prevent pocketing.
  • a connection 20 with suitable exhausting means permits the interior of the kettle to be put under vacuum when desired; and a manhole 22 permits introduction of solids and inspection.
  • of compact type is perature measurement. Heating means are profind a particular type of helical ribbon convey r vided for the kettle, conveniently inthe form oi steam coils 2i surrounding the kettle for a ma or .j portion of its length, and advantageously ,nne, welded thereto.
  • a double agitator-mixer assemblage within the kettle is a double agitator-mixer assemblage.
  • This includes a helical agitator of the conveyor type having 'an' axle 21, advantageously of tubular construction, on which is mounted a helical ribbon 28 by means of struts 9.
  • this inner 'helical agitator terminates with a stub shaft 30, seated for rotation in a thrust bearing 3
  • an outer, coaxial, independently rotated agitator or conveyor includ ing a frame 33 closely spaced from the ribbon 28 and having attached thereto a plurality of staggered and inclined paddle blades 34. At their ends, these blades carry flexible metal scraper elements 35 arranged to scrape the kettle walls (Figs. 2, 3 and ,4) and clamped to the blade ends as shown at 36, for example.
  • a bottom-scraping blade 31 is attached to frame 33, and is shaped to conform to the kettle bottom, as shown. It is advantageously cut out, as shown'at 38, to clear the thermocouple 2
  • the interior of the kettle is smooth and accurately cylindrical, so that grease is continually removed from the walls and bottom by the scrapers without leaving any dead pockets or dead films.
  • the annular zones of the kettle walls traversed by scrapers 35 slightly overlap, so that all parts of the wall are subjected to scraping action; there are no dead annular spaces untouched by the scrapers.
  • the bottom of frame 33 is provided with a bearing collar 39 surrounding the stub shaft 30 above the kettle by a support 41 receives the ends Shaft 32 is seated in an I of shafts 32 and 4
  • is seated in a lower bearing 49, sealed at 50 to prevent leakage of lubricant (not shown) from the housing.
  • Shaft 32 .carries a gear meshing with a gear 52 on a jack-shaft 53, and shaft 4
  • the sprocket is driven from a sprocket 56 on the jack-shaft 53 1 by a chain 51.
  • the jack-shaft extends through the top of the housing and is driven by a geared speed-reduction motor 58 through a coupling 59. Shafts 32 and 4
  • and 52, and of sprockets 54 and 56, are so selected that the inner helical agitator 28 is driven at a somewhat higher an gular speed than the outer agitator blades 34. These ratios are so selected that the quantity of material in the kettle moved downward a given distance by the outer agitator during a given period is about equal to the quantity moved upward by the inner agitator during the same period.
  • the gearing in box is shown as speedincreasing gearing, but speed-reduction gearing can be provided instead, depending on the speed of the motor 58.
  • Fig. 7 shows another driving mechan sm for the compound agitators, which has the advantage of rendering the interior of the kettle readily accessible by simply removing the cover.
  • both terminate within the kettle, at a point below joint l3.
  • the inner driveshaft 32 is supported by a bearing 60, advantaadjacent the walls of the kettle.
  • the tall and relatively narrow kettle maintains the charge or grease mixture in the form of a tall column during the compounding, blending and finishing operations.
  • a greater amount of grease is maintained in contact with the kettle shell; and this facilitates temperature control.
  • a lesser amount of grease is exposed at the top of the kettle and this minimizes oxidationwhen air is present above the grease.
  • the charging arrangement shown in the drawing is also convenient, since all materials can be delivered to the kettle and the kettle operation can be completely controlled from a charging platform (not shown) near the top of the kettle.
  • The-feed pipe or inlet IT conveniently serves to deliver all of the liquid grease constituents to the kettle; these including mineral oils, fatty oils, molten fatty acids, aqueous solutions of alkali, etc., which may be admixed prior-to charging or may be introduced separately. If
  • inlets in the kettle should generally be held to a minimum as this facilitates'the maintenance of the kettle in a gas-tight condition during vacuum operation.
  • the vacuum connection 23 mav also be used for controlling pressure during stages when the kettle is operated under superatmospherie conditions; during saponification, for example.
