MXPA97003100A - Emulsion formation - Google Patents
Emulsion formationInfo
- Publication number
- MXPA97003100A MXPA97003100A MXPA/A/1997/003100A MX9703100A MXPA97003100A MX PA97003100 A MXPA97003100 A MX PA97003100A MX 9703100 A MX9703100 A MX 9703100A MX PA97003100 A MXPA97003100 A MX PA97003100A
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- Prior art keywords
- fluid
- emulsion
- coupling
- jet
- emulsification
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Abstract
The present invention relates to a method for causing emulsification comprising: delivering a coherent jet of fluid having a velocity greater than 152.4 meters per second, providing a second coherent flow fluid, and in a chamber, directing the coherent jet and the coherent flow along trajectories that maintain a boundary between the jet and the coherent flow so that it produces shear stress, and therefore mixed, at the border
Description
EMULSION FORMATION
BACKGROUND This invention relates to the formation of 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, the emulsifying agents, known as emulsifiers or surfactants, serve to stabilize the emulsions and facilitate their formation, surrounding the droplets in the oil phase, and separating them from the water phase. The uses of emulsions have been increasing for many years. Most processed food and beverage products, medical and personal care products, paints, inks, tints, and photographic media are emulsions or emulsions. In recent years, the demand for emulsions with smaller and more uniform droplets has increased. The applications of artificial blood, for example, require almost uniform droplets that average 0.2 microns. Inkjet printing has similar requirements for size and distribution.
High-pressure homogenizers are often used to produce small and uniform droplets or particles, which employ a device that is commonly referred to as a 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 previously mixed crude emulsion is fed at a high pressure, generally between 70 and 1,050 kg / cpr, towards the center of the valve seat. When the fluid pressure exceeds the force closing the valve, a narrow annular gap (10 to 200 microns) is opened between the valve seat and the valve plug. The crude emulsion flows through it, suffering a rapid acceleration, as well as a sudden drop in pressure, which breaks the oil phase into small droplets. More recently, a new type of high pressure homogenizer was introduced, which uses two or more fixed orifices, and which is capable of reaching 2,800 kg / cm2. When forced through these orifices, the crude emulsion previously mixed forms jets of liquid that make each other impact. A description is found in the Patents of the United States of North America Nos. 4,533,254 and 4,908,154. The typical mechanism for emulsification in this type of device is the controlled use of shear stress, impact, and cavitation forces in a small area. The relative effects of these forces generally depend on fluid characteristics, but in the vast majority of emulsion preparation schemes, cavitation is the dominant force. The tearing of the fluid is created by differential velocity within the fluid stream, generated by the sudden acceleration of the fluid entering the orifice or small gap, by the difference between the extremely high velocity at the center of the orifice, and the zero velocity. in the surfaces that define the hole, and by the intense turbulence that occurs after leaving the hole. Cavitation occurs when the pressure falls momentarily below the vapor pressure of the water phase. Small bubbles of vapor form, and then collapse (within 10-3 to 10-9 seconds), generating shock waves that break the surrounding oil droplets. Cavitation occurs in the homogenizing valves when the sudden acceleration in the orifice, with a simultaneous drop in pressure, causes the local pressure to fall momentarily below the vapor pressure. More generally, it has come to be known that cavitation occurs when two surfaces separate faster than some critical speed, and those cavitation bubbles affect their surroundings only during the emulsion ingredients and the processing pressure , as well as accelerates the speed of agglomeration of the droplets after the emulsification process. Some processes require very small solid polymer or resin particles; and this is often done by dissolving the polymers or the solid resins in volatile organic compounds (VOC), and then using mixing equipment to reduce the size of the droplets, and finally removing the volatile organic compounds.
SUMMARY In general, in one aspect the invention provides 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 controlled flow along a new path, orienting itself in the first trajectory and the new trajectory to cause tearing and cavitation in the fluid. The implementations of the invention may include the following features. The first trajectory and the new trajectory can be oriented in essentially opposite directions. The coherent flow can be a cylinder surrounding the jet. The formation of the cavities, and not during the collapse of the cavities, as it had assumed for a long time. Another discovery of interest is that cavitation can occur either entirely within the liquid, or at the solid-liquid interfaces, depending on the relative strength of solid-liquid adhesion and the cohesion of liquid-1-liquid. Typical emulsification schemes have several characteristics that should be noted. Cavitation occurs only once, for a very short time (10-3 to 10-9 seconds), and equipment that employs a high energy density imparts emulsification energy to only a very small portion of the product at any given time . The emulsification process is thus highly sensitive to the uniformity of the feedstock, and several passes are usually required through the equipment before the desired average droplet size and uniformity are achieved. The size of the final droplet depends on the interaction speed of the surfactant with the oil phase. Because the surfactants generally can not surround the oil droplets at the same rate at which they are being formed by the emulsification process, agglomeration takes place, and the average droplet size is increased. There is a typical acute increase in the temperature of the product during the process, which limits the choice of the interposed structure may have a reflecting surface that is generally hemispherical, or that is generally thinned, and that remains at the end of a well. Adjustments can be made to the pressure in the well, in the distance from the opening of the well to the reflecting surface, and the size of the opening to the well. The controlled flow, as it leaves the well, can be directed in an annular sheet away from the opening of the well. An annular flow of a refrigerant can be directed in a direction opposite to the direction of the annular sheet. An additional component can be flowed into the space adjacent to the reflecting surface, and generally in the direction of the new flow path controlled. In general, in another aspect, the invention provides a method for use in the stabilization of a hot emulsion immediately after its 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 emulsion flow and in sufficiently close proximity to exchange heat with the emulsion flow. The implementations of the invention may include the following features. The emulsion can 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 the emulsion. The cooling fluid may be a liquid or a gas compatible with the emulsion. The fluids of the emulsion and the cooling fluid can be presented in an annular valve opening. In general, in another aspect, the invention provides a method to be used to cause emulsification of a first fluid component within a second fluid component. In the method, an essentially stagnant supply of the first fluid component in a cavity is provided. A jet of the second fluid component is directed towards the second fluid component. The temperatures and jet velocities of the fluids are selected to cause cavitation, due to