Forming emulsions

Information

  • Patent Grant
  • 6764213
  • Patent Number
    6,764,213
  • Date Filed
    Tuesday, August 20, 2002
    22 years ago
  • Date Issued
    Tuesday, July 20, 2004
    20 years ago
Abstract
Emulsification is achieved by directing a jet of fluid along a first path, and interposing a structure in the first path to cause the fluid to be redirected in a controlled flow along a new path, the first path and the new path being oriented to cause shear and cavitation in the fluid. A hot emulsion is stabilized immediately after formation by causing the emulsion to flow away from the outlet end of an emulsion forming structure, and causing a cooling fluid to flow in a direction generally opposite to the flow of the emulsion and in close enough proximity to exchange heat with the emulsion flow. In another aspect, emulsification of a first fluid component within a second fluid component is achieved by providing an essentially stagnant supply of the first fluid component in a cavity, and directing a jet of the second fluid component into the first fluid component, with the temperatures and the jet velocities of the fluids being chosen to cause cavitation due to hydraulic separation at the interface between the two fluids. In other aspects, a coiled tube is used to reduce pressure fluctuations in an emulsifying cell fed from a fluid line by a high pressure pump; A two-piece nozzle is used in an emulsification structure; an absorption cell has a reflective surface at the end of the chamber for reflecting the jet, and a mechanism is provided for adjusting the distance from the reflective surface to the open end; a modular emulsification structure includes a series of couplings that can be fitted together in a variety of ways.
Description




BACKGROUND OF THE INVENTION




This invention relates to forming emulsions.




We use the term “emulsion” for a system comprising two immiscible liquid phases, with one phase dispersed as small droplets in the other phase. For simplicity we will call the dispersed phase “oil” and the continuous phase “water”, although the actual components may vary widely. As additional components, emulsifying agents, known as emulsifiers or surfactants, serve to stabilize emulsions and facilitate their formation, by surrounding the oil phase droplets and separating them from the water phase.




The uses of emulsions have been increasing for many years. Most processed food and beverage products, medicine and personal care products, paints, inks, toners, and photographic media are either emulsions or employ emulsions. In recent years, demand for emulsions with smaller and more uniform droplets has increased. Artificial blood applications, for example, require nearly uniform droplets averaging 0.2 micrometers. Jet-ink printing has similar requirements of size and distribution.




High pressure homogenizers are often used to produce small and uniform droplets or particles, employing a device which is commonly referred to as an homogenizing valve. The valve is kept closed by a plug forced against a seat by means of a spring or hydraulic or pneumatic pressure. The pre-mixed raw emulsion is fed at a high pressure, generally between 1,000 and 15,000 psi, to the center of the valve seat. When the fluid pressure overcomes the force closing the valve, a narrow annular gap (10-200 um) is opened between the valve seat and the valve plug. The raw emulsion flows through, undergoing rapid acceleration as well as sudden drop in pressure which breaks down the oil phase into small droplets. More recently, a new type of high pressure homogenizer was introduced, employing two or more fixed orifices, and capable of reaching 40,000 psi. When forced through these orifices, the pre-mixed raw emulsion forms liquid jets which are caused to impinge at each other. A description is found in U.S. Pat. Nos. 4,533,254 and 4,908,154.




The typical mechanism for emulsification in this type of device is the controlled use of shear, impact, and cavitation forces in a small zone. The relative effects of these forces generally depend on the fluid's characteristics, but in the vast majority of emulsion preparation schemes, cavitation is the dominant force.




Fluid shear is created by differential velocity within the fluid stream, generated by the sudden fluid acceleration upon entering the orifice or small gap, by the difference between the extremely high velocity at the center of the orifice and zero velocity at the surfaces defining the orifice, and by the intense turbulence which occurs after exiting the orifice.




Cavitation takes place when pressure drops momentarily below the vapor pressure of the water phase. Small vapor bubbles form and then collapse (within 10-3 to 10-9 sec.), generating shock waves which break down surrounding oil droplets. Cavitation occurs in homogenizing valves when the sudden acceleration in the orifice, with a simultaneous pressure drop, causes the local pressure to drop momentarily below the vapor pressure.




More generally, it has become known that cavitation occurs when two surfaces are separated faster than some critical velocity, and that cavitation bubbles affect their surrounding only during the formation of the cavities, and not during the collapse of the cavities, as had been long assumed. Another discovery of interest is that cavitation can occur either totally within the liquid, or at the solid-liquid interfaces, depending on the relative strength of solid-liquid adhesion and the liquid—liquid cohesion.




Typical emulsification schemes have several characteristics worth noting. Cavitation takes place only once, for a very short time (10-3 to 10-9 seconds), and equipment which employs high power density imparts emulsification energy only to a very small portion of the product at any given time. The emulsification process is thus highly sensitive to the uniformity of the feed stock, and several passes through the equipment are usually required before the desired average droplet size and uniformity are achieved. The final droplet size depends on the surfactant's rate of interaction with the oil phase. Because surfactants cannot generally surround the oil droplets at the same rate they are being formed by the emulsifying process, agglomeration takes place and average droplets size increases. There is a typical sharp increase in product temperature during the process, which limits the choice of emulsion ingredients and processing pressure, as well as accelerating the agglomeration rate of the droplets after the emulsification process. Some processes require very small solid polymer or resin particles; and this is often accomplished by dissolving solid polymers or resins in VOC's (volatile organic compounds), then employing mixing equipment to reduce the droplets size, and finally removing the VOC.