  • a branch of this pipe may be employed for venting the kettle, as by means of a pressure release valve; and the same or another branch maybe connected to a'source of compressed gas.
  • a pressure gage may also be connected to this line.
  • the single connection may be. used to control all pressures during the various operations, by means of suitable connections and valves.
  • the compound agitator illustrated in the drawing is highly eflicient and the concentric rotation of the agitators in opposite direction produces a double motion agitation which is most efiicient in producing grease having a uniform gel structure.
  • agitation of this type the grease mixture is maintained in turbulent flow with a major flow upwardly at the .center of the kettle and a major flow dovmwardly around the upwardly moving core of grease and
  • both major flows have a superimposed spiral component.
  • This highly disturbed flew. in ad.- dition to producing uniform blending gives better control of the temperatures of the grease. Rapid heat exchange with relatively quick heating and cooling are obtained, without local overheating or chilling.
  • the design of the inner helical agitator conveyor is important.
  • the relatively narrow spiral ribbon of this element picksup the grease at the bottom of the kettle and lifts it upwardly to the top of the body of grease mixture, where it flows radially to join the outer downwardly flowing grease.
  • Some of this upwardly flowing central core of grease is also forced outwardly toward the walls while thoroughly agitating it.
  • the vanes are set at a substantial angle to the plane of rotation, with the result that the grease is forced downwardlyin a continuous spiral path adjacent the walls of the kettle.
  • the rigid bottom scraping blade 31 When the grease reaches the bottom of the kettle it is forced along the curved bottom by the rigid bottom scraping blade 31 until it is picked up by the inner spiral agitator as described.
  • the kettle In operation, the kettle is charged with grease ingredients up to a suitable level, which may be substantially below the joint 13.
  • the temperature of the charge is brought to the desired point, usually with thorough agitation in the manner described and with at least a substantial part of the agitation effected under vacuum.
  • Example 1 a hard type of sodium soap grease, useful as a locomotive driving journal compound, was prepared. For each 100 parts of finished grease to be made, the kettle was initially charged with 9 parts of a previous batch of the grease and 7 parts of-caustic soda dissolved in 9.8 parts of water. The mixture in the kettle was thoroughly stirred and superheated steam at a tempera ture of 500 to 700 F. was passed through the heating coil. To this initial charge there was added a mixture of 42.5 parts of fatty acid and 47.8 parts of lubricating oil stock, which had been pre-heated to a temperature of 175 F. to melt the fatty acid and dissolve it'in the lubricating oil. The lubricating oil stock employed was a mixture of 85 per cent of cylinder stock and 15 per cent of a wax discharge from solvent treated Mid-Continent oil. The properties of the mixture were as follows:
  • dome-like cover I 2 This provides a substantial space or "gas cushion above the charge, and also serves to prevent or minimize difliculties due to frothing of the charge.
  • the fatty acid used in this case was a, highmelting point product produced by the hydrogenation of a fish oil, followed by splitting the glyceride and recovering the fatty acid.
  • This fatty acid had the following properties:
  • the grease was then drawn from the kettle through a IO-mesh screen into molds, applying low air'pressure to expedite the flow, with care that no air was included in the flowing grease, The grease was allowed to cool in the molds for about thirty hours, until it would form a smooth firm cheese" when pressed and cut. The grease was then pressed hard (applying a total pressure of at least twenty tons) and removed from the molds, cut and wrapped.
  • the composition of this grease was as follows:
  • Lubricating oil stock Sodium soap of a fatty acid 46. 7 Water by distillation Trace Free NaOH 0. 8
  • Example 2 In another embodiment of my invention, the grease produced was of a semifibrous type and relatively soft consistency, useful as a universal joint lubricant.
  • the final composition of this grease was approximately as follows:
  • the Texas lubricating oil used in this grease was an acid treated oil of 750 viscosity S. U. V.
  • the tallow employed in this grease as a constituent of the soap was edible beef tallow?
  • the stearic acid was the single pressed grade.