the hydraulic separation at the interface between the two fluids. The 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 can be a discontinuous phase in the emulsion, for example, a solid discontinuous phase. The second fluid can be provided in an annular chamber, and the jet can be applied from an outlet of an orifice opening to the annular chamber. After emulsification by hydraulic separation, the product can be passed through a hole to cause additional emulsification, or it can be applied to a subsequent processing chamber, where an additional component can be added to the emulsion. A cooling fluid may be applied to the product in the subsequent processing chamber to cool and quickly stabilize the emulsion. The subsequent processing chamber may be an absorption cell towards which a product jet is directed. In general, in another aspect, the invention provides an apparatus for reducing pressure fluctuations in an emulsifier cell fed from a fluid line by a high pressure pump. A tube wound in the fluid line between the pump and the emulsifier cell has an internal volume, a wall thickness, a coil diameter, and a suitable coiling pattern to absorb pressure fluctuations and capable of withstanding the high pressure generated by the pump. The apparatus may include a cover around the coiled tube with gates to fill the cover with heating or cooling fluid. In general, in another aspect, the invention provides a nozzle for use in an emulsification structure. In the structure, two body parts that have flat surfaces are formed to form the nozzle, at least one of the members having a groove to form a hole in the nozzle. The surfaces are sufficiently flat, such that, when the two body parts are pressed together with sufficient force, the flow of fluid to the orifice is confined. In the implementations of the invention, the cavitation inducing surfaces can be defined on the groove; and a wall of the groove can be coated with diamond or non-polar materials or polar materials. In general, in another aspect, the invention provides an absorption cell for use in an emulsification structure. The cell includes an elongated chamber having an open end for receiving a fluid jet having two immiscible components. A reflecting surface is provided at the other end of the chamber to reflect the jet. And a mechanism is provided to adjust the distance from the reflecting surface to the open end. The implementations of the invention may include the following features. The reflective surfaces can be interchangeable for different applications. There may be a removable insert for inserting into the chamber at the open end, the insert having a hole one dimension smaller 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 provides a modular emulsification structure comprising a series of couplings that can be adjusted to each other 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, to communicate the fluid from an upstream coupling to a downstream coupling. Gates are provided to feed fluid to, or withdraw fluid from, the coupling. When at least some of the communication openings are small enough to form a jet of liquid. The sealing surfaces are sufficiently smooth to provide a fluid-tight seal when the couplings are stopped from each other by a sufficient compression force directed along the length of the structure. The implementations of the invention may include the following features. A processing chamber can be defined between the male sealing surface of one of the upstream couplings and the female sealing surface of one of the downstream couplings. In some of the couplings, the hole may extend from one end of the coupling to the other. An absorption cell coupling can be used in one of the structures. One of the couplings may extend into another coupling to form a small annular opening to generate an annular flow sheet of cooling fluid. Some of the couplings of the couplings are used for cleaning and / or sterilization procedures of CIP / SIP. In general, in another aspect, the invention provides an emulsification structure having a coupling and an orifice support containing an emulsification orifice having two ends that open to other components of the structure. The orifice support is mounted on the coupling to allow rotation of the support, to reverse the locations of the two ends, each end serving as an entrance or an exit towards the orifice, depending on their locations. The advantages of the invention include the following. Liquid droplets or very small solid particles can be processed in the course of the emulsification, mixing, suspension, dispersion, or deagglomeration of solid and / or liquid materials. Droplets or particles are produced in almost uniform submicrons. The process is uniform over time, because the pressure peaks that are normally generated by the high pressure pump are eliminated. A wider range of types of emulsion ingredients can be used, while their effectiveness is maximized by their separate introduction into the high-velocity fluid jet. Thin emulsions can be produced using fast reaction ingredients, by adding each ingredient separately, and by controlling the locations of its interaction. The control of the temperature before and during the emulsification, allows having multiple stages of cavitation without damaging the heat-sensitive ingredients, making it possible to inject ingredients at different temperatures, and by injecting compressed air or liquid nitrogen before the emulsification step final. The effects of cavitation on the liquid stream are maximized while minimizing the effects of wear on the surrounding solid surfaces, by controlling the hole geometry, material selection, surface characteristics, pressure, and temperature. The absorption of the kinetic energy of the jet into the fluid stream is maximized, while minimizing its effect of wear on the surrounding solid surfaces. Sufficient turbulence is achieved to prevent agglomeration before the surfactants can fully react with the newly formed droplets. Agglomeration is minimized after treatment by rapid cooling, by injection of compressed air or nitrogen, and / or by rapid heat exchange, while the emulsion is subjected to sufficient turbulence to overcome the attractive forces of the oil droplets , and maintaining a sufficient pressure to prevent the water from evaporating. Upward scaling procedures from small-scale laboratory devices to large-scale production systems become simpler, because all process parameters can be carefully controlled. The invention is applicable to emulsions, microemulsions, dispersions, liposomes, and cell ruptures. A wide variety of immiscible liquids can be used, in a wider range of proportions. Smaller amounts (in some cases nothing) of 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 can be produced for various uses such as food, beverages, pharmaceuticals, paints, inks, toners, fuels, magnetic media, and cosmetics. The device is easy to assemble, disassemble, clean, and maintain. The process can be used with fluids of high viscosity, high solids content, and fluids that are abrasive and corrosive. The effect of the emulsification continues for a sufficient time for the surfactants to react with the newly formed oil droplets. The multiple cavitation stages guarantee a complete use of the surfactant with virtually no waste in the form of mycelia. Multiple gates can be used along the process stream for cooling by injecting the ingredient at a lower temperature. The volatile organic compounds can be replaced with hot water to produce the same final products. The water will be heated under high pressure to well above the melting point of the polymer or resin. The polymer or the solid resins will be injected in their solid state, to be melted and sprayed by the hot water jet. The provision of multiple gates eliminates the problematic introduction of large solid particles in high pressure pumps, and requires only conventional industrial pumps. Other advantages and features will become clearer from the following description and claims.