SUMMARY OF THE INVENTION




In general, in one aspect, the invention features a method for use in causing emulsification in a fluid. In the method, a jet of fluid is directed along a first path, and a structure is interposed in the first path to cause the fluid to be redirected in a controlled flow along a new path, the first path and the new path being oriented to cause shear and cavitation in the fluid.




Implementations of the invention may include the following features.




The first path and the new path may be oriented in essentially opposite directions. The coherent flow may be a cylinder surrounding the jet. The interposed structure may have a reflecting surface that is generally semi-spherical, or is generally tapered, and lies at the end of a well. Adjustments may be made to the pressure in the well, in the distance from the opening of the well to the reflecting surface, and in the size of the opening to the well. The controlled flow, as it exits the well, may be directed in an annular sheet away from the opening of the well. An annular flow of a coolant may be directed in a direction opposite to the direction of the annular sheet.




In general, in another aspect, the invention features a method for use in stabilizing a hot emulsion immediately after formation. The emulsion is caused to flow away from the outlet end of an emulsion forming structure, and a cooling fluid is caused to flow in a direction generally opposite to the flow of the emulsion and in close enough proximity to exchange heat with the emulsion flow.




Implementations of the invention may include the following features. The emulsion may be formed as a thin annular sheet as it flows out of the emulsion forming structure. The cooling fluid may be a thin annular sheet as it flows opposite to the emulsion. The cooling fluid may be a liquid or gas compatible with the emulsion. The flows of the emulsion and the cooling fluid may occur in an annular valve opening.




In general, in another aspect, the invention features a method for use in causing emulsification of a first fluid component within a second fluid component. In the method, an essentially stagnant supply of the first fluid component is provided in a cavity. A jet of the second fluid component is directed into the second fluid component. The temperatures and the jet velocities of the fluids are chosen to cause cavitation due to hydraulic separation at the interface between the two fluids.




Implementations of the invention may include the following features. The second fluid component may include a continuous phase of an emulsion or dispersion. The first fluid component may be a discontinuous phase in the emulsion, e.g., a solid discontinuous phase. The second fluid may be provided in an annular chamber, and the jet may be delivered from an outlet of an orifice which opens into the annular chamber. After emulsification by hydraulic separation, the product may be passed through an orifice to cause additional emulsification, or may be delivered to a subsequent processing chamber, where an additional component may be added to the emulsion. A cooling fluid may be applied to the product in the subsequent processing chamber to quickly cool and stabilize the emulsion. The subsequent processing chamber may be an absorption cell into which a jet of the product is directed.




In general, in another aspect, the invention features an apparatus for reducing pressure fluctuations in an emulsifying cell fed from a fluid line by a high pressure pump. A coiled tube in the fluid line between the pump and the emulsifying cell has internal volume, wall thickness, coil diameter and coiling pattern adequate to absorb the pressure fluctuations and capable of withstanding the high pressure generated by the pump. The apparatus may include a shell around the coiled tube with ports for filling the shell with heating or cooling fluid.




In general, in another aspect, the invention features a nozzle for use in an emulsification structure. In the structure, two body pieces having flat surfaces mate to form the nozzle, at least one of the members having a groove to form an orifice in the nozzle. The surfaces are sufficiently flat so that when the two body pieces are pressed together with sufficient force, fluid flow is confined to the orifice. In implementations of the invention, the cavitation inducing surfaces may be defined on the groove; and a wall of the groove may be coated with diamond or non-polar materials or polar materials.




In general, in another aspect, the invention features an absorption cell for use in an emulsification structure. The cell includes an elongated chamber having an open end for receiving a jet of fluid having two immiscible components. A reflective surface is provided at the other end of the chamber for reflecting the jet. And a mechanism is provided for adjusting the distance from the reflective surface to the open end.




Implementations of the invention may include the following features. The reflective surfaces may be interchangeable for different applications. There may be a removable insert for insertion into the chamber at the open end, the insert having an orifice of a smaller dimension than the inner wall of the chamber. There may be several different inserts each suitable for a different application.




In general, in another aspect, the invention features a modular emulsification structure comprising a series of couplings that can be fitted together in a variety of ways. Each of at least one of the couplings includes an annular male sealing surface at one end of the coupling, and an annular female sealing surface at the other end of the coupling. An opening is provided between the male and female sealing surfaces, for communicating fluid from a up-stream coupling to a down-stream coupling. Ports are provided for feeding fluid into or withdrawing fluid from the coupling. At least some of the communicating openings are sufficiently small to form a liquid jet. The sealing surfaces are sufficiently smooth to provide a fluid-tight seal when the couplings are held together by a sufficient compressive force directed along the length of the structure.




