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US3684251A - Apparatus for continuous emulsification - Google Patents

Apparatus for continuous emulsification
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US3684251A
US3684251AUS70297AUS3684251DAUS3684251AUS 3684251 AUS3684251 AUS 3684251AUS 70297 AUS70297 AUS 70297AUS 3684251D AUS3684251D AUS 3684251DAUS 3684251 AUS3684251 AUS 3684251A
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chamber
emulsion
internal phase
chambers
phase
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US70297A
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George W Bowling
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United States Department of the Army
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United States Department of the Army
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Abstract

A continuous method for the production of a high-internal-phaseratio emulsion containing approximately 90 to 99 percent internal phase utilizing an apparatus having a series of stacked consecutive-flow mixing chambers of progressively increasing dimensions. The internal phase is added successively to the separate chambers whereas the external phase is added to the first chamber.

Description

United States Patent Bowling [451 Aug. 15, 1972 [54] APPARATUS FOR CONTINUOUS EMULSIFICATION [72] Inventor: George W. Bowling, Circleville,
Ohio
[73] Assignee: The United States of America as represented by the Secretary of the Army [22] Filed: Sept. 8, 1970 [21] App1.No.: 70,297
[52] US. Cl ..259/8, 252/314, 252/359 R, 259/D1G. 30 [51] Int. Cl. ..B0lf 7/16, BOlf 15/02 [58] Field of Search ..259/DlG. 30, 7, 8, 23, 24, 259/43, 44, 66, 67, 107, 108, 4, 9, 10; 261/84; 252/341, 359 R [56] References Cited UNITED STATES PATENTS 2,751,425 6/1956 Rupp ..252/359 R X 3,544,078 12/1970 Stupakis .25 9/4 1,848,100 3/1932 Benner et a1 ..259/D1G. 30
989,126 4/1911 Currie ..259/24 1,097,474 5/1914 Schroder ..259/DIG. 30
Primary Examiner-Robert W. Jenkins Assistant Examiner-Philip R. Coe
Attorney-Harry M. Saragovitz, Edward J. Kelly and Herbert Berl 5 7] ABSTRACT A continuous method for the production of a high-internal-phase-ratio emulsion containing approximately 90 to 99 percent internal phase utilizing an apparatus having a series of stacked consecutive-flow mixing chambers of progressively increasing dimensions. The internal phase is added successively to the separate chambers whereas the external phase is added to the first chamber.
2 Claims, 2 Drawing Figures APPARATUS FOR CONTINUOUS EMULSIFICATION The invention described herein may be manufactured, used, and licensed by or for the Government for governmental purposes without the payment to me of any royalty thereon.
This invention relates to a method and apparatus for the continuous production of an emulsion containing approximately 90 to 99 percent internal phase.
The present emulsification process is accomplished by a stagewise addition of an internal phase to a series of consecutive-flow mixing chambers. The internal phase of the emulsion produced may be any light hydrocarbon oil such as MIL-T6624 JP-4 fuel. The external phase of the emulsion produced may be any aqueous or nonaqueous material suitable for the production of emulsified fuel known as MEF-2, e.g., a mixture of ethylene glycol, water and tallow amine acetate. In combination, these ingredients represent, e.g., 4 percent by weight of the total emulsion. Mixing chambers are arranged in such a manner that the flow of the emulsion will progress through the series of mixing chambers from the smallest to the largest in size. The size of the individual mixing chambers will vary according to the throughput in the individual chamber such that the residence time in the separate mixing chambers is approximately equal. The external phase of the mixture is added to the mixing chamber having the smallest volume and first in the series flow configuration. It is essential that the flow rate to the first mixing chamber into which the internal phase is added, is such that the volume of internal phase is less than 70 percent of the emulsion formed in that mixing chamber so that the formation of an emulsion with the proper internal phase will be insured. The internal phase can then be added to succeeding mixing chambers to raise the concentration of the internal phase after the initial emulsion has been formed.
Each of the individual mixing chambers contain suitable means to agitate the fluid in the mixing chamber at a sufficient shear level to insure adequate emulsification while at a sufficiently low shear level so that the emulsion is not demulsified. Baffles may be positioned in the individual mixing chambers to assure a uniform mixing action and to eliminate the possibility of dead spots. The internal phase of the emulsion may be added to any or all of the mixing chambers and the selection of the form of addition will be dependent upon the individual formulation of the emulsion being produced. In certain cases, it will be necessary that the internal phase be added to alternate mixing chambers to allow a resting or complete reconstitution of the emulsion as the emulsion progresses through the various stages of the emulsification process. The number of mixing chambers can be expanded or contracted as desired. However, it is envisioned that from 7 to 21 mixing chambers will be sufficient to insure adequate emulsification.
It is an object of this invention to provide and disclose a continuous method for the production of a highintemal-phase-ratio emulsion.