Description Figures 1 and 2 are block diagrams of emulsification systems. Figures 3A and 3B are an end view and a cross-sectional view (in A-A of Figure 3A) of an emulsifier cell assembly. Figure 4 is an enlarged cross-sectional view (in B-B of Figure 3A) of the emulsifier cell assembly. Figure 5 is a cross-sectional view of another modular emulsifier cell assembly. Figure 6 is an isometric view separated in parts, not to scale, of two types of a two piece nozzle assembly. Figures 7A and 7B are an enlarged end view and a cross-sectional view of an adapter for the two-piece nozzle assembly. Figure 8 is a schematic diagram in cross section, not to scale, of the fluid flow in an absorption cell. Figure 9 is a cross-sectional view of an absorption cell. Figures 10 and 11 are diagrams in cross section, not to scale, of the fluid flow in other modular absorption cell assemblies. Figures 12A, 12B, and 12C are an end view, a front view, and a top view of a coil for regulating the process pressure in the emulsifier cell. Figure 13 is a set of three coils shown in Figures 12A to 12C. Figures 14 and 15 are cross-sectional views of sets of emulsifying cells.
In Figure 1, the ingredients of the product are supplied from sources 110, 112, and 114 to a premix system llß. 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 premix system 116 is of a suitable kind (e.g., propeller mixer, colloid mill, homogenizer, etc.) for the type of product. After premixing, the ingredients are fed to the feed tank 118. In some cases, the premix can be made inside the feed tank 118. The product previously mixed from the tank 118 then flows through the line 120 and valve 122, by means of the transfer pump 124 to the high pressure process pump 128. The transfer pump 124 can be any type of pump normally used for the product, on the understanding that it can generate the pressure of power required for proper operation of the high pressure process pump. The pressure indicator 126 is provided to monitor the supply pressure to the pump 128. The high pressure process pump 128 is typically a positive displacement pump, for example, a triplex or intensifier pump.
From the process pump 128, the product flows at a high pressure through the line 130 to the coil 132, where the pressure fluctuations generated by the action of the pump 128 are regulated by the expansion and contraction of the pipeline. of the coil. A more detailed explanation of the coil mechanism is given in the description of Figures 12A to 12C. It may be desirable or necessary to heat or cool the feedstock. The heating system 148 can circulate hot fluid in the cover 154 by means of the lines 150 and 152, or the cooling system 156 can be used. The heating means can be hot oil or steam with the appropriate element to control the temperature and the flow of the hot fluid, in such a way as to obtain the desired product temperature when leaving the coil 132. The product leaves the coil 132 through the line 134, where the pressure indicator 136 and the temperature indicator 138 monitor these parameters, and enter the emulsifying cell 140 at a high and constant pressure, for example, a pressure of 1,050 kg / cm2. The emulsification process takes place in the emulsifier cell 140, wherein the feed material is forced through at least one jet generating orifice, and through an absorption cell, where the kinetic energy of the jet is absorbed by a stream of fluid flowing around the jet and into the stream. opposite direction. In each of the treatment stages (there may be more than two), the intense tearing, impact and / or cavitation forces break the oil phase into extremely small and highly uniform droplets, and allow sufficient time for the emulsifier to interact with these small droplets of oil to stabilize the emulsion. Immediately following the emulsification process, cooling fluid is injected from the cooling system 156 into the emulsion via line 158, instantly cooling the emulsion by intimately mixing the cooling fluid with the hot emulsion inside the emulsification cell 140. The refrigerant system 156 may be a cold compatible liquid source (e.g., cold water), or a compressed gas (e.g., air or nitrogen), with a suitable element for controlling the temperature, pressure, and flow of the liquid. cooling fluid, in such a way that the desired product temperature is obtained upon leaving the emulsification cell 140. The emulsion leaves the emulsification cell 140 through line 142, where the measuring valve 144 is provided to control the return pressure during cooling, and ensures that the hot emulsion remains in a liquid state while it is cooling, thereby maintaining the integrity and stability of the emulsion. Finally, the finished product is collected in tank 146.
In the system illustrated by Figure 2, the continuous phase of the product is supplied from the supply 110 to the feed tank 118, while other ingredients are supplied from the sources 112 and 114 directly to the emulsifying cell 140. Some ingredients can be Mix with each other to reduce the number of separate power lines, or there may be as many power lines as ingredients in the product. The water from the tank 118 flows through the line 120 and the valve 122, by means of the transfer pump 124 to the pump of the high pressure process 128. Elements 128 to 138, and 148 to 158, have similar functions to the same numbered elements of the system of Figure 1. The oil and the emulsifier, each representing a possibly unlimited number and a variety of ingredients that can be introduced separately, flow from the sources 112 and 114 to the 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 the introduction pumps 166 and 168. The introduction pumps 166 and 168 are suitable for the type of product pumped, (for example, sanitary cream, injectable suspension, abrasive paste), and the flow and pressure ranges required. For example, in small-scale systems, peristaltic pumps are used, while in the production system and / or for high-pressure injection, diaphragm or gear pumps are used. Inside the emulsifying cell 140, water is forced through a hole, creating a jet of water. Other ingredients of the product, as exemplified by the oil and the emulsifier, are injected into the emulsifying cell 140. The interaction between the water jet at an extremely high speed inside the emulsifying cell 140 and the stagnant ingredients from lines 162 and 164, subject the product to a series of treatment stages, in each of which the intense forces of tearing, impact and / or cavitation, break the oil and the emulsifier to extremely small and highly uniform droplets, and gives sufficient time for that the emulsifier interacts with the oil droplets. Immediately following the emulsification process, the emulsion cools and then leaves the emulsification cell, and is collected, all in a manner similar to that employed