Implementations of the invention may include the following features. A processing chamber may be defined between the male sealing surface of one of the up-stream couplings and the female sealing surface of one of the down-stream couplings. In some of the couplings, the orifice may extend from one end of the coupling to the other. An absorption cell coupling may be used at one of the structure. One of the couplings may extend into another coupling to form a small annular opening for generating an annular flow sheet of cooling fluid. Some of the ports in the couplings are used for CIP/SIP cleaning and/or sterilization procedures.




Advantages of the invention include the following.




Very small liquid droplets or solid particles may be processed in the course of emulsifying, mixing, suspending, dispersing, or de-agglomerating solid and/or liquid materials. Nearly uniform sub-micron droplets or particles are produced. The process is uniform over time because pressure spikes that are normally generated by the high pressure pump are eliminated. A broader range of types of emulsion ingredients may be used while maximizing their effectiveness by introducing them separately into the high velocity fluid jet. Fine emulsions may be produced using fast reacting ingredients, by adding each ingredient separately and by controlling the locations of their interaction. Control of temperature before and during emulsification allows multiple cavitation stages without damaging heat sensitive ingredients, by enabling injection of ingredients at different temperatures and by injecting compressed air or liquid nitrogen prior to the final emulsification step. The effects of cavitation on the liquid stream are maximized while minimizing the wear effects on the surrounding solid surfaces, by controlling orifice geometry, materials selection, surface characteristics, pressure and temperature. Absorption of the jet's kinetic energy into the fluid stream is maximized, while minimizing its wear effect on surrounding solid surfaces. A sufficient turbulence is achieved to prevent agglomeration before the surfactants can fully react with the newly formed droplets. Agglomeration after treatment is minimized by rapid cooling, by injecting compressed air or nitrogen and/or by rapid heat exchange, while the emulsion is subjected to sufficient turbulence to overcome the oil droplets' attractive forces and maintaining sufficient pressure to prevent the water from vaporizing.




Scale-up procedures from small laboratory scale devices to large production scale systems is made simpler because every process parameter can be carefully controlled. The invention is applicable to emulsions, microemulsions, dispersions, liposomes, and cell rupture. A wide variety of immiscible liquids may be used, in a wider range of ratios. Smaller amounts of (in some cases no) emulsifiers are required. Emulsions can be produced in one pass through the process. The reproducibility of the process is improved. A wide variety of emulsions may be produced for diverse uses such as food, beverages, pharmaceuticals, paints, inks, toners, fuels, magnetic media, and cosmetics. The apparatus is easy to assemble, disassemble, clean, and maintain. The process may be used with fluids of high viscosity, high solid content, and fluids which are abrasive and corrosive.




The emulsification effect continues long enough for surfactants to react with newly formed oil droplets. Multiple stages of cavitation assure complete use of the surfactant with virtually no waist in the form of micelles. Multiple ports along the process stream may be used for cooling by injecting ingredient at lower temperature. VOC's may be replaced with hot water to produce the same end products. The water will be heated under high pressure to well above the melting point of the polymer or resin. The solid polymer or resins will be injected in its solid state, to be melted and pulverized by the hot water jet. The provision of multiple ports eliminates the problematic introduction of large solid particles into the high pressure pumps, and requires only standard industrial pumps.




Other advantages and features will become apparent from the following description and from the claims.











BRIEF DESCRIPTION OF THE DRAWINGS





FIGS. 1 and 2

are block diagrams of emulsification systems.





FIGS. 3A and 3B

are an end view and a cross-sectional view (at A—A of

FIG. 3A

) of an emulsifying cell assembly.





FIG. 4

is a larger scale cross-sectional view (at BB of

FIG. 3A

) of the emulsifying cell assembly.





FIG. 5

is a cross-sectional view of another modular emulsifying cell assembly.





FIG. 6

is an isometric exploded view, not to scale, of two types of a two-piece nozzle assembly.





FIGS. 7A and 7B

are an enlarged end view and a cross-sectional view of an adapter for the two-piece nozzle assembly.





FIG. 8

is a schematic cross-sectional diagram, not to scale, of fluid flow in an absorption cell.





FIG. 9

is a cross-sectional view of an absorption cell.





FIGS. 10 and 11

are cross-sectional diagrams, not to scale, of fluid flow in other modular absorption cell assemblies.





FIGS. 12A

,


12


B and


12


C are an end view, a front view, and a top view of a coil for regulating process pressure in the emulsifying cell.





FIG. 13

is an assembly of three coils shown in FIGS.


12


A through


12


C.











