TWI237577B - Method and device for spray drying granulation - Google Patents

Abstract

A method for spray-drying granulation can be used to obtained a powder obtained by agglomeration of solid particles by spraying and drying a dispersion solution of solid particles in a spray-drying chamber. The spray-drying chamber is formed of a bag-shaped or cylindrical porous film, which is heat resistant and has a good peeling property. During a spray-drying operation, the dispersion solution of solid particles is atomized and a hot wind is used to remove solvent from the dispersion solution. Meanwhile, a dry exhaust portion containing an agglomeration of the dried solid particles passes through the porous film in the spray-drying chamber. Thus, all powder particles are contained in the spray-drying chamber. Furthermore, during the spray granulation process, while maintaining the volume of the spray-drying chamber, the internal pressure of the spray-drying chamber is controlled at about 0 to the negative pressure so that the powder gas spirals in the spray-drying chamber to form particles with a specified particle size.

Description

1237577 V. Description of the invention α) Technical field to which the invention belongs Granulation method and spray drying The present invention relates to a spray drying and granulation device. Previous technologies Today, spraying production methods have increased the number of types required. Many kinds of cleaning must be done frequently when the interior is clean and high quality is needed. However, if the product is in the product, it will be cleaned again. If it is made, it is known in the product bureau to solve the problem shown in Figure 5. The multi-spray drying chamber fog drying method and device, from a small number of species and a large number of products since the knowledge to the products of medical music, exquisite pottery and so on, and require a small amount of production methods, and products that require relatively high purity When manufacturing a high-purity product using a small-scale production method, due to the replacement of the compulsory species, the solid matter attached to the wall must be completely and quickly washed each time. In the case of small-scale production of various types, it is a fatal shortcoming, and the quality of the product requires high purity and the solid matter attached when the quality is switched must be completely washed. It is extremely difficult to clean the solid objects attached to the interior of the drying room. In situations that are harmful to the human body, it is more difficult to directly contact the product. In the case where various types of small-scale production methods and the production of high-purity products are required, the separation of product components that are not a problem is also a problem due to the demand for degree of improvement. For the above problems, the present invention takes a spray drying device as an example. For example, the spray drying chamber is formed by a single bag-shaped or tube-shaped heat resistance and a porous film, and the porous film for exhaust is dried from the formed inner side toward the inner side. The outside passes through, thus the spray drying method and equipment

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1237577 V. Description of the invention (3) The state of sadness) 'will become a void, and there will be a volume and 100 // m or more. In view of the fact that when a spray drying and separation of raw materials are separated and the type is changed, the product may be caused by the peeling of the spray particles even if the spray density is larger than the bulk density of the heavier particles. In the same journey, it is expected to achieve the degree of equipment. In the inside of the dried material (particles) of the buckle, the problem of reduction in β degree is easy to occur. Especially for powders with a heavier specific gravity ^ Due to the fast falling speed, this tendency is that even if the granulation method by the obvious technology is accompanied by rapid and powder, the powder can be lifted to the section with a strange absorption rate in the drying chamber. The device can be easily replaced with a variety of types of valleys, and at the same time, it will be reduced, and the powder particles will be sprayed to save space. This invention is a problem. Coarse granules above the micro-powder washing and drying granules attached to a small amount of spray-dried production side will not be produced during spray granulation. Even when dry due to the high-efficiency of dry-can engineering and products, it is frequently cleaned and retained. As time-drying is changed from fixing the same component to spray-forming, the quality is provided so that it will not fall off in a complicated manner, and time, the interior of the drying room is divided into a series of granules, and Nanchun. SUMMARY OF THE INVENTION The present invention provides a spray-drying In the drying chamber, the solid particle dispersion solution is used as the second method, and the powder obtained by agglomeration of the spray dried particles is characterized by :, and, drying: solid heat resistance and good peelability of the porous solid particles can be obtained ^ The spray-drying chamber is composed of a bag or a tube, and the solid particle dispersion solution is sprayed. When the spray-dried powder solution is removed from the solvent and dried, hot air is used to separate the solid particles from the solid particles. Solid particles