in the system of Figure 1. As seen in Figures 3 to 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 containment unit, forcing together a smooth and thinned sealing surface of each coupling on a corresponding smooth and thin sealing surface of the adjacent coupling, to create a metal-to-metal seal, in a manner very similar to the seal between a standard high pressure nipple and the corresponding female gate. Each coupling (with the possible exception of the end couplings) has a large hole on one side, and a coupling protrusion of a slightly smaller diameter on the other side, such that the protrusion of each coupling fits on the other side. hole of the next coupling, thus aligning the sealing surfaces, and facilitating the assembly of a large number of couplings. The couplings are held together by four screws. In the example of a basic emulsifier cell shown in Figures 3A and 3B, the cell assembly has four couplings: the product inlet coupling 10, the nozzle coupling 12, the coolant inlet coupling 14, and the coupling of product outlet 16. Referring also to Figure 4, the protrusion 26 of the coupling 10 fits into the hole 28 of the coupling 12, while the sealing surface 22 of the coupling 10 is aligned with the sealing surface 24 of the coupling 12, to form a metal-metal seal containing pressure when holding the assembly with four screws 17. The fluid product to be processed enters the emulsifier cell from gate 18, which is a standard 6.35 millimeter H / P gate (eg, Autoclave Engineers # F250C), and flows through round opening 20 (2.362 millimeter diameter orifice). Expelling from the opening 20, the product impacts on the surface 30 of the coupling 12, and then flows in a random turbulent pattern into a generally cylindrical cavity 32, which is formed between the couplings 10 and 12. Consequently, from a speed virtually zero in the axial direction in the cavity 32, the product accelerates to a velocity exceeding 152.4 meters per second as it enters the orifice 34. This sudden acceleration that occurs simultaneously with a severe pressure drop causes cavitation in the orifice. Being a one-piece metal nozzle, the coupling 12 is suitable for relatively low pressure applications in the range of 35 kg / cm2 to 1,050 kg / cm2 of liquid-liquid emulsions. Applications that require a higher pressure or that contain solids, require a two-piece nozzle assembly as shown in Figure 6. The diameter of the orifice 34 determines the maximum pressure that can be obtained for any given flow capacity. . For example, an orifice of 0.381 millimeters in diameter will make it possible to have 700 kg / cpr with a flow rate of 1 liter per minute of water. The more viscous products require a hole as large as 0.8128 millimeters in diameter to obtain the same pressure and flow velocity, while the smaller systems with a pump capacity of less than 1 liter per minute, require a hole as small as of 0.127 millimeters in diameter to obtain 700 kg / cpr. The high velocity jet is ejected from the orifice 34 into a cavity of the absorption cell 38, whose flow pattern is shown in Figure 8. An alternative absorption cell is shown in Figure 9. Referring now to Figure 8, the water jet 35 formed in the orifice 34 remains essentially unchanged as it flows through the opening 36 of the absorption cell. After impacting the surface 40, which may be flat or hemispherical, or may have another configuration that improves its function, the fluid jet reverses its direction of flow, and forms a coherent cylindrical flow stream 37. The cylindrical flow pattern is form because it is the only way for the fluid to exit the cavity 38. With the opening 36 only slightly larger than the orifice 34, the fluid stream 37 is forced to react with the fluid jet 35, absorbing this way the kinetic energy of the fluid jet, generating intense tearing and cavitation forces, and minimizing the effect of wear of the jet impacting on the surface 40. The intensity of the energy input in the product is much lower in the cavity 38 that in the hole 34. In addition to breaking the oil droplets, the interaction of the two streams in the cavity 38 serves to provide sufficient time for the emulsion nante interact with the oil droplets formed in the hole 34, and surround them completely, thus maintaining the oil droplets in the same small size reached in the hole 34, and preventing their agglomeration. The absorption cell provides a controllable environment for the interaction to occur, depending on the diameter of the hole, the shape of the impact surface at the end of the cell, the length of the cell, and other design factors . The cavity 38 is formed inside the rod 42 which is screwed into the outlet coupling 16 (Figure 4). After leaving the cavity 38, the product flows between the surface 44 of the rod 42 and the corresponding surface 46 of the coupling 14. The annular opening between the surfaces 44 and 46 is adjusted by rotating the rod 42 in or out of the coupling 16, thereby controlling the pressure back in the cavity 38. The rod 42 is provided with two planes to facilitate its screwing into the coupling 16, and with a lock nut 48 to secure the rod 42 in place. The gate 50 is provided in the coupling 14 to be connected to a suitable coolant supply. The cooling fluid flows through the opening 52, and passes around the "0" ring 54, which acts as a check valve, to prevent the product from flowing into the cooling system. Then the cooling fluid flows through a narrow annular opening formed between the tip of the coupling 16 and the surface 56 of the coupling 14, towards the cavity 58. Accordingly, in the cavity 58, an annular flow sheet of cooling fluid interacts with a sheet of hot emulsion annular fluid, the two sheets flowing in opposite directions, thereby effecting intimate mixing and instantaneous cooling of the emulsion. The refrigerant fluid can be a compatible liquid or gas. For example, for oil-in-water emulsions, cold water can be used. In this case, the feed material supplied to the gate 18 must contain a lower percentage of water, and the desired final oil / water ratio is realized by injecting the appropriate amount of cold water through the gate 50. In an alternative way, the gas can be used as the cooling fluid. For example, compressed air or nitrogen can be supplied to the gate 50 under pressure, to be injected into the cavity 58, where expansion of the gas from its compressed state requires heat absorption, thereby effecting instantaneous cooling of the emulsion hot. In this case, air or nitrogen is released into the atmosphere after the emulsion leaves the emulsifier cell. From the cavity 58, the emulsion flows through the annular opening 60, to the outlet gate 62, which is of a H / P type of 6.35 millimeters. After leaving the emulsifier cell, the emulsion flows through a metering valve, provided to make