  • the properties of these constituents were:
  • the mixture was heated to a temperature between 150 and 175 F., and 1.7 parts NaOH dissolved the mixture was heated to 255 F. in two hours, with thorough agitation. superheated steam v was then applied while the temperature of the soap concentrate was raised to. 375 F. in two hours. The soap concentrate was then cooled at 300 F. in about 1.25 hours, with saturated steam in the coils.
  • the Mid-Continent lubricating oil was 75 were ,then added in about 1.25 hours, thus reducing the soap content of the batch to about 35 per cent and cooling the grease to about 200 F.
  • a vacuum of 20 inches of mercury was then applied to the grease, and was maintained while the-grease was finished by thoroughly working in 68 parts of Mid-Continent lubricating oil preheated to F. and the small amount (0.002 part) of oil of cassia. During this stage, the grease cooled to a temperature of about F. in three hours. The agitators were then stopped, the vacuum was relieved, and the grease was drawn slowly into drums to-avoid trapping air in the grease.
  • This grease had the following properties:
  • Example 3 In a further embodiment of my invention, a grease having a mixed calcium and sodium soap base, and of a type useful as a wheel-bearing lubricant, was prepared.
  • composition of the final grease was approxi- 10 mately as follows:
  • Example 4 A calcium-tallow soap grease, useful as a cup grease, was also prepared in accordance with my invention.
  • the composition of the finished grease was approximately as follows:
  • the lubricating oil used in this grease was a Texas oil of 305 viscosity at F., having the following properties:
  • the tallow used in this grease had the following properties:
  • the procedure in this case involved forming the soap concentrate under pressure and finishing under vacuum; that is, maintaining a vacuum while adjusting the water content and blending the soap concentrate with oil.
  • the initial charge to' the kettle was 18.6 parts of tallow and 37.2
  • the soap was formed in substantially an equal weight of oil under pressures up to 55 pounds per square inch during a period of 1 to 2 hours. The soap concentrate was then expelled or expanded into the second kettle, open to the atmosphere, and
  • greases of the type know'n as boiled calcium greases can be prepared without boiling, and with relatively low soap contents coupled with improved stability and uniformity, in accordance with this invention.
  • Example 5 In another embodiment of my invention, a calcium-tallow soap was employed with flake graphite and phenthiazine to produce a grease useful as an' air-brake cylinder compound. The final composition of this grease was as follows: 0 v
  • the lubricating oil in this grease was a blend of 14.3 per cent of Mid-Continent neutral oil having a viscosity of 100 at 100 F. with 85.7 per cent of solvent treated Texas oil having a hours.
  • the tallow employed in this grease had the following properties:
  • This grease was manufactured by pressure saponification in part of the oil, followed by at-' mospheric evaporation of most of the excess water, and addition of the finishing oil at atmospheric pressure with final adjustment of the water content under vacuum.
  • the initial charge to the kettle was 15.17 parts tallow, 30.34
  • the blended oil had The pressure was then released by bleed- In a modification of this procedure, saponification in a substantially equal weight of oil was effected under pressures of to 55 pounds per square inch, which required one to two hours.
  • the soap was drawn from the pressure kettle into an open mixer maintained at about 250 to 300 F., so that excess water was flashed off almost instantly, in the form of steam, during the transfer.
  • the water content was adjusted by further heating and the finishing oil and graphite were then worked in under vacuum, as previously described.
  • My invention is not limited to the specific prov cedures described in the above examples, but these examples illustrate some typical instances in grease manufacture in which thorough agitation under vacuum, usually with maintenance of a controlled range of temperatures, is a highly advantageous expedient, especially in finishing the grease. Numerous other procedures involving this step are within the scope of this invention.
  • any kettle provided with adequate means for agitating, evacuating, and controlling temperature may be employed.
  • these conditions and requirement are advantageously met by establishing and maintaining a tall narrow cylindrical charge of grease (or grease constituents) in a hot walled vessel or kettle, the diameter of the kettle being rather small in proportion to its height.
  • the complete charge in the-kettle has a height or depth which is several times as great as its diameter; at least 1.5 times as great.
  • this charge of grease I establish circulation or movement in opposite directions by means of compound agitators.