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1237577 It is provided in a spray-like shape and is held in the spray. The internal pressure of the solid drying chamber will be removed, and the internal pressure of the pressure-compressed porous membrane spray granulation in the separation and drying chamber will be removed from the side where the spray passes. The spray holder of the ground protection, the hot air body part of the spray is outdoor, the spray discharges the dry air outward so that this side, and the dry exhaust part of the powder room gas is passed through the spray film to form the spray film Therefore, when the powder spray granulation is obtained in the spray drying chamber, the internal pressure of the mist-drying chamber of the spray drying chamber is maintained from about 0 to a negative pressure while the powder gas is maintained in the spray drying chamber. The spray-dried powder swirled in the chamber. When granulating, the internal pressure of the spray drying chamber is preferably -200. V. Description of the invention (4) The total amount of the porous material in the drying chamber of the powder is agglomerated, and in the state of accumulation, the spraying At the same time of control, it can be produced with a predetermined particle size at this time. At the time of spraying ~ + 2 0 P a 〇 Also, the present invention provides a single bag or tube drying chamber, which is kept in the drying chamber and introduced into the dry chamber. Device, dry exhaust from the side in the spray-drying chamber, and in the spray-drying chamber, the drying exhaust holder in the hair dryer is preferably a fog-drying and granulating device, including the whole Drying chamber with a predetermined shape of the drying chamber formed by the porous film with good properties and good peeling properties. The particle dispersion solution is sprayed into fine droplets, and the hot air dried by the fine droplets is introduced into the powder gas in the spray drying chamber. The powder is dried. Exhaust gas is discharged to the exhaust device provided in the spray-drying detachable unit to adjust the force adjustment device. During spray-drying, when the formed spray-drying room passes through, the exhaust device and the pressure are installed to about 0. It becomes negative pressure and controls. In the case of mist granulation, the side wall of the spray drying chamber is preferably detachably arranged, and the spray drying chamber is also supported.

2033-5789-PF (Nl); Chentf.ptd Page 9 V. Description of the invention (5) Embodiments The mouth mist of the present invention is dry. In the granulation method, the heat resistance of the bag and tube and good peelability The completed spray drying chamber will be sprayed with a seven-hole plasma membrane (original liquid), and the solid particle dispersion solution (for example, 120 ~ 28 t) from the mist of the service chamber will be blown into the device. Inlet gas temperature solid particles are aggregated: the hot air of the body is heated and dried instantly, and the above-mentioned powder becomes dry. At the same time, the bottom of the spray drying chamber is composed of the upper part and the lower part of the spray drying chamber. Yoshinobu Sekiyoshi ^ yttrium buckle drains the flood, by passing the full amount of powder. In the spray drying room, Xibei can obtain * ,: the separation of the powder and the dry exhaust fiber. The fiber mesh can be separated by passing through the powder constituting the porous membrane. One 'beans can make the granite ants 1 ～~ several hits-the next two i! Mingzhi spray drying. Granulation method, in the field of spray granulation: 2L drying chamber volume state, spray drying chamber The internal pressure of about 0% becomes negative pressure to be controlled. In the spray drying room, the powder gas is introduced into a swirling flow to introduce 'because it can ensure the π side time of dry granulation, even the powder with specific gravity. Coarse granules with a particle size of 100 or more can achieve a high density of dry granules. At the same time, during spray mist granulation, the spray granules adhere to the inner wall of the drying chamber, which reduces the yield. Formation of fancy powders caused by the exfoliation of mist particles. Even the spray drying and granulation method of the present invention, the granulation method, in the same ingredient system 2033-5789-PF (Nl); Chentf.ptd 1237577 V. Due to the spray drying process and spray in the product of the invention description (6) The granulation process can be performed in the same drying chamber, and it is expected that space saving of the device and high-quality and high-purity products can be achieved. Next, the spray drying and granulation apparatus of the present invention will be described with reference to the drawings. Fig. 1 is an example of a spray-drying and granulating apparatus according to the present invention, and is a schematic cross-sectional view showing an embodiment during spray-drying. Fig. 2 is a schematic sectional view showing an embodiment of spray granulation. The spray-drying and granulation device of the present invention has a spray-drying chamber 2 formed of a single bag-shaped or cylindrical heat-resistant and well-peelable porous film as shown in Figs. 1 and 2, A spray chamber 3 for holding the spray drying chamber in a predetermined shape of the drying chamber holders 20, 22, and 24, and spraying the solid particle dispersion solution into fine droplets in the spray drying chamber 2, and in the spray drying chamber 2 The hot air introduction device 4 that introduces hot air for drying minute droplets separates the powder portion in the powder gas in the spray drying chamber 2 from the dry exhaust gas, and discharges the dry exhaust gas to the outside of the spray drying chamber 2. An exhaust device 40 detachably disposed in the spray drying chamber 2 and a pressure adjusting device (not shown) that adjusts the pressure in the spray drying chamber 2. Here, the spray-drying and granulating device of the present invention, in the case of spray-drying, as shown in Fig. 1, a spray-formed bag-shaped or cylindrical-shaped porous film having heat resistance and good peelability is formed. In the mist drying chamber 2, the solid particle dispersion solution (original liquid) sprayed by the sprayer 3 passes through the hot air instant of the inlet gas temperature (for example, 1 2 0 ~ 2 0 0 ° C) blown from the hot air introduction device. It is dried by heating and becomes a powder (fine powder) of agglomerated dry solid particles.