possible in control of the back pressure in the cavity 58, and to prevent "evaporation", or sudden evaporation of the liquid ingredient before the reduction of temperature. In the example of a more elaborate emulsifier cell shown in Figure 5, multiple product inlet gates and multiple orifices are used. The couplings 10 and 12 are connected as described with respect to Figures 3 and 4. The couplings of the class identified as 13A and 13B are provided to make it possible to inject other ingredients of the product through the gates 72 and 74 , which are of the H / P type of 6.35 millimeters, similar to the gate 18. The coupling 13 can be installed before or after coupling 12, or before or after the coupling 15, in conjunction with one or more holes, all depending on the particular characteristics of the product and the desired results. The nozzle adapter 70 is provided to enable a high pressure seal between the couplings 12 and 13A. The coupling 13 can be connected to another coupling 13 or to the coupling 14 without adapters. The coupling 15 contains a 2 piece nozzle assembly. The nozzle adapter 84 enables high pressure sealing between the two hole pieces 80 and 82, as well as between the 2 piece nozzle assembly and the downstream coupling. The continuous phase of the product, water for example, is fed at a high pressure through the gate 18, and then forced through the orifice 34., thus forming a jet of water. Another ingredient, oil for example, is fed through the gate 72 at an appropriate pressure and temperature. The required oil pressure is a function of the inlet water pressure at 18, the size of the orifice 34 and the size of the hole formed by the members 80 and 82. For example, using a water pressure of 1,400 kg / cm2 at 18, a hole of 0.381 millimeters in diameter in 34, and a round hole of 0.8128 millimeters in diameter through members 80 and 82, then the water pressure between the two holes is slightly less than 315 kg / cm2, and therefore, An oil pressure of 315 kg / cm2 is required in gate 72, to guarantee an oil flow to the emulsifier cell. At the interface between the water phase and the oil phase, the cavitation takes place due to the hydraulic separation, effecting a homogeneous mixture of oil in water at the outlet of the coupling 13A. The hole formed between the members 80 and 82 causes another breakdown of the oil droplets, due to the severe acceleration with the simultaneous pressure drop, and due to the geometry of the hole. After this intense input of energy, another ingredient of the product is added through the gate 74, for example emulsifier, which interacts with the jet of the process in a manner similar to the interaction between the oil and the water described above. The feed pressure required in the gate 74 is determined by the adjustment of the rod 42, and will generally be in the range of 3.5 kg / cm2 to 35 kg / cm2. This relatively low feed pressure makes it possible to use ingredients that are difficult or impossible to pump with the high pressure process pump. For example, extremely viscous products and abrasive solids that would cause rapid wear to the piston seals and check valves of the high pressure pump could be supplied to the gate 74 with conventional industrial pumps. The gate 74 can also be used to feed molten polymers or resins, to emulsify in the liquid state in water, thus replacing a common use of the volatile organic compounds. In the two different two-piece nozzle configurations shown in Figure 6, the hole is formed as an open groove on the face of each nozzle member thereby making possible the fabrication of intricate orifice geometries, and facilitating the coating with suitable materials For example, when the members 80 and 82 are compressed together, they form a hole of rectangular cross-section, the surfaces 86 and 88 of the member 82 being optically flat (within a band of light), forming a seal containing pressure with the corresponding surfaces of member 80. Surface 90 forms a step along the flow path in the hole, and serves to induce cavitation. The location of the surface 90 along the orifice may be selected to induce cavitation at the inlet of the orifice or its outlet, depending on the configuration of the emulsifier cell. Additionally, different inclination angles of the surface 90 and the step formed after it can be used to control the speed of cavity formation and collapse, all depending on the characteristics of the product and the 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 the internal surface of the extremely small orifice with materials such as diamond, thus making it possible continuous production of abrasive products at high pressure. This scheme will be useful to produce small solid particles of materials such as ceramic or iron oxide for magnetic media. As seen in Figure 5, the two nozzle members 80 and 82 are inserted into a hole in a nozzle adapter 84. The nozzle adapter is shown in greater detail in Figures 7A and 7B. By clamping the emulsifier cell assembly, the two nozzle members 80 and 82 are forced against the surface 190 of the adapter 84 while the thinned sealing surface 188 of the adapter is forced against the adjacent coupling (13B of Figure 5). The axial compression force on the surface 188 has a radially inward component, which is transmitted through the surface 186 to the two nozzle members 80 and 82, thereby effecting a seal containing pressure between the members 80 and 82. The slots 194 and 196 are provided to facilitate the translation of the axial compression to radial compression of the adapter 84. The round hole 192 is provided for the flow of the product. In the example of a more elaborate absorption cell shown in Figure 9, the length of the cell and its effective internal diameter can be varied. The rod 242 has the same external dimensions as the rod 42 of Figures 3, 4, and 5, and consequently, the rods 42 and 242 are interchangeable. The rod 242 is provided with a precise positioning of the rod, and provides a convenient scale for the registration. The two absorption cell assemblies of Figures 10 and 11 exemplify a variety of ways to accommodate particular product requirements. The nozzle inserts 300, 302A, 302B and 304 are examples of a wide variety of inserts that can be used. The generally concave internal opening of the insert 300 induces cavitation when the fluid enters the cavity 306. The fluid immediately near the surface 308 will flow along a path defined by that surface, tending to separate from the flow path defined by the anterior surface 310. With a simultaneous pressure drop resulting from the largest cross-sectional area of the cavity 306, cavitation occurs. The generally convex internal opening of the insert 304 (Figure 11) induces cavitation in the fluid stream upon exiting the insert. The fluid pressure increases momentarily as the