  • the improved process of manufacturing lubricating grease free from occluded gases which comprises establishing a vertically elongated charge of grease constituents including a soap and a lubricating oil, applying heat peripherally to said charge, thoroughly agitating said charge to blend the said constituents, and maintaining the charge under a substantial vacuum during the agitation thereof, the vacuum being suflicient to prevent the trapping and occluding of gases And this eificient and the thorough agitation comprising a positive downward, turbulent flow of the peripheral 'portion of the charge, the peripherally heated material being continuously admixed with the downwardly flowing peripheral portion by such turbulent flow, and a positive upward, turbulent flow of the core of said charge, the said upward and downward flows being in direct, contact at their;
  • said agitating means including an inner helical ribbon agitator and a concentric outer paddle agitator'provide'd with scrappers posi-.
  • Apparatus for manufacturing lubricating grease comprising in combination a vertically elongated kettle, means for applying heat peripherally to said kettle, an agitator mounted within said kettle, a pressure-tight closure for the top of the kettle, means for maintaining a vacuum within the kettle when closed, means for operating said agitator with the kettle maintained under vacuum, means for withdrawing contents from the bottom of the kettle, and means for charging the kettle through the said closure, said agitator being a compound agitator comprising an inner helicoid ribbon adapted to impart an upward flow to the central portion of the contents of the kettle and an external agitator having a plurality of vanes adapted to impart a downward flow to the peripheral portion of the said contents, said vanes being provided with terminal scrapers adapted to free the walls of the kettle from adhering deposits.
  • a compound agitator comprising an inner helicoid ribbon adapted to impart an upward flow tothe central portion of the contents of the kettle and an external agitator having a plurality of vanes adapted to impart a downflow to the peripheral portion of said contents, the said vanes being provided with terminal'scrapers adapted to free the walls of the kettle from adhering deposits.
  • homogeneous lubricating greases having a uniform gel structure
  • the improvement which comprises continuously circulating a grease mixture containing a soap and lubricating oil, while maintaining said mixture in the form of a vertically elongated, cylindrical column,'by flowing the core and peripheral portion of said mixture in opposite directions with the core and peripheral portion in direct contact to produce turbulent flow at their interface, the core having a positive upfiow and the peripheral portion having a positive downflow and both flows having a helical component and being turbulent, such 6.
  • the improved process of claim 5 wherein the grease mixture is peripherally heated and the heated portion is continuously intermixed with the downfiowing peripheral portion and this admixture is recycled, the said circulation being continued until the grease mixture is brought to a substantially uniform temperature throughout saitc:I column by said turbulent flow in a helical pa 7.
  • the improved process of claim 5 wherein the grease is peripherallycooled and the cooled portion is continuously intermixed with the downflowing peripheral portion and this admixture is recycled, the said circulation 'being continued until the grease is brought to a substantially uniform temperature throughout said column by such turbulent flow in a helical path.
  • the improvement which comprises thoroughly agitating the grease mixture under vacuum during at least one of the said operations, the agitated grease mixture beingcontinuously circulated and exposed to .a vacuum equivalent to a subatmospheric pressure of at least five inches of mercury below atmospheric pressure and the agitation and vacuum being so adjusted relative to each other as to produce a final grease substantially free of occluded gas and vapors.
  • An improved apparatus for manufacturing stable homogeneous lubricating greases comprise ing a vertically elongated kettle, a pressure-tight closure for the top of the kettle, means for charging the kettle, means for' maintaining a vacuum within the kettle when closed, an agitator mounted within said kettle and means for operating said agitator with the kettle maintained under vacuum, said agitator being a compound agitator comprising an inner helicoid ribbon and an external agitator having scrapers contacting the inner walls-of the kettle, said inner and outer agitators being concentric and capable of rotatmg in opposite directions to cause a positive upward flow of the central portion and a positive downflow of the peripheral portion of the con-' tents of the kettle, with the said upward and downward flows in direct contact at their interface, and means for withdrawing the grease from the bottom of the kettle.
  • an improved compound agitator comprising an outer agitator and an inner agitator mounted concentrically about a common vertical axis and capable of being rotated in opposite directions about said common axis and means for so rotating said outer and inner agitators in opposite directions, the outer agitator being a paddle agitator comprising a rectangular frame and having a plurality of inclined paddles circulation being continued until a grease having 7 a uniform gel structure is obtained.