DESCRIPTION OF THE PREFERRED EMBODIMENTS




In

FIG. 1

, the product ingredients are supplied from sources


110


,


112


, and


114


into a pre-mixing system


116


. For simplicity, only three types of ingredients are shown by way of example: water, oil, and emulsifier; but a wide variety of other ingredients could be used depending on the product to be made. The pre-mixing system


116


is of a suitable kind (e.g. propeller mixer, colloid mill, homogenizer, etc.) for the type of product. After pre-mixing, the ingredients are fed into the feed tank


118


. In some cases, the pre-mixing may be performed inside feed tank


118


. The pre-mixed product from tank


118


then flows through line


120


and valve


122


, by means of transfer pump


124


to the high pressure process pump


128


. Transfer pump


124


may be any type of pump normally used for the product, provided it can generate the required feed pressure for proper operation of the high pressure process pump. Pressure indicator


126


is provided to monitor feed pressure to pump


128


. The high pressure process pump


128


is typically a positive displacement pump, e.g., a triplex or intensifier pump. From process pump


128


the product flows at high pressure through line


130


into coil


132


, where pressure fluctuations generated by the action of pump


128


are regulated by expansion and contraction of the coil tubing. A more detailed explanation of the coil mechanism is given in the description of

FIGS. 12A through 12C

. It may be desirable or necessary to heat or cool the feed stock. Heating system


148


may circulate hot fluid in shell


154


via lines


150


and


152


, or cooling system


156


may be used. The heating medium may be hot oil or steam with the appropriate means to control the temperature and flow of the hot fluid, such that the desired product temperature is attained upon exiting coil


132


. The product exits coil


132


through line


134


, where pressure indictor


136


and temperature indicator


138


monitor these parameters, and enters the emulsifying cell


140


at a high and constant pressure, for example a pressure of 15,000 psi.




The emulsification process takes place in emulsifying cell


140


, where the feed stock is forced through at least one jet generating orifice and through an absorption cell wherein the jet's kinetic energy is absorbed by a fluid stream flowing around the jet and in the opposite direction. In each of the treatment stages (there may be more than two), intense forces of shear, impact, and/or cavitation break down the oil phase into extremely small and highly uniform droplets, and sufficient time is allowed for the emulsifier to interact with these small oil droplets to stabilize the emulsion.




Immediately following the emulsification process, cooling fluid from cooling system


156


is injected into the emulsion via line


158


, cooling the emulsion instantly by intimate mixing of the cooling fluid with the hot emulsion inside emulsification cell


140


. Cooling system


156


, may be a source of cool compatible liquid (e.g., cold water) or of compressed gas (e.g., air or nitrogen), with suitable means to control the temperature, pressure and flow of the cooling fluid, such that the desired product temperature is attained upon exiting emulsification cell


140


. The emulsion exits the emulsification cell


140


through line


142


, where metering valve


144


is provided to control back-pressure during cooling, and ensuring that the hot emulsion remains in liquid state while being cooled, thereby maintaining the emulsion integrity and stability. Finally, the finished product is collected in tank


146


.




In the system illustrated by

FIG. 2

, the product's continuous phase is supplied from supply


110


into feeding tank


118


, while other ingredients are supplied from sources


112


and


114


directly into the emulsifying cell


140


. Some ingredients may be mixed together to reduce the number of separate feed lines, or there may be as many feed lines as product ingredients.




Water from tank


118


flows through line


120


and valve


122


, by means of transfer pump


124


to the high pressure process pump


128


. Elements


128


through


138


, and


148


through


158


have similar functions to the same numbered elements of the system of FIG.


1


.




Oil and emulsifier, each representing a possibly unlimited number and variety of ingredients which may be introduced separately, flow from sources


112


and


114


into emulsifying cell


140


, through lines


162


and


164


, each with a pressure indicator


170


and


172


, and a temperature indicator


174


and


176


, by means of metering pumps


166


and


168


. Metering pumps


166


and


168


are suitable for type of product pumped (e.g. sanitary cream, injectable suspension, abrasive slurry) and the required flow and pressure ranges. For example, in small scale systems peristaltic pumps are used, while in production system and/or for high pressure injection, diaphragm or gear pumps are used.




Inside emulsifying cell


140


the water is forced through an orifice, creating a water jet. Other product ingredients, as exemplified by the oil and emulsifier, are injected into emulsifying cell


140


. The interaction between the extremely high velocity water jet inside emulsifying cell


140


and the stagnant ingredients from lines


162


and


164


, subjects the product to a series of treatment stages, in each of which intense forces of shear, impact, and/or cavitation break down the oil and emulsifier to extremely small and highly uniform droplets, and allows sufficient time for the emulsifier to interact with the oil droplets. Immediately following the emulsification process, the emulsion is cooled and then exits the emulsification cell and is collected, all in a manner similar to the one used in the system of FIG.


1


.




As seen in

FIGS. 3 through 9

, the emulsifying cell is constructed using a series of interchangeable couplings, each for a particular purpose. The couplings are used to form an integral pressure containing unit by forcing together a smooth and tapered sealing surface of each coupling into a smooth and tapered corresponding sealing surface in the adjacent coupling, to create a metal-to-metal seal, much like the seal between a standard high pressure nipple and the corresponding female port. Each coupling (except possibly for the end couplings) has a large bore in one side, and a matching protrusion of slightly smaller diameter on the other side, such that each coupling's protrusion fits into the bore of the next coupling, thereby aligning sealing surfaces and facilitating assembly of a large number of couplings. The couplings are fastened together by four bolts.