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V. Explanation of the invention (7) While the above powder sinks the bottom of the spray-drying chamber by most of its own weight, the dry exhaust portion of the powder gas containing the above-mentioned powder passes through the porous material constituting the spray-drying chamber. The film 'f' obtained the entire amount of the powder in the spray-drying chamber. In the case of spray-drying, the internal pressure of the spray-drying chamber 2 becomes +200 to 1,200,000 pa. In the state of the spray-drying and spray-granulation of the present invention, as shown in FIG. 2 After switching from the first product recovery unit 16 (refer to the first figure) to the second product recovery unit 18, the exhaust device 40 is connected to the exhaust port of the product recovery unit 18, and the spray drying chamber 2 is inside The pressure changes from about 0 to negative pressure. Based on the measurement result of the differential waste meter, it is controlled by a pressure adjustment device. In this way, the dry exhaust gas in the spray drying chamber 2 is introduced into a swirling flow (refer to Figure 2). Arrow) ° With this, the dried granulated material and the sprayed granules are slowly dropped by the swirling flow of the dried exhaust gas, and the sprayed granules contact the dried exhaust gas to be spray granulated. Here, the spray drying chamber 2 is provided with drying chamber holders 20, 22, and 24 respectively arranged on the holding frame 10, and the four sides of the upper, middle, and lower portions of the spray drying chamber 2 are engaged with the holding frame 10 . By this means, even when the inside of the spray drying chamber 2 becomes a negative pressure, the spray drying chamber 2 can maintain a predetermined shape. The spray drying chamber 2 is suspended from the inside of the holding frame 10, and can be moved up and down by the elevator 30. Also, the holding frame 10 is preferably provided with a side wall that inhibits the passage of dry exhaust gas.

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The device ^ spray "is suitable for :; disc) and the 3 ~~: from the spray i spray: ΐ3 mist ~ 4; in the device 'in the spray drying chamber 2, the hot air is introduced, please contact Disperse the solution (original liquid) of the wind body, and exchange heat with the slave. "Convection contact, which can make an efficient exhaust device 40 by rotary, household cry (blower) 46, spray dry;:! The rear filter 44 and the exhaust fan are -2 0 0 to + 20 Pa), Chun; the internal pressure from 2 to 2 changes from about 0 to negative pressure (the most powerful adjustment device for control. According to the differential pressure gauge 50% Measurements and results, when used in the present invention, when the far green porous membrane is…, 'from: powder adheres and accumulates on the appropriate sweep down powder is not possible =' finally does not stop and does not stop operation 'therefore ^ 乂^ ^ ^ TtVm Im% ^ ^ ^ ^ ^ ^ ^ ^ ^; can be applied more closely = 彳 drying room " completely cleaned. X The porous membrane used must be heat resistant and compatible with

