NZ577687A - Spray drying metod and apparatus, where the spraying device produces a pressure drop of more than 15 bar across the outflow opening - Google Patents

Abstract

Method for spray drying a high-viscosity fluid product using a spraying device 2, comprises projecting the fluid product out of an outflow opening 6 of the spraying device 2 for obtaining droplets of the fluid product, where the spraying device is arranged to cause a pressure drop in the fluid product across the outflow opening which is larger than 15 bar, and at least partially drying the droplets in a drying medium to become particles.

Description

Received at IPONZ on 5 April 2012 1 Method and apparatus for spray drying and powder produced using said method The invention relates to a method for spray drying a fluid product using a spraying device, wherein the method comprises projecting the fluid product out of an outflow opening of the spraying device for obtaining droplets of the fluid product and at least partially drying the droplets in a drying medium, such as air, to become particles.

Methods for spray drying a fluid product are known per se. In one type of spray drying method, the fluid product is fed to a nozzle, which produces a mist of droplets of the fluid product in a vessel. The droplets are subsequently dried, e.g. in a stream of air.

Another method for spray drying a fluid product is known from WO 2005/058473. This known method comprises projecting, by means of nozzles, jets of liquid 10 and disturbing the jets to cause break up thereof into streams of droplets. Further, the droplets are contacted with streams of gas to cause or allow the droplets to, at least partially, solidify.

The known (conventional) spray drying methods, however, have the disadvantage that a relatively large amount of energy is required for drying the droplets to 15 become particles.

It is an object of the present invention to partially obviate the above problem, or at least to provide a useful alternative to know spray drying methods and apparatus.

According to a first aspect of the invention, the amount of energy required for drying the droplets to become particles can be reduced by spray drying high-viscosity fluid 20 products.

A fluid product to be spray dried usually comprises a solvent, e.g. a liquid such as water, and dry matter dissolved and/or suspended in the solvent. In the fluid product to be spray dried, the viscosity is inter alia related to the concentration of the dry matter in the solvent. When the viscosity of the fluid product is high (i.e. higher than viscosities 25 conventionally used for fluid WO 2008/069639 PCT/NL2006/000622 2 products to be spray dried), the concentration of dry matter is larger than the concentration of dry matter in fluid products which are spray dried using known spray drying methods. Hence, according to the first aspect of the invention, the droplets of the high-viscosity fluid product comprise less solvent 5 than droplets of fluid products in conventional spray drying methods, so that less energy is required to remove the solvent from the droplets to dry the droplets to become dry particles.

Conventional spray drying methods, and spray drying equipment, are not suitable for spray drying high-viscosity fluid products. The high-10 viscosity fluid product prevents natural formation of droplets. Further, in methods using projecting jets of liquid and disturbing the jets to cause break up thereof into streams of droplets, use of a high-viscosity fluid product prevents the formation of jets and/or the controlled break-up of the jets into droplets.

Further, generally, the skilled person will not consider high-viscosity fluid products as starting material for spray-drying. In this light, reference is made to the review of Prof. Walzel in Chem.-Ing.-Tech. 62 (1990) Nr. 12, pages 983-994, who observes that the commonly used "Hohlke geldu.se n sind fur hohere Flussigkeitsviskositaten ungeeignet". For a 1 mm nozzle, a viscosity of 20 50 mPa-s is said to be the maximum viscosity.

In order to overcome this problem, according to a second aspect of the invention the spraying device is arranged to cause a pressure drop in the fluid product across the outflow opening which is larger than 15 bar. Preferably, the pressure drop is larger than 50 bar, more preferably larger 25 than 100 bar, most preferably larger than 300 bar.

Hence it is possible to spray dry a high-viscosity fluid product using a spraying device, wherein the method comprises projecting the fluid product out of an outflow opening of the spraying device for obtaining droplets of the fluid product and at least partially drying the droplets in a drying medium, 30 such as air, to become particles. 3 Here a fluid product to be spray dried is considered a high-viscosity fluid product if the viscosity, determined at a spray drying temperature which in use prevails in the outflow opening, e.g. -50 to 300 °C, preferably 40-100 °C, and a shear rate as in use present in the outflow opening, e.g. 1-104 - 1-106 s_1, using a capillary viscosity meter, is higher than 10 mPa-s, preferably higher than 25 mPa-s, more preferably higher than 50 mPas, even more preferably higher than 100 mPa-s and most preferably higher than 200 mPa-s. Since products to be spray dried are usually shear-thinning and since the viscosity normally decreases with increasing temperature, it has been shown that these viscosities may well correspond with viscosities above 1 Pa-s at 20 °C and zero shear.

Alternatively, or additionally, as the droplets comprise less solvent, it is also possible to dry the droplets in a shorter time. It is also possible to dry the droplets, after having been ejected by the outflow opening along a shorter flight path. Hence it is possible to dry the droplets in a smaller installation, e.g. in a smaller vessel.