  • a helicoidal agitator comprising a helicoid ribbon mounted on and spaced from a rotatable shaft
  • the said helicoidal agitator being rotatably mounted within said frame.
  • an improved compound agitator comprising an inner helical ribbon agitator and a concentric outer paddle agitator provided with outer end thereof. and the inner agitator being prising a helicoid ribbon mounted on and spaced from a rotatable shaft and said outer agitator comprising a plurality of inclined vanes mounted on opposite sides of an agitator frame in staggered arrangement and extending outwardly from said frame, said frame being rotatably mounted on the shaft of said inner agitator and surrounding said inner helicoid ribbon, the vanes of said outer agitator being so inclined as to force the peripheral portion. of the grease downward when the outer agitator is rotated.
  • a compound agitator comprising an inner helical ribbon agitator and a concentric outer paddle agitator provided with scrapers positioned to contact the said inner surface of the kettle, said inner and outer agitators being concentrically mounted in the kettle and being capavble of rotating in opposite directions, the paddles of said outer agitator being so inclined as to force the peripheral portion of the grease downward when the agitator is rotated in the kettle.
  • An improved apparatus for manufacturing lubricating grease comprising in combination a vertically elongated kettle, means for applying heat peripherally to said kettle, an agitator mounted within said kettle, a pressure-tight closure for the top of the kettle, means for maintaining a vacuum within the kettle when closed, means for operating said agitator with the kettle maintained under vacuum, means for withdrawing the contents from the bottom of the kettle,
  • said agitator being a compound agitator comprising an inner element and an outer element adapted to cause a positive upfiow of the central portion of the contents of the kettle and a positive downfiow of the peripheral portions of said contents with the said upward flow and downward flow in direct contact at their interface
  • the said outer element being a paddle agitator carrying scrapers adapted to free the walls of the kettle from adhering deposits
  • said inner element being a helicoid ribbon agitator
  • said inner and outer elements being centrally mounted within the kettle on concentric shafts driven by a single power source external to the kettle.
  • lubricating grease which comprises establishing and maintaining a vertically elongated charge of grease constituents including a soap and a lubricating oil, agitating said charge by continuously raising the core thereof to the top of the charge and causing a positive downward flow of the peripheral portionof-the charge around said core, and maintainingthe charge under a substantial vacuum during said agitation,'the said downflow being in direct contact with said core, producing turbulent flow and intermixing at the interface of said core and peripheral portion, and said vacuum being sufficient to prevent trapping and occluding of air during such agitation and flow.
  • the improvement which comprises agitating a grease mixture including a lubricating oil and a soap in a kettle closed to the atmos phere under a vacuum suflicient to prevent the trapping and occluding of gases and vapors during the agitation, the agitated grease mixture being continuously circulated and exposed to a .justed relative to each other as to produce a grease having a uniform continuous'gel structure .free from occluded air and other undesirable gases and'vapors.