In the example of a basic emulsifying cell shown in

FIGS. 3A and 3B

, the cell assembly has four couplings: product inlet coupling


10


, nozzle coupling


12


, coolant inlet coupling


14


, and product outlet coupling


16


. Referring also to

FIG. 4

, protrusion


26


of coupling


10


fits into bore


28


in coupling


12


, while sealing surface


22


of coupling


10


is aligned with sealing surface


24


in coupling


12


, to form a pressure containing metal-to-metal seal upon fastening of the assembly with four bolts


17


. The product fluid to be processed enters the emulsifying cell from port


18


, which is a standard ¼″ H/P port (e.g., Autoclave Engineers #F250C), and flows through round opening


20


(0.093″ dia. hole). Ejecting from opening


20


, the product impinges on surface


30


of coupling


12


, and then flows in a random turbulent pattern inside a generally cylindrical cavity


32


, which is formed between couplings


10


and


12


.




Thus, from virtually zero velocity in the axial direction in cavity


32


, the product is accelerated to a velocity exceeding 500 ft/sec upon entering orifice


34


. This sudden acceleration which occurs simultaneously with a severe pressure drop causes cavitation in the orifice. Being a one piece metallic nozzle, coupling


12


is suitable for relatively low pressure applications in the range of 500 psi to 15,000 psi of liquid—liquid emulsions. Applications requiring higher pressure, or which contain solids, require a 2-piece nozzle assembly as shown in FIG.


6


. The diameter of orifice


34


determines the maximum attainable pressure for any given flow capacity. For example a 0.015 in. diameter hole will enable 10,000 psi with a flow rate of 1 liter/min. of water. More viscous products require an orifice as large as 0.032 in. diameter to attain the same pressure and flow rate, while smaller systems with pumps' capacity under 1 liter/min, require an orifice as small as 0.005 in. diameter to attain 10,000 psi. The high velocity jet is ejected from orifice


34


into an absorption cell cavity


38


, the flow pattern of which is shown in FIG.


8


. An alternate absorption cell is shown in FIG.


9


.




Referring now to

FIG. 8

, water jet


35


formed in orifice


34


is maintained essentially unchanged as it flows through opening


36


of the absorption cell. After impacting surface


40


, which may be flat or semi-spherical, or have another configuration otherwise enhancing its function, the jet fluid reverses its flow direction, and forms a coherent cylindrical flow stream


37


. The cylindrical flow pattern is formed because that is the only way for the fluid to exit cavity


38


. With opening


36


only slightly larger than orifice


34


, fluid stream


37


is forced to react with the jet fluid


35


, thereby absorbing the kinetic energy of the jet fluid, generating intense forces of shear and cavitation, and minimizing the wear effect of the jet impacting on surface


40


. The intensity of energy input into the product is much lower in cavity


38


than in orifice


34


. Rather than further breaking down oil droplets, the interaction of the two streams in cavity


38


serves to provide sufficient time for the emulsifier to interact with the oil droplets formed in orifice


34


and completely surround them, thereby maintaining the oil droplets at the same small size achieved in orifice


34


and preventing their agglomeration. The absorption cell provides a controllable environment for the interaction to occur, depending on the diameter of the bore, the shape of the impact surface at the end of the cell, the length of the cell, and other design factors.




Cavity


38


is formed inside stem


42


, which is threaded into outlet coupling


16


(FIG.


4


). After exiting the cavity


38


, product flows between surface


44


of stem


42


and corresponding surface


46


in coupling


14


. The annular opening between surfaces


44


and


46


is adjusted by turning stem


42


in or out of coupling


16


, thereby controlling the back-pressure in cavity


38


. Stem


42


is provided with two flats to facilitate screwing it into coupling


16


, and with a lock-nut


48


for locking stem


42


in place. Port


50


is provided in coupling


14


for connection to a suitable cooling fluid supply. Cooling fluid flows through opening


52


and passes around “O”-ring


54


, which acts as a check-valve to prevent product flow to the cooling system. The cooling fluid then flows through a narrow annular opening formed between the tip of coupling


16


and surface


56


of coupling


14


, into cavity


58


. Thus, in cavity


58


, an annular flow sheet of cooling fluid interacts with an annular fluid sheet of hot emulsion, the two sheets flowing in opposite directions, thereby effecting intimate mixing and instantaneous cooling of the emulsion. The cooling fluid may be a compatible liquid or gas. For example, for oil-in-water emulsions, cold water may be used. In this case, the feed stock supplied to port


18


must contain a lower percentage of water, and the desired final oil/water ratio is accomplished by injecting the appropriate amount of cold water through port


50


. Alternatively, gas may be used as a cooling fluid. For example, compressed air or nitrogen may be supplied to port


50


under pressure, to be injected into cavity


58


, where the gas expansion from its compressed state requires heat absorption, thereby effecting instantaneous cooling of the hot emulsion. In this case, the air or nitrogen are released to atmosphere after the emulsion exits the emulsifying cell. From cavity


58


, the emulsion flows through annular opening


60


, to outlet port


62


which is a ¼″ H/P type. After exiting the emulsifying cell, the emulsion flows through a metering valve, provided to enable control of back-pressure in cavity


58


and to prevent “flashing” or sudden evaporation of liquid ingredient before temperature reduction.