According to a third aspect of the invention, the step of projecting the fluid product out of the outflow opening comprises generating a fluid jet projecting from the outflow opening, and disturbing the fluid jet for breaking the fluid jet into droplets with a narrow size distribution. Preferably, the step of disturbing the fluid jet comprises varying the pressure of the fluid product upstream of the outflow opening, e.g. by moving an end of a control element in a direction from/to the outflow opening, for instance at a predetermined distance of 2-1500 p.m, preferably 15-500 |im, to the outflow opening, for varying the pressure of the fluid product by vibrating the control element. Thus, controlled break-up of the jet into droplets is possible. The larger concentration of dry matter in the droplets and the narrow size distribution further allow reduction of the amount of energy required for drying the droplets, because it is not necessary to over-dry the droplets to be sure that even the largest particles are fully dried. 4 Preferably, the pressure of the fluid product upstream of the outflow opening is varied at a predetermined, substantially constant, frequency. This aids in providing the narrow particle distribution. A droplet diameter may be determined by controlling the predetermined frequency.

Hence, it is possible to generate particles with a relatively narrow particle size distribution, e.g. a particle size distribution with a monodispersity index of less than 1, preferably less than 0.7, more preferably less than 0.1. The monodispersity index of the particle size distribution is defined as (dgo-dio)/d50, wherein dio, dso and d9o represent the 10%, 50% and 90% particle size 10 percentiles, respectively.

A narrow particle size distribution has, inter alia, the advantage that substantially all particles posses a desired property, such as good solubility. Further, it can be prevented that dust, i.e. particles that are so small that they are blown into the environment, e.g. by drying air, is produced. 15 Hence, the yield of the spray drying process can be larger.

Preferably, the predetermined frequency is chosen such that a distance between two droplets consecutively ejected at the outflow opening is greater than or equal to two times the droplet diameter, preferably greater than or equal to three times the droplet diameter. Hence, it is effectively 20 prevented that droplets coagulate after being formed. Thus, the narrow size distribution is better maintained.

Preferably, the predetermined frequency is chosen such that a distance between two droplets consecutively ejected at the outflow opening is smaller than or equal to eight times the droplet diameter, preferably smaller 25 than or equal to four times the droplet diameter. Hence, droplets can be produced at a high repetition rate.

According to a fourth aspect of the invention, the step of projecting the fluid product out of the outflow opening comprises providing the fluid product to an outflow opening at a predetermined feed pressure. Preferably, 30 the feed pressure is kept substantially constant. This provides the advantage, that a jet is formed wherein break-up into droplets is not influenced by variations in the feed pressure. Thus, the narrow size distribution is better maintained.

The feed pressure may be kept substantially constant by means of 5 applying pressure to the fluid product hydraulically or pneumatically. Hydraulically is understood to mean: using a liquid; and pneumatically is understood to mean: using a gas. Through the ability to apply the feed pressure to the fluid product utilizing a gas and/or a liquid, the fluid product can be supplied to the outflow opening in a stable manner at a very high 10 pressure of e.g. more than 15 bars.

Alternatively, or additionally, the feed pressure may be kept substantially constant by means of a pump.

According to a fifth aspect of the invention, the method may comprise projecting the fluid product out of a plurality of outflow openings of 15 the spraying device for obtaining droplets of the fluid product. Hence, it is possible to increase the volume of fluid product per unit time that can be spray dried using the method.

According to a sixth aspect of the invention, the viscosity of the fluid product, determined at the spray drying temperature which in use prevails in 20 the outflow opening, e.g. -50 to 300 °C, preferably 40-100 °C, and a shear rate as in use present in the outflow opening, e.g. l-104-l-106s'1, using a capillary viscosity meter, is higher than 10 mPa-s, preferably higher than 25 mPa-s, more preferably higher than 50 mPa-s, even more preferably higher than 100 mPa-s and most preferably higher than 200 mPa-s. Hence, a high-viscosity 25 fluid product can be spray-dried.

Further, preferably a transverse dimension, e.g. a smallest transverse dimension such as a diameter, of the outflow opening is smaller than or equal to 150 fJ.ni, preferably smaller than or equal to 100 jum, more preferably smaller than or equal to 80 [am. Hence, it is possible to produce 6 relatively small droplets, e.g. droplets with an average size smaller than or equal to 250(j.m.