It is a further object of this invention to provide and disclose a continuous method for the production of an emulsion containing 90 to 99 volume percent internal phase.
It is a further object of this invention to provide and disclose a system for the continuous production of a high-internal-phase-ratio emulsion.
It is a further object of this invention to provide and disclose a system for the production of an emulsion containing to 99 volume percent internal phase.
Other objects and a fuller understanding of the invention may be had by referring to the following description and claims taken in conjunction with the accompanying drawing in which:
FIG. I shows a prospective view of the emulsification system.
FIG. II shows an enlarged sectional view through 2- 2 of FIG. I.
Referring now to the drawing the system compriseshousing 15 having a series of vertically positioned stacked emulsion chambers l to 14 positioned therein.Housing 15 is supported on means 17. Bores 19 connect the series of chambers. For purposes of illustration, the volume of each chamber has been designated on the drawing.Common shaft 16, which extends axially through the interior of chambers l to 14, is operable connected tomixer drive 18.Blade assembly 20 is attached toshaft 16 thereby providing the agitation means. The internal phase is conducted fromstorage 21, by any conventional power means, e.g.,pump 25, into U-shaped feed conduit means 22. Feed conduit means 22 may be positioned on any suitable support, e.g., means 23. Flow meters 1' to 14' are positioned on feed conduit means 22. Said flow meters regulate the flow of the internal phase into the emulsification chambers. Conduit means 1" to 14" connectflow meters 1 to 14' with the emulsification chambers. The external phase is conducted fromstorage 27 by any conventional power means,pump 29, throughconduit 1" intoemulsification chamber 1. The flow of the external phase is regulated byflow meter 1". The emulsion exits fromchamber 14 by means ofoutlet 24 and is recovered.
In an illustrative example of the production of an emulsion containing 96 percent internal phase, an external phase consisting of a mixture of about 12.50 percent tallow-amine acetate, 54.75 percent water and 32.75 percent ethylene glycol is fed intochamber 1 until the chamber is completely full. At this point,mixer drive 18 is engaged andcommon shaft 16 on whichimpeller blades assembly 20 are affixed within each chamber is rotated at a fixed RPM between 500 and 1000. The specific RPM selected is dependent on the particular emulsion being produced in that the agitation must be less than the critical shear parameter of that emulsion. For a number of formulations this has been shown to be in the range of approximately 10,000 sec. When the chamber is full of external phase material and the shaft rotation begins, JP-4 (internal phase) is fed intochamber 1 at the proper rate for which the unit was designed. For example, the present system is designed for a one gallon-per-minute production rate with a 4 percent by volume emulsion. Therefore, sincechamber 1 has a volume capacity of 0.06 gallons, the flow rate of external phase intochamber 1 is 0.04 gallons-per-rninute and the flow rate of the internal phase is 0.02 gallons-per-minute. This procedure has the effect of providing complete agitation of the ingredients within the chamber. When the mixture ofchamber 1 has been forced upward intochamber 2, additional JPn4 is added tochamber 2.Chamber 2 has a volume capacity of 0.07 gallons.Chamber 2 receives 0.06 gallons fromchamber 1. Therefore, the JP-4 flow rate throughconduit 2" is 0.01 gallon -per-minute. This procedure is followed through chamber M where a 96 percent internal phase emulsion is recovered. The exact input of the internal phase into each chamber as you progress upward can be calculated by taking the volume of a specific chamber as shown in the drawing and subtracting it from the volume of the previous chamber, e.g.,chamber 5 has a volume ofO. l 7 gallons;chamber 6 has a volume of 0.22 gallons; consequently, the internal phase is introduced intochamber 6 at the rate of 0.05 gallons-per-minute to satisfy the 0.22 gallon volume ofchamber 6.
Utilization of the present invention has resulted in the obtainment of a cleaner, uniform product than was possible under the batch method. In addition, the present method inhibits the loss of light ends (volatile) of certain ingredients, e.g., JP-4 fuel.
Although I have described my invention with a certain degree of particularity, it is understood that the present disclosure has been made only by way of example and that numerous changes in the details of construction and the combination and arrangement of parts and/or formulation of emulsions may be resorted to without departing from the spirit and scope of the invention as hereinafter claimed.
Having described my invention, 1 claim:
ll. An apparatus for the continuous production of emulsions comprising a series of stacked interconnecting chambers of progressively increasing capacity commencing from the bottom to the top of the series, a common shaft extending axially through the stacked chambers, agitating means attached to the shaft and confined within each chamber, means for the introduction of an external phase of an emulsion into the first of the chambers at the bottom of the series, means for the introduction of an internal phase of an emulsion separately into each of the series of chambers, and means for recovery of the emulsion.
2. An apparatus in accordance withclaim 1 comprising 7 to 21 chambers.