fluid passes through the center of insert 304. As in insert 300, the tendency of the fluid to follow the shape of the solid surface with a simultaneous pressure drop induces cavitation. The inserts 302A and 302B are identical and are configured to achieve the desired results for a particular product. Various identical inserts such as 302 can be used together, end-to-end, to form a continuous internal bore. Alternatively, several inserts with different internal diameters can be used to induce turbulence in the outgoing fluid stream. Yet another alternative, shown in Figure 10, is to leave a small space between the inserts to disturb laminar flow and generate turbulence. Still another alternative is to use several inserts such as 300 and / or 304 in series. In Figure 11, the reflective surface 440 exemplifies a variety of shapes that can be used to improve its function or for a particular application. Compared to semi-spherical or flat reflective surfaces, surface 440 has a much larger surface area that reflects the fluid jet "This scheme can be used to effect a more gradual flow reversal, and for abrasive solids applications, to extend the service life of the reflecting surface. The coil shown in Figures 12A to 12C is used to remove pressure fluctuations (Article 132 in Figures 1 and 2). The coil is made of conventional high pressure pipe (for example, Butech M / P of 6.35 millimeters, # 20-109-316), the diameter of the coil being large enough not to significantly affect the pressure index of the coil. the pipeline (for example, 10.16 centimeters), and of a sufficient length to remove smooth inner hole 238 at one end, internal threads at the other end, and a thinned sealing surface 208 therebetween. The nozzle insert 200 fits in the hole of the rod 238, secured by elements such as press fit or adhesive material, to form the opening of the cavity 236. The use of inserts with a variety of lengths, internal surface geometries and sizes , makes it possible to control the tear rate, cavitation, turbulence, and impact on the surface 240. The rod 202 is inserted into the rod 242 to provide the impact surface 240 of the absorption cell. The depth of the cavity 238, determined by the placement of the rod 202, controls the residence time of the product in the absorption cell, which in turn makes it possible to provide sufficient interaction time between the emulsifier and the oil droplets. The sleeve 204 is provided to secure the rod 202 in place, as well as to provide a seal between the rod 202 and the rod 242. Once the location of the rod 202 is selected, the sleeve 204 is tightened. The sealing surface The thinned 206 of the sleeve 204 is then pressed against the thinned sealing surface 208 of the rod 242, thereby forming a seal between the sleeve 204 and the rod 242, as well as between the sleeve 204 and the rod 202. the exposed end of the rod 202 facilitates pressure peaks (eg, 18,288 meters). The pipe expands slightly when the pump generates a pressure peak, acting in this way to absorb the excess energy generated by the pressure peak. At the end of the pressure peak, the pipe contracts, thus releasing the stored energy. This action of the coil is similar to the action of conventional hydraulic accumulators that are used in hydraulic systems for essentially the same purpose. Water jet cutting systems employ a similar principle (for example, the "Attenuator" from Flow International Corp.), in the form of a straight, long cylinder between the high-pressure intensifier pump and the nozzle, to generate a Constant flow velocity through the nozzle. As can be seen in Figures 12A to 12C, the pipe is wound in a manner that allows each ring of the coil to flex in response to pressure fluctuations, in an action similar to a Bourdon tube (used in water meters). Pressure) . Because the outer side of each coil ring has an area larger than the inner side, the pressure in the pipe tends to open each ring. This movement in response to pressure fluctuations provides another mechanism for absorbing and releasing energy. The coil in this way provides an element to remove pressure fluctuations, heating or cooling the product, while it is suitable for sterile CIP / SIP systems. Figure 13 illustrates a scheme for connecting several coils such as in Figures 12A to 12C, which make it possible to use a conventional pipe length (e.g., 6,096 meters), and conventional bending tools, to produce such long coils as necessary. Other embodiments are within the scope of the following claims. For example, it has been discovered, in the device test, that some products plug the orifice occasionally, forming a plug at the entrance of the orifice. One of the features of the emulsifier cell assemblies of Figures 14 and 15 is the ability to easily remove the capped product from the orifice. When that filler occurs, the pump must stop, and the pressure in the system must be released. The nozzle is then removed from the emulsifier cell assembly, and then installed again in an inverted direction. The product previously stuck at the inlet end of the hole thus moves towards the outlet end of the hole. When pressure is applied again, the jammed product leaves the hole, and normal operation can be resumed. Accordingly, as seen in Figure 14, the emulsifier cell includes: the inlet adapter 501, the body 502, the nozzle assembly 503, the insert 504, and the absorption cell assembly within the lid 505. The 521 thinned sealing surface of the inlet fitting 501 fits into the mating sealing surface 524 of the nozzle assembly 503. The thinned sealing surface 522 of the insert 504 fits into a mating sealing surface 525 of the nozzle assembly 503, and the 523 thinned sealing surface of the insert 504 is fitted into a mating sealing surface 526 of the body 502, to form a metal-to-metal seal containing pressure upon clamping the inlet fitting 501 in the body 502. The product fluid that is going away to process enters the emulsifying cell from gate 530, which consists of internal threads in the input fitting 501, and a female thinned sealing surface in the coupling 510, forming together a conventional H / P gate of 9.525 millimeters (for example Autoclave Engineers # F375C). The thinned sealing surface 527 of the coupling 510 fits in a coupling sealing surface 528 in the inlet fitting 501, to form a metal-metal seal containing pressure, by holding a conventional H / P nipple of 9.525 millimeters (eg , Autoclave Engineers # CN6604) in gate 530. Coupling 510 contains a round opening 531 along its center line (3.175 mm diameter hole) between the conventional female thinned sealing surface of gate 530 and opening 532 ( orifice of 3.175 millimeters in diameter), which remains at an angle to the center line of the coupling 510 (eg, 20 degrees). By ejecting from the opening 532, the product flows in a random turbulent pattern