In a special embodiment, the viscosity of the fluid product, determined at the spray drying temperature which in use prevails in the 5 outflow opening, e.g. 40-100 °C, and a shear rate as in use present in the outflow opening, e.g. 1-104-1106 s*1, using a capillary viscosity meter, is higher than 30 mPa-s, while the transverse dimension, e.g. the diameter, of the outflow opening is smaller than or equal to 100 |um. ;The invention further relates to a powder produced using the 10 method according to the invention and an apparatus for spray drying a high-viscosity fluid product ;Further details, aspects and embodiments of the invention will be described, by way of example only, with reference to the drawings. 15 Fig. 1 shows an example of a first embodiment of an apparatus for spray drying a fluid product according to the invention. ;Fig. 2 shows an example of a second embodiment of an apparatus for spray drying a fluid product according to the invention. ;Fig. 3 shows an example of a third embodiment of an apparatus for 20 spray drying a fluid product according to the invention. ;Figs. 4a-4g show examples of plan views of a plurality of outflow openings of embodiments of a spraying device according to the invention. ;Fig. 1 shows an example of a first embodiment of an apparatus 1 for 25 spray drying a fluid product according to the invention. The apparatus 1 ;comprises a spraying device 2. In this example, the spraying device 2 is in fluid communication with a product supply line 4, for supplying the fluid product to be spray dried to the spraying device 2. The spraying device 2 is arranged for projecting the fluid product out of an outflow opening 6 of the spraying device 30 for obtaining droplets 8 of the fluid product. In this example, the spraying ;WO 2008/069639 PCT/NL2006/000622 ;7 ;device 2 projects the droplets 8 into a vessel 10. Here, the vessel 10 forms drying means for allowing the droplets 8 to dry to become particles. It is also possible that the apparatus comprises drying means for causing the droplets 8 to dry to become particles, e.g. supply means for drying air. Such supply means 5 may e.g. provide drying air flowing along with the droplets or in a counter flow flowing opposite to the direction of the droplets. ;In use, the fluid product to be spray dried is supplied to the spraying device 2. According to the invention the fluid product is a high-viscosity fluid product. The viscosity of the fluid product is higher than 10 mPa-s, preferably 10 higher than 25 mPa-s, more preferably higher than 50 mPa-s even more preferably higher than 100 mPa-s, most preferably higher than 200 mPa-s, determined at the spray drying temperature which in use prevails in the outflow opening, e.g. -50 to 300, in this example 40-100 °C, and a shear rate as in use present in the outflow opening, e.g. 1-104-1-106 s-1, in this example 5-105 15 S'1, using a capillary viscosity meter. ;In this Example a smallest transverse dimension, such as a diameter, of the outflow opening 6 is smaller than or equal to 150 |am, preferably smaller than or equal to 100 p,m, more preferably smaller than or equal to 80 pm. ;20 Hence, it is possible to spray dry a fluid product having a viscosity of higher than 10 mPa-s using an outflow opening 6 of smaller than or equal to 150 jam, or a fluid product having a viscosity of higher than 25 mPa-s using an outflow opening of smaller than or equal to 150 |a.m, or a fluid product having a viscosity of higher than 50 mPa-s using an outflow opening of smaller than or 25 equal to 150 |am, or a fluid product having a viscosity of higher than 100 mPa-s using an outflow opening of smaller than or equal to 150 jam, or a fluid product having a viscosity of higher than 200 mPa-s using an outflow opening of smaller than or equal to 150 |am, or a fluid product having a viscosity of higher than 10 mPa-s using an outflow opening of smaller than or equal to 100 jam, or 30 a fluid product having a viscosity of higher than 25 mPa-s using an outflow ;WO 2008/069639 ;PCT/NL2006/000622 ;8 ;opening of smaller than or equal to 100 (am, or a fluid product having a viscosity of higher than 50 mPas using an outflow opening of smaller than or equal to 100 (am, or a fluid product having a viscosity of higher than 100 mPa-s using an outflow opening of smaller than or equal to 100 |am, or a fluid product 5 having a viscosity of higher than 200 mPa-s using an outflow opening of smaller than or equal to 100 jam, or a fluid product having a viscosity of higher than 10 mPa-s using an outflow opening of smaller than or equal to 80 |am, or a fluid product having a viscosity of higher than 25 mPa-s using an outflow opening of smaller than or equal to 80 jam, or a fluid product having a viscosity 10 of higher than 50 mPa-s using an outflow opening of smaller than or equal to 80 (am, or a fluid product having a viscosity of higher than 100 mPa-s using an outflow opening of smaller than or equal to 80 |am, or a fluid product having a viscosity of higher than 200 mPa-s using an outflow opening of smaller than or equal to 80 (am, wherein the viscosity is defined at the spray drying 15 temperature which in use prevails in the outflow opening, e.g. -50 to 300 °C, in this example 40-100 °C, and a shear rate as in use present in the outflow opening, e.g. 1104-1106 s1, in this example 5-105 s-1, using a capillary viscosity meter. ;Spray drying the high-viscosity fluid product with the above 20 viscosity, is effected using the spraying device 2, having the above outflow opening 6, which is arranged to cause a pressure drop in the fluid product across the outflow opening 6 which is larger than 15 bar, preferably larger than 50 bar, more preferably larger than 100 bar, most preferably larger than 300 bar. The combination of the pressure drop, high viscosity and dimension of 25 the outflow opening provide that droplets of the high-viscosity fluid product can be produced having a desired size, of e.g. smaller than or equal to 250 jam in average, while the amount of energy required to dry the droplets is reduced with respect to conventional spray drying methods. ;Fig. 2 shows an example of a second embodiment of an apparatus 1 30 for spray drying a fluid product according to the invention. In the example of ;WO 2008/069639 ;PCT/NL2006/000622 ;9 ;Fig. 2 the spraying device 2 comprises feed pressure generating means 12 for providing the fluid product to the outflow opening 6 at a predetermined feed pressure for obtaining a fluid jet. Here, the feed pressure generating means 12 are arranged for keeping the feed pressure substantially constant. Hence, a 5 fluid jet is generated, while the feed pressure generating means 12 substantially do not disturb the jet. ;In the example of Fig. 2, the feed pressure generating means comprise a pump 14 for supplying the fluid product at the desired pressure. The pump 14 may be arranged for keeping the feed pressure substantially 10 constant. Thereto, the pump may comprise a pressure regulator, such as for instance an overpressure valve and/or a