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  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • Lubricants (AREA)
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Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2417495A (en) * 1943-12-10 1947-03-18 Girdler Corp Manufacture of grease
US2483282A (en) * 1945-09-15 1949-09-27 Girdler Corp Art of grease manufacture
US2567412A (en) * 1947-05-17 1951-09-11 Mcgraw Electric Co Transformer and method of impregnation
US2610042A (en) * 1946-10-11 1952-09-09 Dryon Paul Apparatus for working pastes
US2890039A (en) * 1953-11-02 1959-06-09 Karl Schmidt Metallschmelzwerk Apparatus for the introduction of substances into liquids of high specific gravity
US2908652A (en) * 1955-08-15 1959-10-13 Forrester Gilbert Process and apparatus for defoaming liquids
US3439836A (en) * 1967-01-27 1969-04-22 Ronald J Ricciardi Apparatus for conditioning and dispensing particulated material
US3475337A (en) * 1967-05-29 1969-10-28 Texaco Inc Method of grease manufacture
US3475335A (en) * 1963-12-24 1969-10-28 Texaco Inc Method and apparatus for continuous grease manufacture
US3970289A (en) * 1974-10-21 1976-07-20 Joseph Rich, Jr. Variable rate opposing rotational mixer and feeder
US4232973A (en) * 1978-01-20 1980-11-11 Societe Symac Continuous mixing apparatus for flowable products
US4859073A (en) * 1988-08-05 1989-08-22 Howseman Jr William E Fluid agitator and pump assembly
US5338115A (en) * 1992-12-11 1994-08-16 The United States Of America As Represented By The United States Department Of Energy Mixing device for materials with large density differences
US5518312A (en) * 1993-12-27 1996-05-21 Kajima Corporation Mixing device and method
US5549382A (en) * 1995-04-27 1996-08-27 Correia, Ii; Bernard A. Stirrer for food preparation
US5718510A (en) * 1995-02-28 1998-02-17 Inco Limited Paste production and storage apparatus
WO1998043725A1 (en) * 1997-03-27 1998-10-08 Nova Chemicals (International) S.A. Polymerization process using a dual shear mixing element
US5823667A (en) * 1996-03-19 1998-10-20 Pacific Machinery & Engineering Co., Ltd. Mixer having a segmented helical mixing blade
US5908240A (en) * 1994-06-30 1999-06-01 Hood; Max George Apparatus for cement blending capable of forming a thick slurry
JP3001387B2 (ja) 1993-12-27 2000-01-24 鹿島建設株式会社 混練装置
JP2000140596A (ja) * 1999-01-01 2000-05-23 Kajima Corp 混練方法
US6390664B1 (en) * 1999-10-21 2002-05-21 Harald Kniele Compulsory mixer used, in particular, as a cement mixer
US20040057338A1 (en) * 2000-04-06 2004-03-25 Egidio Pecis Mixer for preparing feedstuffs
US20070242562A1 (en) * 2006-04-12 2007-10-18 Mao-Hsin Huang Beverage dispenser
CN103831056A (zh) * 2012-11-25 2014-06-04 新疆福克油品股份有限公司 风冷式润滑脂喷丝加工激冷装置
US20140330055A1 (en) * 2011-09-19 2014-11-06 Korea Institute Of Industrial Technology Method and apparatus for improving heat transfer and reaction efficiency of gas hydrate reactor using scraper
US20140336034A1 (en) * 2013-05-07 2014-11-13 Comadur S.A. Mixer, method of mixing raw material for powder metallurgy binder for injection moulding composition
US20160310921A1 (en) * 2013-12-31 2016-10-27 Shenzhen China Star Optoelectronics Technology Co., Ltd Crucible device and the use of the crucible device in lcd panel productions
US20170181444A1 (en) * 2015-12-28 2017-06-29 Tetra Laval Holdings & Finance S.A. Apparatus for producing a food product
US20180178176A1 (en) * 2015-07-01 2018-06-28 Sumitomo Heavy Industries Process Equipment Co., Ltd. Stirring Device
EP3852897A4 (en) * 2018-09-19 2022-05-18 Haven Technology Solutions LLC METHOD AND DEVICE FOR SEPARATE A LIGHTER DENSITY FLUID FROM A HEAVIER DENSITY FLUID

Cited By (37)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2417495A (en) * 1943-12-10 1947-03-18 Girdler Corp Manufacture of grease
US2483282A (en) * 1945-09-15 1949-09-27 Girdler Corp Art of grease manufacture
US2610042A (en) * 1946-10-11 1952-09-09 Dryon Paul Apparatus for working pastes