into a generally cylindrical cavity 533, then through the opening 534 and then through a small hole 535 in the nozzle 511. A detailed description of the Effects of the hole with the description of Figures 3A, 3B, and 4 above. If the product clogs and can not pass through the hole, the inlet fitting 501 can be unscrewed to release the nozzle assembly 503. Once loose, the nozzle assembly 503 can be rotated 180 ° along its axis , and then clamped again with the input fitting 501. The guide pin 512 inside the nozzle assembly 503 and the slot 513 in the body 502, facilitates this operation by guiding the nozzle assembly to its correct orientation. The jet of fluid formed in the orifice 535 remains essentially unchanged as it flows through the opening 536 of the insert 504, then through the opening 537 in the body 502 and through the opening 538 of the absorption cell . The surface 542 of the plug 509, which may be flat or hemispherical, or which may have another configuration that otherwise improves its function, forces the fluid jet to reverse its flow direction, and forms a coherent cylindrical flow stream, such as is described in more detail in conjunction with Figure 8. The absorption cell of Figure 14 is formed of an alternating series of ring seals 506 and reactors 507, which are available with different sizes and shapes of openings, as described with detail in conjunction with Figures 9 through 11. The opening 539 of the body 502 and the sleeve 508 support the reactors 507, and align them concentrically to the fluid jet. The sleeve 508 is supported by the round opening 540 in the lid 505, which in turn is held on the body 502. The modular design of this absorption cell 14 allows the operator to easily change the reactors, in order to test the effects of their sizes and opening shapes on the product. When replacing two reactors with a rod plug 541, the operator can change the length of the absorption cell, and consequently, the length of processing in the cell. After leaving the absorption cell, the processed product is expelled out of the emulsifier cell through gate 560, which is a standard 6.35 millimeter M / P gate (eg, Autoclave Engineers # SF250CX20). In the emulsifier cell shown in Figure 15, articles 601, 602, 603, 604, 606, 607, 610, 608 and 641 are identical to the corresponding articles of Figure 14 (501, 502, 503 and so on). The fastener 630 of Figure 15 is similar to the cap 505 of Figure 14, in the manner in which it supports the sleeve 608, and in the manner in which it is fastened to the body 602, however, the fastener 630 has a male thread 650 additional makes possible the addition of another fastener 631. The fasteners 630 and 631 are identical, as well as the shirts 608 and 627. Consequently, the flow of the product to be processed, from the inlet gate to the cells of absorption, is identical in the emulsifying cell of Figure 14 and Figure 15. The coupling 632 is fastened to the fastener 631 to provide another gate 637 (eg, Tri-Clover of 2.54 centimeters). The opening 633 of the coupling 632 is a cylindrical orifice, ending with a conventional short thinning 639 (eg, Morse Thinner). The insert 629 has a thinned engaging surface 638 to enable it to be secured in place. The surface 640 of the insert 629 deflects the stream from the jet coming from the hole, and can be of any shape or configuration, as described in detail in conjunction with Figure 8. The 628 plastic seal provides a tight seal when tightening the coupling 632 to the fastener 631, to maintain the integrity of the absorption cell, and prevent the product from leaking out of the emulsifier cell. The gate 637 makes it possible to add the ingredients of the product to be processed in the absorption cell. The product fluid to be added through the gate 637 enters through the round recess 636, which allows the flow from the center of the tube connected to the gate 637 to four round holes 635. Expelling from the holes 635, the fluid from the gate 637 interacts with the fluid from the orifice after it is diverted by the surface 640, and the two streams are mixed together by the intense turbulent flow in the cavity 633. Then the mixture enters the opening 651 of the absorption cell, where it forms a coherent cylindrical flow stream around the jet stream as described in detail in conjunction with Figure 8. The introduction of the product fluid through the gate 637 must be done with sufficient pressure to maintain the flow to the emulsifier cell. The required pressure is determined by the viscosity of the fluid and the operational parameters in the emulsifier cell (operating pressure, orifice diameter, diameter and length of the absorption cell, and can generally be provided by conventional pumps used in the industry
(diaphragm pumps, gear pumps, peristaltic pumps, etc.). The appropriate pump should be selected according to the pressure required and the specific requirements of each product (chemical compatibility, abrasion resistance, possibility of cleaning, etc.). The pressure required for each product and the setting of the operating parameters can be determined by reading the pressure in the supply line to gate 637 (for example, using a pressure indicator 172 such as Figure 2), while the high-pressure system pressure is operating but no product is flowing into the supply line (Figure 2, Article 164). Another feature of the emulsifier cell of Figure 15 is the ability to extend the length of the absorption cell to a large degree. This feature can be used to extend the duration of the process. A longer process duration is required to slowly react the emulsifying agents, as well as for many product formulations that require longer processing time. Another benefit of a longer absorption cell is the ability to minimize wear on the reflective surface 640 resulting from the impact of the jet stream. This feature is especially useful when processing abrasive products. Another feature of the emulsifier cell of Figure 15 is the additional gate to introduce the ingredients of the product into the emulsifier cell. The second gate can be used to introduce abrasive solids, which otherwise could not be processed in this device or in any other similar devices, such as homogenizing valves, due to the rapid wear of the orifice. The second gate can also be used when the chemical reaction between the ingredients of the product must be minimized. Since the product is. heated by approximately 0.75 ° C per 70 kg / cm2 when flowing through the orifice, another use for the second gate may be to inject one of the ingredients of the product at a low temperature in order to reduce the temperature of the product. This is especially useful for heat-sensitive products, such as enzymes. Finally, the second gate can be used for any product that can be damaged by high pressure or severe pressure drop in the hole.