1237577 V. Description of the invention (9) The powder has excellent peelability. That is, the temperature of the hot air introduced into the spray drying room is generally 120 ~ 280 ° C at the inlet and 70 ~ 150 ° C at the outlet, so it must be able to withstand this temperature. In addition, the powder often adheres and is easy to accumulate, and it must have good peelability due to continuous use. Even the porous membrane used in the present invention separates the resulting powder from the dry exhaust gas. As a porous membrane having such a function, a specific type is not limited, and a mesh-like [, gland fabric, woven fabric or τ y] having a good peelability from powder is generally used as a strength material. 、, amine. ^ ^ Non-woven) composition for the above mesh-like film, for example, polytetrafluoroethylene mouth name · Teflon (polytetrafluoroethylene) series film, polytrifluoroethylene series film, as P but FE ] (Commercial filter cloth, for example, polyimide, heat-resistant nylon, polyester, is more suitable for the above-mentioned heat resistance. Huoxiang polyamine products below, the present invention will be described in more detail according to the examples, but is not limited to these The embodiment of the present invention

After using the spray-drying and pelletizing adhesive PVA (20 7) in the amount shown in Figure 2 to adjust the barium tungstate material '2.0% 65%), use -20 ~ + 20Pa ( -2.〇 ~, 'water (internal pressure of the slurry concentration drying chamber, spray-dried in the spray-drying chamber · 〇mniAq) separately adjusted to make granulated powder. To 2, by From the top, the temperature of the hot air is 200 ° C, the number of revolutions of the atomizing cry 9c 5, rpm, mud

1237577 V. Description of the Invention (ίο) The amount of slurry spray is 10OKg / hour. Next, the relationship between the bulk density and the internal pressure of the drying chamber in each of the granulated powders obtained is shown in Fig. 6. In addition, using granulated powder having a bulk density of 1.53Kg / 1, the change over time (the number of samples: 150) of the molding monomer during spin spray molding is shown in Section 7 (a), 7 (b), 7 (c). In the comparative example, a spray drying / granulation device shown in FIG. 5 was used, and 2.0% by mass of a binder PV A (207) was added to a slurry of barium tungstate (the slurry concentration was 65%). After the adjustment, in the spray-drying chamber 2 after the adjustment, the granulated powder is produced by spraying the slurry. The hot air temperature was 200 ° C, the number of revolutions of the atomizer 25 was 50 000 r p m, and the amount of mud spray was 10 OKg / hour. Next, the relationship between the bulk density and the internal pressure of the drying chamber in each of the granulated powders obtained is shown in Fig. 6. In addition, using granulated powder having a bulk density of 1.46 Kg / I, the change over time of the molding monomers during the rotary spray molding (the number of samples: 2.5) is shown in Section 8 (a) , 8 (b), 8 (c). As shown in FIG. 6, in the embodiment, in the embodiment, the slurry is sprayed in the spray drying chamber 2 adjusted with a drying chamber pressure of -20 to + 20 Pa (-2.0 to + 2.0 mmAq). Compared with the comparative example, while the bulk density of the granulated powder is increased, the process of forming a negative pressure in the spray drying chamber increases the density of the granulated powder significantly.

2033-5789-PF (Nl); Chentf.ptd Page 15 1237577 V. Description of the invention (11) Book 3 35: In the granulated powder obtained in the example, the single I # in continuous molding has little change in gravity, and the molding Conditions cannot be adjusted and can be continuously formed. The method of availability in the early-body industry and its installation are accompanied by rapid timeliness, that is, the space saved by the granules in the drying and peeling is transmitted through the above description. The spray drying and granulation method of the present invention is not applicable during spray drying. Separation of composition occurs, and even when frequent types are switched in a variety of small-scale production methods, washing and sweeping of finely adhered particles can be easily performed, and spray granulation makes the specific gravity of powder and 丨 0 Coarse particles greater than 0 # m can increase the dry bulk density and reduce the yield due to the spray particles 卩 = ^ indoor wall during spray granulation, and there is no strange-shaped powder produced by the fixed particles. It is expected to achieve the formation of wear-through, high-quality and high-purity products. Lang