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US70297A1970-09-081970-09-08Apparatus for continuous emulsificationExpired - LifetimeUS3684251A (en)

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Cited By (21)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
US3764115A (en)*1971-06-301973-10-09IbmMethod and apparatus for mixing fluids
US3779518A (en)*1971-02-111973-12-18Agfa Gevaert AgContinuous photographic emulsion processing
US3807703A (en)*1972-10-121974-04-30Usm CorpMixer-emulsators
US3836126A (en)*1971-12-271974-09-17Allis ChalmersMixer pump
US4746460A (en)*1984-12-071988-05-24The British Petroleum Company P.L.C.Preparation of emulsions
US5147134A (en)*1986-08-211992-09-15Petrolite CorporationProcess for the continuous production of high-internal-phase-ratio emulsions
US5320832A (en)*1992-03-271994-06-14Colgate PalmoliveContinuous process for making a non-Newtonian paste or cream like material
US5399293A (en)*1992-11-191995-03-21Intevep, S.A.Emulsion formation system and mixing device
US5753596A (en)*1995-11-091998-05-19Baker Hughes IncorporatedMethods and emulsions for inhibition of oil well corrosion
US5843334A (en)*1994-06-201998-12-01Nippon Shinyaku Co., Ltd.Method of producing emulsions and an emulsification apparatus
US20050282914A1 (en)*2004-06-182005-12-22Reed Ted AContinuous manufacture of high internal phase ratio emulsions using relatively low-shear and low-temperature processing steps
US20060078606A1 (en)*1997-09-182006-04-13Skyepharma Inc.Sustained-release liposomal anesthetic compositions
US9585838B2 (en)1997-11-142017-03-07Pacira Pharmaceuticals, Inc.Production of multivesicular liposomes
US11033495B1 (en)2021-01-222021-06-15Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11278494B1 (en)2021-01-222022-03-22Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11357727B1 (en)2021-01-222022-06-14Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12151024B2 (en)2021-01-222024-11-26Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12156940B1 (en)2024-05-202024-12-03Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12251468B1 (en)2024-05-202025-03-18Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12251472B1 (en)2024-05-202025-03-18Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12285419B2 (en)2021-10-142025-04-29Pacira Pharmaceuticals, Inc.Bupivacaine multivesicular liposome formulations and uses thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
US989126A (en)*1910-06-081911-04-11James CurrieMachine for hydrating lime.
US1097474A (en)*1913-07-231914-05-19Wilhelm Gotthilf SchroederDevice for mixing emulsions.
US1848100A (en)*1924-10-301932-03-08Universal Oil Prod CoApparatus for producing suspensions
US2751425A (en)*1951-02-011956-06-19Exxon Research Engineering CoMethod and apparatus for mixing and contacting fluids
US3544078A (en)*1967-04-281970-12-01Du PontJet fluid mixing process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
US989126A (en)*1910-06-081911-04-11James CurrieMachine for hydrating lime.
US1097474A (en)*1913-07-231914-05-19Wilhelm Gotthilf SchroederDevice for mixing emulsions.
US1848100A (en)*1924-10-301932-03-08Universal Oil Prod CoApparatus for producing suspensions
US2751425A (en)*1951-02-011956-06-19Exxon Research Engineering CoMethod and apparatus for mixing and contacting fluids
US3544078A (en)*1967-04-281970-12-01Du PontJet fluid mixing process