Claims (45)
- CLAIMS 1. A method to be used to cause emulsification in a fluid, which comprises: 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 trajectory, orienting the first trajectory and the new trajectory to cause tearing and cavitation in the fluid. The method of claim 1, which further comprises: orienting the first path and the new path in essentially opposite directions. The method of claim 1, which further comprises: configuring the coherent flow as a cylinder surrounding the jet. 4. The method of claim 1, wherein the interposed structure comprises a reflecting surface. The method of claim 4, wherein the reflecting surface is generally hemispherical. 6. The method of claim 4, wherein the reflecting surface is generally thinned. 7. The method of claim 4, wherein the reflecting surface is at the end of a well. 8. The method of claim 7, which further comprises adjusting the pressure in the well. The method of claim 7, which further comprises adjusting the distance from the well opening to the reflecting surface. The method of claim 7, which further comprises an element for varying the size of the opening to the well. The method of claim 7, which further comprises directing the controlled flow, as it leaves the well, in an annular sheet away from the opening of the well. The method of claim 11, which further comprises directing an annular flow of a refrigerant in a direction opposite to the direction of the annular sheet. 13. A method for employing the stabilization of a hot emulsion immediately after its formation, which comprises: causing the emulsion to flow away from the outlet end of an emulsion forming structure, and causing a cooling fluid to flow in one direction generally opposite to the emulsion flow, and in a close enough proximity to exchange heat with the flow of the emulsion. The method of claim 13, which further comprises: forming the emulsion as a thin annular sheet as it flows out of the emulsion forming structure. 15. The method of claim 13, further comprising: forming the cooling fluid as a thin annular sheet as it flows oppositely to the emulsion. The method of claim 13, wherein the refrigerant fluid comprises a liquid or gas compatible with the emulsion. 17. The method of claim 13, further comprising: causing the emulsion and refrigerant fluid flows to occur in an annular valve opening. 18. A method for employing emulsification of a first fluid component within a second fluid component, which comprises: providing a supply of the first fluid component into a cavity, wherein the first fluid is essentially stagnant, and directing a jet of the second fluid component to the first fluid component, the temperatures and jet velocities of the fluids being selected to cause cavitation due to the hydraulic separation at the interface between the two fluids. The method of claim 18, wherein the second fluid component comprises a continuous phase of an emulsion or dispersion. The method of claim 18, wherein the first fluid component comprises a discontinuous phase in the emulsion. The method of claim 18, wherein the first fluid component comprises a solid discontinuous phase in the dispersion. 22. The method of claim 18, wherein the supply of the first fluid is provided in an annular chamber., and the jet is delivered from an outlet of an orifice that opens towards an annular chamber. The method of claim 18, which further comprises: after emulsification by hydraulic separation, passing the product through a hole to cause additional emulsification. The method of claim 18, which further comprises: following the emulsification by hydraulic separation, delivering the product to a subsequent processing chamber. 25. The method of claim 24, wherein an additional component is added to the emulsion in the subsequent processing chamber. 26. The method of claim 24, wherein a refrigerant fluid is applied to the product in the subsequent processing chamber, to rapidly cool and stabilize the emulsion. 27. The method of claim 24, wherein the subsequent processing chamber is an absorption cell toward which a product jet is directed. 28. An apparatus for reducing pressure fluctuations in an emulsifier cell fed from a fluid line by a high pressure pump, which comprises: a tube wound in the fluid line, between the pump and the emulsifier cell, having the tube an internal volume, a wall thickness, a diameter of the coil, and a suitable winding pattern to absorb the pressure fluctuations and able to withstand the high pressure generated by the pump. 29. The apparatus of claim 28, which further comprises a cover around the wound tube, with gates for filling the cover with heating or cooling fluid. 30. A nozzle for use in an emulsification structure, which comprises: "two body parts having flat surfaces that engage to form the nozzle, with at least one of the members having a groove to form a hole in the nozzle, the surfaces being sufficiently flat so that, when the two body parts are compressed together with sufficient force, the flow of fluid to the orifice is confined 31. The nozzle of claim 30, which further comprises: cavitation inducing surfaces defined on the groove 32. The nozzle of claim 30, which further comprises: a coating on the wall of the groove 33. The nozzle of claim 32, wherein the coating comprises diamond or non-polar materials or polar materials. 34. An absorption cell for use in an emulsification structure, the cell comprising: an elongated chamber having: u An open end for receiving a fluid jet having two immiscible components, a reflective surface at the other end of the chamber for reflecting the jet, and a mechanism for adjusting the distance from the reflective surface to the open end. 35. The absorption cell of claim 34, which further comprises: interchangeable reflective surfaces, each suitable for a different application. 36. The absorption cell of claim 34, further comprising: a removable insert for insertion into the chamber, at the open end, the insert having a hole one dimension smaller than the inner wall of the chamber. 37. The absorption cell of claim 36, which further comprises: interchangeable inserts, each suitable for a different application. 38. A modular emulsification structure, which comprises: a series of couplings that can be adjusted together in a variety of ways, each including at least one of the couplings: 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 between the male and female sealing surfaces, to communicate fluid from an upstream coupling to a downstream coupling, gates to feed fluid to, or withdraw fluid from, the coupling, at least some of the communication apertures being small enough to form a liquid jet, the sealing surfaces being sufficiently smooth to provide a fluid-tight seal when the couplings they are held together by a sufficient compression force directed along the length of the structure. 39. The structure of claim 38, wherein a processing chamber is defined between the male sealing surface of one of the upstream couplings, and the female sealing surface of one of the downstream couplings. 40. The structure of claim 38, wherein, in some of the couplings, the hole extends from one end of the coupling to the other. 41. The structure of claim 38, which further comprises an absorption cell coupling in one of the structures. 42. The structure of claim 38, wherein one of the couplings extends into another coupling to form a small annular opening for generating an annular flow sheet of the cooling fluid. 43. The structure of claim 38, wherein some of the couplings of the couplings are used for CIP / SIP cleaning and / or sterilization processes. 44. The method of claim 4, further comprising: directing a flow of an additional component into a space adjacent to the reflecting surface, and generally in the direction of the new path of the controlled flow. 45. An apparatus for use in an emulsification structure, comprising: a coupling, an orifice support containing an emulsification orifice, having two ends that open towards other components of the structure, mounting the orifice support in the coupling to allow the rotation of the support, to invert the locations of the two ends, serving each of the ends as an entrance or as an exit to the orifice, depending on their locations. PB.qttMtnt The 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. An emulsification cell has an inlet gate (18) leading to the opening (20) from where the fluid impacts the surface (30) of a coupling (12), and then flows in a random turbulent pattern inside a cavity generally cylindrical (32), formed between the couplings (10) and (12), and a high velocity jet is ejected from the orifice (34) to an absorption cell cavity (38). The emulsion flows through the opening (60) and discharges into the gate (62).
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US08330448 | 1994-10-28 | ||
PCT/US1995/013665 WO1996014141A1 (en) | 1994-10-28 | 1995-10-24 | Forming emulsions |
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EP (2) | EP1249270A2 (en) |
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- 1995-10-24 JP JP51533796A patent/JP3429508B2/en not_active Expired - Fee Related
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