US2567412A (en) * 1947-05-17 1951-09-11 Mcgraw Electric Co Transformer and method of impregnation
US2890039A (en) * 1953-11-02 1959-06-09 Karl Schmidt Metallschmelzwerk Apparatus for the introduction of substances into liquids of high specific gravity
US2908652A (en) * 1955-08-15 1959-10-13 Forrester Gilbert Process and apparatus for defoaming liquids
US3475335A (en) * 1963-12-24 1969-10-28 Texaco Inc Method and apparatus for continuous grease manufacture
US3439836A (en) * 1967-01-27 1969-04-22 Ronald J Ricciardi Apparatus for conditioning and dispensing particulated material
US3475337A (en) * 1967-05-29 1969-10-28 Texaco Inc Method of grease manufacture
US3970289A (en) * 1974-10-21 1976-07-20 Joseph Rich, Jr. Variable rate opposing rotational mixer and feeder
US4232973A (en) * 1978-01-20 1980-11-11 Societe Symac Continuous mixing apparatus for flowable products
US4859073A (en) * 1988-08-05 1989-08-22 Howseman Jr William E Fluid agitator and pump assembly
US5338115A (en) * 1992-12-11 1994-08-16 The United States Of America As Represented By The United States Department Of Energy Mixing device for materials with large density differences
US5518312A (en) * 1993-12-27 1996-05-21 Kajima Corporation Mixing device and method
JP3001387B2 (ja) 1993-12-27 2000-01-24 鹿島建設株式会社 混練装置
US5908240A (en) * 1994-06-30 1999-06-01 Hood; Max George Apparatus for cement blending capable of forming a thick slurry
US5718510A (en) * 1995-02-28 1998-02-17 Inco Limited Paste production and storage apparatus
US5806977A (en) * 1995-02-28 1998-09-15 Inco Limited Paste production and storage process
US5549382A (en) * 1995-04-27 1996-08-27 Correia, Ii; Bernard A. Stirrer for food preparation
US5823667A (en) * 1996-03-19 1998-10-20 Pacific Machinery & Engineering Co., Ltd. Mixer having a segmented helical mixing blade
WO1998043725A1 (en) * 1997-03-27 1998-10-08 Nova Chemicals (International) S.A. Polymerization process using a dual shear mixing element
JP2000140596A (ja) * 1999-01-01 2000-05-23 Kajima Corp 混練方法
US6390664B1 (en) * 1999-10-21 2002-05-21 Harald Kniele Compulsory mixer used, in particular, as a cement mixer
US20040057338A1 (en) * 2000-04-06 2004-03-25 Egidio Pecis Mixer for preparing feedstuffs
US6752530B2 (en) * 2000-04-06 2004-06-22 Seko Spa Mixer with helical feeder and recirculation scroll for preparing material for animal feeding
US20070242562A1 (en) * 2006-04-12 2007-10-18 Mao-Hsin Huang Beverage dispenser
US10023821B2 (en) * 2011-09-19 2018-07-17 Korea Institute Of Industrial Technology Method and apparatus for improving heat transfer and reaction efficiency of gas hydrate reactor using scraper
US20140330055A1 (en) * 2011-09-19 2014-11-06 Korea Institute Of Industrial Technology Method and apparatus for improving heat transfer and reaction efficiency of gas hydrate reactor using scraper
CN103831056A (zh) * 2012-11-25 2014-06-04 新疆福克油品股份有限公司 风冷式润滑脂喷丝加工激冷装置
CN103831056B (zh) * 2012-11-25 2016-02-10 新疆福克油品股份有限公司 风冷式润滑脂喷丝加工激冷装置
US20140336034A1 (en) * 2013-05-07 2014-11-13 Comadur S.A. Mixer, method of mixing raw material for powder metallurgy binder for injection moulding composition
US9908261B2 (en) * 2013-05-07 2018-03-06 Comadur S.A. Mixer, method of mixing raw material for powder metallurgy binder for injection moulding composition
US20160310921A1 (en) * 2013-12-31 2016-10-27 Shenzhen China Star Optoelectronics Technology Co., Ltd Crucible device and the use of the crucible device in lcd panel productions
US20180178176A1 (en) * 2015-07-01 2018-06-28 Sumitomo Heavy Industries Process Equipment Co., Ltd. Stirring Device
US10478791B2 (en) * 2015-07-01 2019-11-19 Sumitomo Heavy Industries Process Equipment Co., Ltd. Stirring device
US20170181444A1 (en) * 2015-12-28 2017-06-29 Tetra Laval Holdings & Finance S.A. Apparatus for producing a food product
EP3852897A4 (en) * 2018-09-19 2022-05-18 Haven Technology Solutions LLC METHOD AND DEVICE FOR SEPARATE A LIGHTER DENSITY FLUID FROM A HEAVIER DENSITY FLUID

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