damper. ;Alternatively, or additionally, the feed pressure generating means 12 may be arranged for applying pressure to the fluid product hydraulically or pneumatically for keeping the feed pressure substantially constant, i.e. the 15 feed pressure generating means 12 may use pressurized liquid or gas, ;respectively, to exert a substantially constant pressure on the fluid product. ;Preferably, the feed pressure generating means 12 generate the feed pressure which is in the interval of 15-3000 bars, more preferably in the interval of 15-600 bars. Hence, it is possible to spray dry the high-viscosity 20 fluid product. ;Fig. 3 shows an example of a third embodiment of an apparatus for spray drying a fluid product according to the invention. ;In the example of Fig. 3 the spraying device 12 comprises pressure varying means 16 for varying the pressure of the fluid product upstream of the 25 outflow opening 6. When the jet is projected from the outflow opening, variations in the pressure of the fluid product of the jet cause the jet to contract at points of minimum pressure. Subsequently, the fluid jet will break up at the contractions, thus forming droplets. An amplitude of the variations in the pressure of the fluid product may be approximately 10% of the feed ;WO 2008/069639 PCT/NL2006/000622 ;10 ;pressure. The amplitude of the variations in the pressure may be 1 mbar to 100 bar, preferably smaller than or equal to 25 bar. ;In this example, the pressure varying means 16 comprise a control element 18, which is movable in a direction from/to the outflow opening 6. ;5 Vibrating the control element 18 relative to the outflow opening 6 causes the pressure of the fluid product to vary between the control element 18 and the outflow opening 6. When the fluid product is projected from the outflow opening 6 in the fluid jet, the variations in pressure in the fluid product extend into the jet. ;10 The pressure varying means 16 may e.g. comprise a piezo-electric element, an electrostrictive element, an acoustic element, an electromagnetic actuator, a voice-coil, and/or mechanical means for moving the control element 18 in the direction from/to the outflow opening 6. ;In a preferred embodiment, the control element 18 is positioned at a 15 predetermined distance of 2-1500 |im, preferably 15-500 |am, to the outflow opening 6. This provides the advantage that a pressure variation exerted to the high-viscosity fluid product is prevented from being damped by the high-viscosity fluid product to an extent that the jet projected from the outflow opening does not experience a pressure variation with large enough amplitude 20 to effectively break up into droplets. ;In a particularly effective embodiment, the pressure varying means 16 are arranged for varying the pressure of the fluid product upstream of the outflow opening 6 at a predetermined frequency. Preferably, the predetermined frequency is substantially constant. Hence, the fluid jet will 25 contract, and subsequently break up, at substantially equidistant positions along the fluid jet. Thus, substantially equal sized droplets will be formed, providing droplets with a relatively narrow droplet size distribution, e.g. a droplet size distribution with a monodispersity index of less than 1, preferably smaller than 0.7, more preferably smaller than 0.1. The monodispersity index ;WO 2008/069639 ;PCT/NL2006/000622 ;11 ;of the droplet size distribution is defined as (dgo-dioVdso, wherein dio, dso and dgo represent the 10%, 50% and 90% droplet size percentiles, respectively. ;In this example, the predetermined frequency is chosen such that a distance between two droplets consecutively ejected at the outflow opening 6 is 5 greater than or equal to two times the droplet diameter, preferably greater than or equal to three times the droplet diameter. Thus, coagulation of droplets can be prevented, maintaining a narrow droplet size distribution. ;In this example the predetermined frequency is in the interval of 500-200000 Hz. For example, when using a fluid product having a viscosity of 10 50 mPa-s and using an outflow opening having a transverse dimension, e.g. a smallest transverse dimension such as a diameter, of 80 (am, the frequency may be chosen between 500 and 40000 Hz for obtaining droplets with an average size (dso) of 133 jam to 575 jam depending on chosen frequency and volume flow of fluid product through the outflow opening. ;15 In the examples of Figs. 1-3 the spraying device 2 comprises one outflow opening 6. It will be appreciated that it is also possible that the spraying device 2 comprises a plurality of outflow openings 6 for projecting the fluid product out of the plurality of outflow openings for obtaining droplets of the fluid product. Thereto, the outflow openings may e.g. may be arranged as 20 bores in a surface of the spraying device. The plurality of outflow openings may be arranged for generating a plurality of mutually divergent jets of the fluid product. Thereto, the outflow openings may e.g. may be arranged as bores in a surface of the spraying device, which bores extend in mutually diverging directions, e.g. in directions which are non-perpendicular with respect to the 25 surface of the spraying device 2. When the jets are mutually divergent, the risk of coagulation of droplets ejected by mutually different outflow openings is reduced, since a distance between the droplets ejected by the mutually different outflow openings increases during flight. It is possible to use the plurality of outflow openings in combination with a single control element for ;WO 2008/069639 PCT/NL2006/000622 ;12 ;varying the pressure of substantially all fluid jets generated by the plurality of outflow openings. ;Preferably, the outflow openings of the plurality of outflow openings have substantially identical dimensions, to allow droplets of substantially identical dimensions to be ejected from each separate outflow opening, hence allowing the droplets to be produced with the relatively narrow size distribution. ;Preferably, a distance between two adjacent outflow openings of the plurality of outflow openings is larger than 1.5 times a transverse dimension, such as a diameter, of at least one of the two adjacent outflow openings, more preferably larger than 2 times, most preferably larger than or equal to 2.5 times the transverse dimension. Hence, the risk of coagulation of droplets ejected by mutually different outflow openings is reduced. Preferably, a distance between two adjacent outflow openings of the plurality of outflow openings is smaller than 5 times a transverse dimension, such as a diameter, of at least one of the two adjacent outflow openings, more preferably smaller than 4 times, most preferably smaller than or equal to 3 times the transverse dimension. Hence, a physical size of the spraying device 2 may be limited. ;Figs. 4a-4g show examples of plan views of the plurality of outflow openings 6 of embodiments of the spraying device 2 according to the invention. In the examples of Figs. 4a-4d, the plurality of outflow