In the example of a more elaborate emulsifying cell shown in

FIG. 5

, multiple product inlet ports and multiple orifices are used. Couplings


10


and


12


are connected as described with respect to

FIGS. 3 and 4

. Couplings of the kind identified as


13


A and


13


B are provided to enable injection of other product ingredients through ports


72


and


74


, which are ¼″ H/P type, similar to port


18


. Coupling


13


may be installed before or after coupling


12


, or before or after coupling


15


, in conjunction with one or more orifices, all depending on the particular product characteristics and the desired results. Nozzle adapter


70


is provided to enable high-pressure sealing between couplings


12


and


13


A. Coupling


13


may be connected to another coupling


13


or to coupling


14


without any adapters. Coupling


15


contains a 2-piece nozzle assembly. Nozzle adapter


84


enables high-pressure sealing between the two orifice pieces


80


and


82


, as well as between the 2-piece nozzle assembly and the coupling down-stream.




The product's continuous phase, water for example, is fed at high pressure through port


18


and then forced through orifice


34


, thereby forming a water jet. Another ingredient, oil for example, is fed through port


72


at an appropriate pressure and temperature. The required oil pressure is a function of inlet water pressure at


18


, the size of the orifice


34


, and the size of the orifice formed by members


80


and


82


. For example, using water pressure of 20,000 psi at


18


, orifice of 0.015 in. dia. at


34


, and round orifice of 0.032 in. dia. by members


80


and


82


, then water pressure between the two orifices is slightly below 4,500 psi, and thus oil pressure of 4,500 is required at port


72


to assure oil flow into the emulsifying cell. At the interface between the water phase and oil phase, cavitation takes place due to hydraulic separation, effecting a homogeneous oil in water mixture at the exit of coupling


13


A. The orifice formed between members


80


and


82


causes further break down of oil droplets, due to the severe acceleration with simultaneous pressure drop and due to orifice geometry. After this intense energy input, another product ingredient is added through port


74


, for example emulsifier, which interacts with the process jet in a manner similar to the interaction between oil and water described above. The required feed pressure at port


74


is determined by the adjustment of stem


42


, and will be generally in the range of 50 psi to 500 psi. This relatively low feed pressure enables use of ingredients that are difficult or impossible to pump with the high pressure process pump. For example, extremely viscous products and abrasive solids which would cause rapid wear to the plunger seals and check-valves of the high pressure pump, could be supplied to port


74


with standard industrial pumps. Port


74


may be also used for feeding melted polymers or resins, to be emulsified in liquid state into water, thereby replacing a common use of VOC's.




In the two different two-piece nozzle arrangements shown in

FIG. 6

, the orifice is formed as an open groove on the face of each nozzle member, thereby enabling fabrication of intricate orifice geometries and facilitating coating with suitable materials. For example, when members


80


and


82


are pressed together, they form a rectangular cross section orifice, with surfaces


86


and


88


of member


82


being optically flat (within 1 light band), forming a pressure containing seal with the corresponding surfaces of member


80


. Surface


90


forms a step along the flow path in the orifice and serves to induce cavitation. The location of surface


90


along the orifice may be chosen to induce cavitation at the entrance of the orifice or at its exit, depending on the configuration of the emulsifying cell. Additionally, various slope angles of surface


90


and of the step formed after it may be used to control the rate of cavity formation and collapse, all depending on the product characteristics and desired results. The nozzle assembly made of members


92


and


94


will be essentially the same as a round hole in a solid block, but the two-piece construction allows coating of the inner surface the extremely small orifice with materials such as diamond, thereby enabling continuous production of abrasive products at high pressure. Such a scheme would be useful for producing small solid particles of materials such as ceramics or iron-oxide for magnetic media.




As seen in

FIG. 5

, the two nozzle members


80


and


82


are inserted into a bore in a nozzle adapter


84


. The nozzle adapter is shown in greater detail in

FIGS. 7A and 7B

. Upon fastening the emulsifying cell assembly, the two nozzle members


80


and


82


are forced against surface


190


of adapter


84


, while the adapter tapered sealing surface


188


is forced against the adjacent coupling (


13


B in FIG.


5


). The axial compressive force on surface


188


has an inward radial component, which is transmitted through surface


186


to the two nozzle members


80


and


82


, thereby effecting a pressure containing seal between the members


80


and


82


. Slots


194


and


196


are provided to facilitate the translation of axial compression to radial compression of adapter


84


. Round hole


192


is provided for product flow.