Cited By (42)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
US3779518A (en)*1971-02-111973-12-18Agfa Gevaert AgContinuous photographic emulsion processing
US3764115A (en)*1971-06-301973-10-09IbmMethod and apparatus for mixing fluids
US3836126A (en)*1971-12-271974-09-17Allis ChalmersMixer pump
US3807703A (en)*1972-10-121974-04-30Usm CorpMixer-emulsators
US4746460A (en)*1984-12-071988-05-24The British Petroleum Company P.L.C.Preparation of emulsions
US5147134A (en)*1986-08-211992-09-15Petrolite CorporationProcess for the continuous production of high-internal-phase-ratio emulsions
US5320832A (en)*1992-03-271994-06-14Colgate PalmoliveContinuous process for making a non-Newtonian paste or cream like material
US5399293A (en)*1992-11-191995-03-21Intevep, S.A.Emulsion formation system and mixing device
US5843334A (en)*1994-06-201998-12-01Nippon Shinyaku Co., Ltd.Method of producing emulsions and an emulsification apparatus
US5753596A (en)*1995-11-091998-05-19Baker Hughes IncorporatedMethods and emulsions for inhibition of oil well corrosion
US20060078606A1 (en)*1997-09-182006-04-13Skyepharma Inc.Sustained-release liposomal anesthetic compositions
US8182835B2 (en)1997-09-182012-05-22Pacira Pharmaceuticals, Inc.Sustained-release liposomal anesthetic compositions
US8834921B2 (en)1997-09-182014-09-16Pacira Pharmaceuticals, Inc.Sustained-release liposomal anesthetic compositions
US9192575B2 (en)1997-09-182015-11-24Pacira Pharmaceuticals, Inc.Sustained-release liposomal anesthetic compositions
US9205052B2 (en)1997-09-182015-12-08Pacira Pharmaceuticals, Inc.Sustained-release liposomal anesthetic compositions
US9585838B2 (en)1997-11-142017-03-07Pacira Pharmaceuticals, Inc.Production of multivesicular liposomes
US20050282914A1 (en)*2004-06-182005-12-22Reed Ted AContinuous manufacture of high internal phase ratio emulsions using relatively low-shear and low-temperature processing steps
US7144148B2 (en)*2004-06-182006-12-05General Electric CompanyContinuous manufacture of high internal phase ratio emulsions using relatively low-shear and low-temperature processing steps
US11185506B1 (en)2021-01-222021-11-30Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11925706B2 (en)2021-01-222024-03-12Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11033495B1 (en)2021-01-222021-06-15Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11278494B1 (en)2021-01-222022-03-22Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11304904B1 (en)2021-01-222022-04-19Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11311486B1 (en)2021-01-222022-04-26Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11357727B1 (en)2021-01-222022-06-14Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11426348B2 (en)2021-01-222022-08-30Pacira Pharmaceuticals, Inc.Compositions of bupivacaine multivesicular liposomes
US11452691B1 (en)2021-01-222022-09-27Pacira Pharmaceuticals, Inc.Compositions of bupivacaine multivesicular liposomes
US11819574B2 (en)2021-01-222023-11-21Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11819575B2 (en)2021-01-222023-11-21Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US11179336B1 (en)2021-01-222021-11-23Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12144890B2 (en)2021-01-222024-11-19Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12151024B2 (en)2021-01-222024-11-26Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12296047B2 (en)2021-01-222025-05-13Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12178909B1 (en)2021-01-222024-12-31Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12285419B2 (en)2021-10-142025-04-29Pacira Pharmaceuticals, Inc.Bupivacaine multivesicular liposome formulations and uses thereof
US12246092B1 (en)2024-05-202025-03-11Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12251468B1 (en)2024-05-202025-03-18Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12251472B1 (en)2024-05-202025-03-18Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12280149B1 (en)2024-05-202025-04-22Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12156940B1 (en)2024-05-202024-12-03Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12318483B1 (en)2024-05-202025-06-03Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes
US12370142B1 (en)2024-05-202025-07-29Pacira Pharmaceuticals, Inc.Manufacturing of bupivacaine multivesicular liposomes

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