openings 6 is arranged in a substantially ring-shaped formation 20. In Fig. 4a an example is shown of a ring of closely packed outflow openings, e.g. in hexagonal close packing. Hence, a hollow cone of droplets may be generated. In Fig. 4b an example is shown of a ring comprising a single endless line of outflow openings. The single line of outflow openings reduces the risk of coagulation of droplets. In Fig. 4c an example is shown wherein the plurality of outflow openings is arranged in a formation comprising a plurality of substantially ring-shaped sub-formations, here three spaced concentric rings each comprising a single endless line of outflow openings. The spaced single line rings reduce the risk of coagulation of ;WO 2008/069639 ;PCT/NL2006/000622 ;13 ;droplets, while reducing the surface area size required for providing a predetermined number of outflow openings, with respect to the example of Fig. 4b. In Fig. 4d an example is shown wherein the plurality of outflow openings is arranged in a formation comprising a plurality of substantially ring-shaped 5 sub-formations, here five non-concentric rings each comprising a single endless line of outflow openings. ;Fig. 4e shows an example of a circle of closely packed outflow openings, e.g. in hexagonal close packing. Hence, a full cone of droplets may be produced, giving a large number of droplets per unit surface area of spraying 10 device comprising outflow openings. Hence, a compact spray drying apparatus may be provided. ;Fig. 4f shows an example of a substantially straight line of outflow openings. This e.g. allows for spray drying into a narrow wide vessel. Fig. 4g shows an example of a plurality of spaced substantially straight lines of 15 outflow openings. ;According to the invention a method for spray drying a high-viscosity fluid product is provided. This method can e.g. be performed using the spraying device 2 according to any one of the Figures. The method comprises projecting the fluid product out of the outflow opening 6 of the spraying device 20 2 for obtaining droplets of the fluid product, wherein the spraying device 2 is arranged to cause a pressure drop in the fluid product across the outflow opening 6 which is larger than 15 bar, and at least partially drying the droplets in a drying medium, such as air, to become particles. ;As already explained with respect to the apparatus 1, the pressure 25 drop is preferably larger than 50 bar, more preferably larger than 100 bar, most preferably larger than 300 bar. ;Using the method according to the invention, a powder may be produced. The powder may have a monodispersity index smaller than 1, preferably smaller than 0.7, more preferably smaller than 0.1. The 30 monodispersity index of the powder is defined as (d90-dio)/d5o, wherein dio, dso ;WO 2008/069639 ;PCT/NL2006/000622 ;14 ;and d9o represent the 10%, 50% and 90% particle size percentiles of the powder, respectively. The powder may have an average particle diameter smaller than or equal to 250 |_im. ;According to the invention, the powder is produced from the high-5 viscosity fluid product by spray drying. As already mentioned this has the advantage, that the fluid product to be spray dried may comprise relatively large concentrations of dry matter, so that relatively small amounts of solvent have to be removed from droplets expelled by the outflow opening to yield dry particles. Without wishing to be bound by any theory, it is believed that this 10 causes less inclusion of solvent within a dry outer crust of the particle, so that after drying particles are obtained with lower porosity and/or a lower percentage of included gas. Hence, using the method according to the invention, it is possible to produce the powder having small percentage of the volume of the particles consisting of gas and/or voids, e.g. less than 5% of a 15 volume of particles of the powder consists of gas and/or voids. Further, using the method according to the invention, it is possible to produce the powder having a high density, e.g. having a bulk density larger than or equal to 550 kg/m3 or preferably larger than or equal to 650 kg/m3 for food powders, generally mainly comprising fat, protein and/or carbohydrates. 20 For food powders comprising fat a bulk density may be obtained which is higher than a reference bulk density according to the equation ;RBD = ZFD - 5 x FC wherein RBD represents the reference bulk density in kg/m3, ZFD represents a zero-fat-density which represents the bulk density (in kg/m3) of a powder 25 containing no fat, and FC represents the fat content in percents by weight of the dried product. Using the spray drying method according to the invention, a powder may be obtained having bulk density (in kg/m3) which is higher than the RBD according to the above equation wherein ZFD is equal to or larger than 650 kg/m3, preferably equal to or larger than 800 kg/m3. ;WO 2008/069639 PCT/NL2006/000622 ;15 ;Exemplary powders were produced using the spray drying method according to the invention. A first powder had a fat content of 50% by weight and a bulk density of 540 kg/m3. A second powder had a fat content of 78 percent by weight and a bulk density of 420 kg/m3. ;5 ;Example 1 ;The production of highly monodisperse maltodextrin powder was conducted according to the following procedure: ;A solution of 60% by weight maltodextrin and 40% by weight of 10 water was prepared, having a density of 1250 mg/ml. This solution was fed into a high viscosity spraying device as described hereinabove. The spraying device used has a substantially circular outflow opening with a diameter of 50 micrometers. The solution was projected out of the outflow opening with a feed rate of 1.25 ml/min, and a firing frequency of 23.7 kHz (i.e. droplets were 15 produced at a rate of 23.7-103 droplets per second). The temperature of the spraying device at the outflow opening was 80 °C and the feed pressure applied in the spraying device was 35 bar. The resulting droplets had an average diameter of 120 jam. ;To dry these droplets to obtain a monodisperse powder, the droplets 20 were ejected into a spray drying tower with an entrance temperature of 170 °C and exit temperature of 85 °C. The running length for drying was 1.8 meter and the venting percentage was 60%, which resulted in an average residence time of 2-6 s for each droplet. The particles of the resulting powder produced had an average diameter of 95 jam and a monodispersity index of 0.60. The 25 powder produced had a bulk density of 840 kg/m3. ;30 ;Example 2 ;Monodisperse creamer-powder was produced according to the following procedure. ;WO 2008/069639 PCT/NL2006/000622 ;16 ;A solution of 30% by weight water, 3% by weight Sodium Casemate, and 38% by weight maltodextrin was prepared, into which 29% by weight sunflower oil was emulsified using a high pressure homogeniser. The emulsion had a viscosity of 30-40 mPas at 85 °C and high shear (5-105 s*1) and a 5 viscosity of 700-900 mPa-s at low shear (300 s1) and 20 °C, both measured with a capillary viscosity meter.