In the example of a more elaborate absorption cell shown in

FIG. 9

, the length of the cell and its effective internal diameter may be varied. Stem


242


has the same external dimensions as stem


42


in

FIGS. 3

,


4


and


5


, thus stems


42


and


242


are interchangeable. Stem


242


is provided with a smooth internal bore


238


at one end, internal threads at the other end, and a tapered sealing surface


208


in between. Nozzle insert


200


is fitted into the stem bore


238


, secured by such means as press-fitting or adhesive material, to form the cavity opening


236


. The use of inserts with a variety of lengths, internal surface geometry and size, enables control of the shear rate, cavitation, turbulence, and the impact at surface


240


. Rod


202


is inserted into stem


242


to provide the impact surface


240


of the absorption cell. The depth of cavity


238


, as determined by the positioning of rod


202


, controls the residence time of product in the absorption cell, which in turn enables providing sufficient interaction time between emulsifier and oil droplets. Sleeve


204


is provided to lock rod


202


in place, as well as to provide sealing between rod


202


and stem


242


. Once the location of rod


202


is selected, sleeve


204


is tightened. Tapered sealing surface


206


of sleeve


204


is then pressed against tapered sealing surface


208


of stem


242


, thereby forming a seal between sleeve


204


and stem


242


, as well as between sleeve


204


and rod


202


. Graduation marks at the exposed end of rod


202


facilitate accurate positioning of the rod and provide a convenient scale for recording.




The two absorption cell assemblies in

FIGS. 10 and 11

exemplify a large variety of ways to accommodate particular product requirements. Nozzle inserts


300


,


302


A,


302


B and


304


are examples of a large variety of inserts that may be used. The generally concave internal opening of insert


300


induces cavitation when fluid enters cavity


306


. The fluid immediately near surface


308


will flow along a path defined by that surface, tending to separate form the flow path defined by the previous surface


310


. With simultaneous pressure drop resulting from the larger cross-section area of cavity


306


, cavitation occurs. The generally convex internal opening of insert


304


(

FIG. 11

) induces cavitation in the fluid stream upon exiting the insert. Fluid pressure is increased momentarily when fluid passes through the center of insert


304


. As in insert


300


, the fluid's tendency to follow the shape of the solid surface with a simultaneous pressure drop induces cavitation. Inserts


302


A and


302


B are identical and are arranged to achieve desired results for a particular product. Several identical inserts such as


302


may be used together, end-to-end, to form one continuous internal bore. Alternatively, several inserts with different internal diameters may be used to induce turbulence in the exiting fluid stream. Yet another alternative, shown in

FIG. 10

, is to leave a small space between the inserts to disrupt laminar flow and generate turbulence. Yet another alternative is to use several inserts such as


300


and/or


304


in series. In

FIG. 11

, reflecting surface


440


exemplifies a large variety of shapes that may be used to enhance its function or for a particular application. As compared with semi-spherical or flat reflecting surfaces, surface


440


has a much larger surface area reflecting the jet fluid. Such a scheme may be used to effect a more gradual flow reversal, and for abrasive solids applications for extending the service life of the reflecting surface.




The coil shown in

FIGS. 12A through 12C

is used for removing pressure fluctuations (item


132


in FIGS.


1


and


2


). The coil is made of standard high pressure tubing (E.g., Butech ¼″ M/P, #20-109-316), with coil diameter sufficiently large as not to effect significantly the pressure rating of the tubing (e.g., 4 in.), and of sufficient length to remove the pressure spikes (e.g, 60 ft.). The tubing expands slightly when the pump generates a pressure spike, thereby acting to absorb the excess energy generated by the pressure spike. At the end of the pressure spike, the tubing contracts, thereby releasing the stored energy. This action of the coil is similar to the action of standard hydraulic accumulators that are used in hydraulic systems for essentially the same purpose. Waterjet cutting systems employ similar principle (e.g. Flow International Corp.'s “Attenuator”), in the form of a long straight cylinder between the high pressure intensifier pump and the nozzle, for generating constant flow rate through the nozzle. As can be seen in

FIGS. 12A through 12C

, the tubing is coiled in a way that allows each coil ring to flex in response to pressure fluctuations, in a similar action of a Bourdon tube (used in pressure gauges). Because the external side of each coil ring has a larger area than the internal side, pressure in the tubing tends to open each ring. This movement in response to pressure fluctuations provides another mechanism for absorbing and releasing energy. The coil thus provides means for removing pressure fluctuations, heating or cooling the product, while being suitable for CIP/SIP sterile systems.

FIG. 13

illustrates a scheme for connecting several coils such as in

FIGS. 12A through 12C

, enabling the use of standard tubing length (e.g. 20 ft.) and standard bending tools to produce coils as long as necessary.




Other embodiments are within the scope of the following claims.