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1237577 Brief Description of Drawings Fig. 1 shows an example of a spray-drying / granulation device according to the present invention, and is a schematic cross-sectional view showing an embodiment during spray-drying. Fig. 2 shows an example of a spray-drying / granulation apparatus according to the present invention, and is a schematic cross-sectional view showing an embodiment during spray-drying. FIG. 3 shows another example of the spray-drying and granulation apparatus of the present invention, and shows a schematic cross-sectional view of an embodiment during spray-drying. FIG. 4 shows another example of the spray-drying and granulation apparatus of the present invention, and shows a schematic cross-sectional view of an embodiment during spray-drying. Fig. 5 is a schematic cross-sectional view showing an example of a spray drying apparatus. Fig. 6 is a graph showing the relationship between the bulk density in the obtained granulated powder and the pressure in the drying chamber. Figures 7a, 7b, and 7c show the change over time of the weight of the monomers of the molded body formed by the rotary spraying using the granulated powder with a bulk density of 1.5 3 kg / 1 obtained in the examples (the number of samples: 1 5 0) Figure. Figures 8a, 8b, and 8c show the change over time of the weight of the monomers of the molded body formed by the rotary spray using the granulated powder of 1. 4 6 kg / 1 obtained in the example (the number of samples: 2 5 0) Figure. Explanation of symbols 2 ~ spray drying chamber; 3 '-sprayer; 4' hot air introduction device; 8 ~ exhaust port; 10 ~~ holding frame; 12 ~ side wall; 16 '~ first product recovery section; 18 ~ second product Recovery section 25 '~ sprayer; 26 ~ spray nozzle;

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Claims (1)

I eight! ^ A method of spray granulation, by spraying and drying solid particles: knife ^ = liquid in a spray drying chamber to obtain a powder obtained by agglomeration of solid particles, which is characterized by: Xi: Pi i ΐ f drying chamber It is made of 20% of bag-shaped or tube-shaped heat resistance and good peelability. During spray drying, #solid particle dispersion solution is used as a blast to remove the solvent from the solid particle dispersion solution and dry it. @ = = Dry Two points of the powder gas of the powder agglomerated by the solid particles pass through the porous film constituting the spray drying chamber, thereby obtaining the entire amount of the powder in the drying chamber ..., in the spray granulation 1 ί:!: In the state of the volume of the spray drying chamber, the spray drying chamber is controlled to a negative pressure while controlling, and the powder_% & mist drying chamber is rotated to produce a tool. Powder with a predetermined particle size. In the spray granulation method described in item 1 of the Lolli range, the internal pressure of the spray drying chamber when f k granules is -200 ~ + 20 Pa. 3. —A kind of spray granulation device, including: a spray-drying chamber, the entire office is equipped with a peelable porous structure; a tube-shaped pair of heat 2 :: a holder is used to maintain the predetermined set of the spray-drying chamber Shape; small droplets; β spraying the solid particle dispersion solution into the micro-hot air introduction in the drying chamber; f hot air introduction; and 1 inside the drying chamber, the tiny droplets are dried and dried. The powder part in the powder gas in the spray drying room, the knife is off, and the dry exhaust is discharged to the spray drying room. Ϊ237577 -t ^ L20m . The spray drying chamber is detachably arranged; and a pressure adjusting device adjusts the pressure in the spray drying chamber; when drying, the dry exhaust gas is formed from a porous film and dried to pass through the inside It is discharged to the outside, and during spray granulation, the exhaust pressure and the pressure device are used to control the internal pressure of the spray drying chamber from about 0 to negative pressure. 4. The spray granulation device according to item 3 of the scope of the patent application, wherein during spray granulation, a side wall of the spray drying chamber is detachably provided with a side wall which inhibits the passage of the dry exhaust gas. ^ 5 The spray granulation device as described in item 3 of the scope of patent application, wherein the drying chamber holder is configured to detachably hold the spray drying chamber. 6. The spray granulation device according to item 4 of the scope of the patent application, wherein the drying chamber holder is used to detachably hold the spray drying chamber. Page 20 2033-5789-PFl (Nl) .ptc