This solution was fed into a high viscosity spraying device as described hereinabove, having a substantially circular outflow opening with a diameter of 50 micrometers. The solution was projected out of the outflow 10 opening with a feed rate of 1 ml/min, and a firing frequency of 25 kHz. The temperature of the spraying device at the outflow opening was 73 °C and the feed pressure applied in the spraying device was 60 bar. To dry the droplets produced to obtain monodisperse powder, the droplets were ejected into a spray drying tower with an entrance temperature of 129 °C and exit 15 temperature of 85 °C. The running length for drying was 1.8 meter and the venting percentage was 60%, which resulted in an average residence time of 2-6 s for each droplet. The resulting powder produced had an average particle diameter of 147 |a.m and a monodispersity index of 0.69. The powder produced had a bulk density of 550 kg/m3.

The method and apparatus according to the invention may be used for spray drying products such as a nutrient or an ingredient therefore, e.g. dairy products, proteins, carbon hydrates, fats, or combinations thereof. Alternative products are, however, not excluded.

In the foregoing specification, the invention has been described with reference to specific examples of embodiments of the invention. It will, however, be evident that various modifications and changes may be made therein without departing from the broader spirit and scope of the invention as set forth in the appended claims. For example, instead of for spray drying 30 nutrients or ingredients therefore, the method may also be used for spray 17 drying other products such as, but not limited to, detergents, pigments, catalysts, pharmaceuticals, cosmetics, polymeric resins, ceramic powders, powder coating materials, adhesives, gypsum, cement, metal powders, etc.

However, other modifications, variations and alternatives are also 5 possible. The specifications, drawings and examples are, accordingly, to be regarded in an illustrative rather than in a restrictive sense.

In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. The word 'comprising' does not exclude the presence of other features or steps then those listed in a claim.

Furthermore, the words 'a' and 'an' shall not be construed as limited to 'only one', but instead are used to mean 'at least one', and do not exclude a plurality. The mere fact that certain measures are recited in mutually different claims does not indicate that a combination of these measures cannot be used to advantage.

Received at IPONZ on 5 April 2012

Claims (92)

18 Claims

1. Method for spray drying a high-viscosity fluid product using a spraying device, wherein the method comprises: projecting the fluid product out of an outflow opening of the spraying device for obtaining droplets of the fluid product, wherein the spraying device is arranged to cause a pressure drop in the fluid product across the outflow opening which is larger than 15 bar; and at least partially drying the droplets in a drying medium to become particles.

2. Method according to claim 1, wherein the drying medium is air.

3. Method according to claim 1 or claim 2, wherein the pressure drop is larger than 50 bar.

4. Method according to claim 3, wherein the pressure drop is larger than 100 bar.

5. Method according to claim 4, wherein the pressure drop is larger than 300 bar.

6. Method according to claim 1 or claim 2, wherein the pressure drop is in the interval of 15-3000 bar.

7. Method according to claim 6, wherein the pressure drop is in the interval of 50-600 bar.

8. Method according to any one of the preceding claims, wherein the step of projecting the fluid product out of the outflow opening comprises: generating a fluid jet projecting from the outflow opening; and disturbing the fluid jet to break the fluid jet into droplets with a narrow size distribution.

9. Method according to any one of the preceding claims, wherein the step of projecting the fluid product out of the outflow opening comprises: providing the fluid product to an outflow opening at a predetermined feed pressure.

10. Method according to claim 8, wherein the step of disturbing the fluid jet comprises: varying the pressure of the fluid product upstream of the outflow opening.

11. Method according to claim 10, wherein the step of varying the pressure comprises: Received at IPONZ on 11 April 2012 19 moving an end of a control element in a direction from/to the outflow opening at a predetermined distance to the outflow opening to vary the pressure of the fluid product by vibrating the control element.

12. Method according to claim 11, wherein the predetermined distance is 2-1500 5 jj,m.

13. Method according to claim 12, wherein the predetermined distance is 15-500 jam.

14. Method according to any one of claims 11-13, wherein the control element is vibrated using at least one of a piezo-electric element, an electrostrictive element, an 10 acoustic element, an electromagnetic actuator, a voice-coil, or mechanical means.

15. Method according to any one of claims 10-14, wherein the pressure of the fluid product upstream of the outflow opening is varied at a predetermined, substantially constant, frequency.

16. Method according to claim 15, wherein a droplet diameter is determined by 15 controlling the predetermined frequency and/or material throughput through the outflow opening.