Claims
  • 1. A method for use in causing emulsification of a first fluid component within a second fluid component, comprisingproviding a supply of the first fluid component in a cavity wherein the first fluid is essentially stagnant, and directing a jet of the second fluid component into the first fluid component, the velocity of the jet being chosen to cause cavitation due to hydraulic separation at an interface between the two fluids, wherein the first fluid component is different from the second fluid component.
  • 2. The method of claim 1 wherein the second fluid component comprises a continuous phase of an emulsion or dispersion.
  • 3. The method of claim 1 wherein the first fluid component comprises a discontinuous phase in the emulsion.
  • 4. The method of claim 1 wherein the first fluid component comprises a solid discontinuous phase in the dispersion.
  • 5. The method of claim 1 wherein the supply of the first fluid is provided in an annular chamber, and the jet is delivered from an outlet of an orifice which opens into the annular chamber.
  • 6. The method of claim 1 further comprisingafter the emulsification by hydraulic separation, passing the product through an orifice to cause additional emulsification.
  • 7. The method of claim 1 comprising controlling the temperature of the first or second fluid.
  • 8. The method of claim 1 further comprisingfollowing the emulsification by hydraulic separation, delivering the product to a subsequent processing chamber.
  • 9. The method of claim 8 wherein an additional component is added to the emulsion in the subsequent processing chamber.
  • 10. The method of claim 8 wherein a cooling fluid is applied to the product in the subsequent processing chamber to quickly cool and stabilize the emulsion.
  • 11. The method of claim 8 wherein the subsequent processing chamber is an absorption cell into which a jet of the product is directed.
  • 12. The method of claim 8 wherein said absorption cell is an elongated cell including a wall surface shaped to vary localized pressure conditions within the cell.
  • 13. The method of claim 8 or 12 wherein the absorption cell comprises an elongated cell having a reflective surface defining an end thereof.
CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation and claims the benefit of priority under 35 USC 120 of U.S. application Ser. No. 08/920,042, filed Aug. 28, 1997, now abandoned, which, in turn, is a continuation and claims the benefit of priority under 35 USC 120 of U.S. application Ser. No. 08/330,448, filed Oct. 28 1994 now U.S. Pat. No. 5,720,551, the entire contents of both of which are hereby incorporated by reference.

US Referenced Citations (44)
Number Name Date Kind
1496858 Knollenberg Jun 1924 A
1593762 Heitmann Jul 1926 A
1926484 Hoffmann Sep 1933 A
2068136 Hulbert Jan 1937 A
2584805 Leftwich Feb 1952 A
2705620 Borck Apr 1955 A
2882025 Loo Apr 1959 A
3153578 Taylor Oct 1964 A
3459407 Hazlehurst et al. Aug 1969 A
3476521 Wise Nov 1969 A
3807632 Johnson, Jr. Apr 1974 A
3852013 Upmeier Dec 1974 A
3883121 Guillaud May 1975 A
3941355 Simpson Mar 1976 A
3941552 Cottell Mar 1976 A
3965975 Edmundson Jun 1976 A
4081863 Rees Mar 1978 A
4087862 Tsien May 1978 A
4124309 Yao Nov 1978 A
4159881 Gogneau Jul 1979 A
4299498 Sauerbrunn Nov 1981 A
4337161 Stayner Jun 1982 A
4440500 Schneider Apr 1984 A
4452917 Proksa et al. Jun 1984 A
4533254 Cook et al. Aug 1985 A
4568003 Sperry et al. Feb 1986 A
4597671 Marelli Jul 1986 A
4701055 Anderson Oct 1987 A
4723715 Mazurkeiwicz Feb 1988 A
4908154 Cook et al. Mar 1990 A
4944602 Buschelberger Jul 1990 A
4996004 Rucheler et al. Feb 1991 A
5035362 Mazurkiewicz Jul 1991 A
5086982 Hirano et al. Feb 1992 A
5147412 Klinksiek et al. Sep 1992 A
5279463 Holl Jan 1994 A
5289981 Kamiwano et al. Mar 1994 A
5366287 Verstallen Nov 1994 A
5720551 Shechter Feb 1998 A
5765766 Yoshida et al. Jun 1998 A
5843334 Saheki et al. Dec 1998 A
5931771 Kozyuk Aug 1999 A
6106145 Winslow Aug 2000 A
6502979 Kozyuk Jan 2003 B1
Foreign Referenced Citations (10)
Number Date Country
166 309 Aug 1904 DE
0 568 070 Mar 1993 EP
0 770 422 May 1997 EP
539016 Mar 1922 FR
26582 Aug 1971 JP
56-172325 May 1980 JP
56-158136 Dec 1981 JP
51 135 878 Nov 1996 JP
WO 86 02577 May 1986 WO
WO 9535157 Dec 1995 WO
Non-Patent Literature Citations (5)
Entry
Premier Mill, “The Reversible Emulsifier”, brochure (1 pp), No date.
Schubert et al., “Principles of Formation and Stability of Emulsions”, Internationial Chemical Engineering, vol. 32, No. 1, Jan., 1992, pp. 14-28, Federal Republic of Germany.
APV Gaulin Brochure, pp. 2-11. No date.
Takamura et al., “The Influence of Cooling Rate on Emulsion Stability”, Translation of Japanese Article, Presented at 101st Japan Pharmaceutical Academy Conference at Kumamoto, Apr., 1981.
Jeffries et al., “Thermal Equilibration During Cavitation”, Science, Apr. 10, 1992, vol. 256, No. 5054, p. 248.
Continuations (2)
Number Date Country
Parent 08/920042 Aug 1997 US
Child 10/223956 US
Parent 08/330448 Oct 1994 US
Child 08/920042 US