17. Method according to claim 15 or 16, wherein the predetermined frequency is chosen such that a distance between two droplets consecutively ejected at the outflow opening is greater than or equal to two times the droplet diameter. 20

18. Method according to claim 17, wherein the predetermined frequency is chosen such that a distance between two droplets consecutively ejected at the outflow opening is greater than or equal to three times the droplet diameter.

19. Method according to any one of the claims 14-18, wherein the predetermined frequency is in the interval of 500-200000 Hz. 25

20. Method according to any one of the preceding claims, comprising projecting the fluid product out of a plurality of outflow openings of the spraying device to obtain droplets of the fluid product.

21. Method according to any one of the preceding claims, wherein a viscosity of the fluid product determined at a spray drying temperature which in use prevails in the outflow 30 opening and a shear rate as in use present in the outflow opening using a capillary viscosity meter, is higher than 10 mPa-s. Received at IPONZ on 5 April 2012 20

22. Method according to claim 21, wherein the spray drying temperature is -50 to 300 °C.

23. Method according to claim 21, wherein the viscosity of the fluid product is higher than 25 mPa-s. 5

24. Method according to claim 21, wherein the viscosity of the fluid product is higher than 50 mPa-s.

25. Method according to claim 21, wherein the viscosity of the fluid product is higher than 100 mPa-s.

26. Method according to claim 21, wherein the viscosity of the fluid product is 10 higher than 200 mPa-s.

27. Method according to any one of claims 21-26, wherein the spray drying temperature is 40-100 °C.

28. Method according to any one of claims 21 to 27, wherein the shear rate is MO4-MO6 s"1. 15

29. Method according to any one of the preceding claims, wherein a transverse dimension of the outflow opening is smaller than or equal to 150 jam.

30. Method according to claim 29, wherein the transverse dimension of the outflow opening is smaller than or equal to 100 jam.

31. Method according to claim 29, wherein the transverse dimension of the outflow 20 opening is smaller than or equal to 80 jam.

32. Method according to any one of claims 29 to 31, wherein the transverse dimension is a smallest transverse dimension.

33. Method according to claim 32, wherein the smallest transverse dimension is a diameter. 25

34. Method according to claim 9, wherein the feed pressure is kept substantially constant.

35. Method according to claim 34, wherein the feed pressure is kept substantially constant by means of applying a pressure to the fluid product hydraulically or pneumatically. 30 36. Method according to claim 34 or 35, wherein the feed pressure is kept substantially constant by means of a pump.

Received at IPONZ on 7 May 2012 21

37. Method according to any one of claims 9-36, wherein the feed pressure is in the interval of 15-3000 bars.

38. Method according to claim 37, wherein the feed pressure is in the interval of 15-600 bars. 5

39. Powder produced using the method according to any one of claims 1-38.

40. Powder according to claim 39 having a monodispersity index smaller than 1.

41. Powder according to claim 40 having a monodispersity index smaller than 0.7.

42. Powder according to claim 41 having a monodispersity index smaller than 0.1.

43. Powder according to any one of claims 39 to 42, having an average particle 10 diameter (d50) smaller than or equal to 250 jam.

44. Powder according to any one of claims 39-43, wherein less than 5% of the volume of the powder particles consists of gas and/or voids.

45. Powder according to any one of claims 39-44, comprising a food product mainly comprising protein, carbohydrate, fat, or a combination thereof. 15

46. Powder according to any one of claims 39-45 having a bulk density larger than or equal to 550 kg/m3.

47. Powder according to claim 46 having a bulk density larger than or equal to 650 kg/m3.

48. Powder according to any one of claims 39-47, which is a food powder 20 comprising fat and having a bulk density higher than a reference bulk density according to the equation RBD = ZFD - 5 x FC wherein RBD represents the reference bulk density in kg/m3, ZFD represents a zero-fat-density which represents the bulk density (in kg/m3) of a powder containing no fat, and FC 25 represents the fat content of the powder in percent by weight, wherein ZFD is equal to or larger than 650 kg/m3.

49. Food powder according to claim 48, wherein ZFD is equal to or larger than 800 kg/m3.

50. Apparatus for spray drying a high-viscosity fluid product comprising 30 a spraying device arranged for projecting the fluid product out of an outflow opening of the spraying device for obtaining droplets of the fluid product, Received at IPONZ on 5 April 2012 22 wherein the spraying device is arranged to cause a pressure drop in the fluid product across the outflow opening which is larger than 15 bar, wherein the spraying device comprises feed pressure generating means for providing the fluid product to the outflow opening at a predetermined feed pressure for 5 obtaining a fluid j et, wherein the spraying device comprises pressure varying means for varying the pressure of the fluid product upstream of the outflow opening for breaking the fluid jet into droplets with a narrow size distribution, wherein the pressure varying means comprise a control element which is 10 movable in a direction from/to the outflow opening at a predetermined distance to the outflow opening for varying the pressure of the fluid product by vibrating the control element, and drying means for causing and/or allowing the droplets to dry to become 15 particles.

51. Apparatus according to claim 50 wherein the pressure drop is larger than 50 bar.

52. Apparatus according to claim 51 wherein the pressure drop is larger than 100 bar.

53. Apparatus according to claim 51 wherein the pressure drop is larger than 300 20 bar.

54. Apparatus according to any one of claims 50 to 53, wherein the control element is movable at a predetermined distance of 2-1500 jam to the outflow opening.

55. Apparatus according to claim 54, wherein the predetermined distance is 15-500 jam. 25

56. Apparatus according to any one of claims 50-55, wherein the pressure varying means are arranged for vibrating the control element using at least one of a piezo-electric element, an electrostrictive element, an acoustic element, an electromagnetic actuator, a voice-coil, or mechanical means.

57. Apparatus according to any one of claims 50-56, wherein the pressure varying 30 means are arranged for varying the pressure of the fluid product upstream of the outflow opening at a predetermined substantially constant frequency. Received at IPONZ on 5 April 2012 23

58. Apparatus according to claim 57, wherein the predetermined frequency is chosen such that a distance between two droplets consecutively ejected at the outflow opening is greater than or equal to two times the droplet diameter.

59. Apparatus according to claim 57, wherein the predetermined frequency is chosen 5 such that a distance between two droplets consecutively ejected at the outflow opening is greater than or equal to three times the droplet diameter.

60. Apparatus according to any one of claims 57 to 59, wherein the predetermined frequency is in the interval of 500-200000 Hz.

61. Apparatus according to claim 50, wherein the feed pressure generating means 10 are arranged for keeping the feed pressure substantially constant.

62. Apparatus according to claim 61, wherein the feed pressure generating means are arranged for applying pressure to the fluid product hydraulically or pneumatically for keeping the feed pressure substantially constant.

63. Apparatus according to claim 61 or 62, wherein the feed pressure generating 15 means comprise a pump for keeping the feed pressure substantially constant.

64. Apparatus according to any one of claims 50-63, wherein the feed pressure generating means are arranged for generating the feed pressure which is in the interval of 15-3000 bars.

65. Apparatus according to claim 64, wherein the feed pressure generating means 20 are arranged for generating the feed pressure which is in the interval of 15-600 bars.

66. Apparatus according to any one of claims 50-65, wherein a transverse dimension of the outflow opening is smaller than or equal to 150 jam.

67. Apparatus according to claim 66, wherein the transverse dimension of the outflow opening is smaller than or equal to 100 jam. 25

68. Apparatus according to claim 66, wherein the transverse dimension of the outflow opening is smaller than or equal to 80 jam.

69. Apparatus according to any one of claims 66-68, wherein the transverse dimension is a smallest transverse dimension.

70. Apparatus according to claim 69, wherein the smallest transverse dimension is a 30 diameter. Received at IPONZ on 5 April 2012 24

71. Apparatus according to any one of claims 50-70, wherein the spraying device comprises a plurality of outflow openings for projecting the fluid product out of the plurality of outflow openings for obtaining droplets of the fluid product.

72. Apparatus according to claim 71, wherein the plurality of outflow openings is 5 arranged for generating a plurality of mutually divergent jets of the fluid product.

73. Apparatus according to claim 71 or claim 72, wherein a distance between two adjacent outflow openings of the plurality of outflow openings is larger than 1.5 times a transverse dimension of at least one of the two adjacent outflow openings.

74. Apparatus according to claims 73, wherein a distance between two adjacent 10 outflow openings of the plurality of outflow openings is larger than 2 times the transverse dimension of at least one of the two adjacent outflow openings.

75. Apparatus according to claim 73, wherein a distance between two adjacent outflow openings of the plurality of outflow openings is larger than 2.5 times the transverse dimension of at least one of the two adjacent outflow openings. 15

76. Apparatus according to any one of claims 73-75, wherein the transverse dimension is a smallest transverse dimension.

77. Apparatus according to claim 76, wherein the smallest transverse dimension is a diameter.

78. Apparatus according to any one of claims 71-77, wherein a distance between 20 two adjacent outflow openings of the plurality of outflow openings is smaller than 5 times a transverse dimension of at least one of the two adjacent outflow openings.

79. Apparatus according to claim 78, wherein a distance between two adjacent outflow openings of the plurality of outflow openings is smaller than 4 times a transverse dimension of at least one of the two adjacent outflow openings. 25

80. Apparatus according to claim 78, wherein a distance between two adjacent outflow openings of the plurality of outflow openings is smaller than 3 times a transverse dimension of at least one of the two adjacent outflow openings.

81. Apparatus according to any one of claims 78-80, wherein the transverse dimension is a smallest transverse dimension. 30 82. Apparatus according to claim 81, wherein the smallest transverse dimension is a diameter.

Received at IPONZ on 5 April 2012 25

83. Apparatus according to any one of claims 71-82, wherein the plurality of outflow openings is arranged in a substantially ring-shaped formation.

84. Apparatus according to any one of claims 71-83, wherein the plurality of outflow openings is arranged in a formation comprising a plurality of substantially ring- 5 shaped sub-formations.

85. Apparatus according to any one of claims 71-82, wherein the plurality of outflow openings is arranged in a substantially straight line.

86. Spraying device of the apparatus according to any one of claims 50-85.

87. Method according to claim 1, substantially as herein described with reference to 10 any one of the Examples and/or Figures thereof.

88. Method according to any one of claims 1 to 38, substantially as herein described.

89. Powder according to claim 39, substantially as herein described with reference to any one of the Examples and/or Figures thereof.

90. Powder according to any one of claims 39-49, substantially as herein described. 15

91. Apparatus according to claim 50, substantially as herein described with reference to any one of the Examples and/or Figures thereof.

92. Apparatus according to any one of claims 50-86, substantially as herein described.