CN111644122A - Hot-melting spouted bed granulation device and method - Google Patents
Hot-melting spouted bed granulation device and method Download PDFInfo
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- CN111644122A CN111644122A CN202010356023.1A CN202010356023A CN111644122A CN 111644122 A CN111644122 A CN 111644122A CN 202010356023 A CN202010356023 A CN 202010356023A CN 111644122 A CN111644122 A CN 111644122A
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- spouted bed
- wall material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
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Abstract
The invention relates to a hot-melting spouted bed granulation device, which comprises a spouted bed, a negative pressure unit, an atomized gas supply unit, an atomization unit and a molten grease supply unit, wherein the top of the spouted bed is connected with the negative pressure unit, the negative pressure unit comprises an exhaust fan and a negative pressure pipeline, and the top of the spouted bed is connected with the exhaust fan through the negative pressure pipeline; the atomized gas supply unit comprises an air compressor, a gas storage tank and a gas heater which are sequentially connected through a high-pressure gas pipeline; the atomization unit comprises a two-fluid nozzle arranged at the bottom of the spouted bed, and a high-pressure gas pipeline is connected to the two-fluid nozzle at the bottom of the spouted bed from the gas outlet of the heater; the molten grease supply unit comprises a water bath and a peristaltic pump which are sequentially connected through a feed pipe, and the feed pipe is connected to a two-fluid nozzle of the spouted bed after passing through the peristaltic pump. The invention adopts a spouted bed with bottom spraying to granulate the wall material and the powder core material after melting, and realizes the controllability of the product shape by controlling the particle diameter ratio of the wall material to the core material.
Description
Technical Field
The invention belongs to the technical field of microcapsule preparation methods, and particularly relates to a hot-melt spouted bed granulation device and method.
Background
The microcapsule technology is a technology for embedding a core material to be protected into micro particles by using a wall material capable of forming a film, protects the core material from the influence of severe environment, and effectively exerts the bioactivity function of the core material. The microcapsule technology has the functions of changing the state and the property of the substance, protecting sensitive ingredients of food raw materials, covering bad smell, controlling the release of active substances and the like, and is widely applied to the industries of food, medicine, cosmetics, pesticides and the like. At present, the common microcapsule spray preparation methods comprise four methods of spray drying, spray congealing, spray coating and spray polycondensation.
Patent CN109806818A "a method for preparing microcapsules" discloses a method for preparing microcapsules in the field of microcapsule preparation, comprising the following steps: adding maltodextrin to water to obtain maltose liquid; adding an emulsifier into the obtained maltose liquid to perform microencapsulation to obtain microcapsule emulsion; stirring and molding the microcapsule emulsion; sucking the stirred and formed substances to obtain a finished product; packaging and selling the obtained finished product; the maltodextrin is added into water to obtain maltose liquid, the maltose liquid is added with emulsifier to be microencapsulated to obtain microcapsule emulsion, the microcapsule emulsion is stirred and formed and then is sucked to obtain a finished product, and the finished product is packaged and sold, so that the steps of the microcapsule process can be greatly reduced, the efficiency is improved, and the method can be used for preparing microcapsules.
Patent CN108936677A method for preparing probiotic microcapsules by spray drying discloses a method for preparing probiotic microcapsules by spray drying, which comprises the following steps of preparation of a culture medium; secondly, activating thalli; third, proliferation and heat shock of thalli: inoculating the activated thallus with the inoculation amount of 1%, culturing in a thermostat at 37 ℃, putting the culture dish into a constant-temperature water bath kettle at 60-80 ℃ after culturing for 11-13 hours, and carrying out water bath for 4-6 minutes; fourthly, concentration of thalli: pouring the heat-shocked culture solution into a sterilized tube, and placing the sterilized tube into a centrifuge, wherein the centrifuge is set to be at a rotating speed of 6000r/min and a temperature of 4 ℃ and the centrifugation time is 10 minutes; fifthly, preparing mixed suspension; sixthly, spray drying; and seventhly, packaging. The invention relates to the technical field of microorganisms. The method for preparing the probiotic microcapsules by spray drying solves the problem of high death rate of thalli caused by high temperature in a dryer, and ensures the viable count of bacterial powder.
Patent CN109589883A "a preparation method of plant essential oil powder microcapsule" provides a preparation method of plant essential oil powder microcapsule, which comprises preparation of plant essential oil, primary embedding of wall material, spray drying and secondary embedding of wall material. The preparation method comprises embedding plant essential oil in micropores with beta-cyclodextrin, and then embedding with zein or wheat gliadin attached membrane to form a completely closed structure with essential oil embedding rate of 80-88%. The stability of the plant essential oil at normal temperature and high temperature can be improved through secondary embedding, the volatility is reduced, and the high temperature resistance is enhanced.
At present, most of microcapsules are prepared by adding water and an emulsifier into raw materials to prepare a mixture, and then performing spray drying, so that the prepared product has poor purity, additives such as the emulsifier and the like still need to be removed in the later period, the process is complex, and the energy consumption is high.
Hot melt fluidized bed coating is a common technique for preparing microcapsules. The hot-melt fluidized bed coating is to coat fluidized core material with atomized molten material as wall material to prepare microcapsule. Hot melt fluid bed coating is a process that is a coupled of processes and is still an "empirical" unit operation that is not controllable with respect to product morphology and quality.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a hot-melting spouted bed granulation device and method, which utilize a physical method for granulation, do not add any emulsifier, have simple process, low process energy consumption and controllable product form.
The technical problem to be solved by the invention is realized by the following technical scheme:
a hot-melting spouted bed granulation device comprises a spouted bed, a negative pressure unit, an atomized gas supply unit, an atomization unit and a molten grease supply unit, wherein the top of the spouted bed is connected with the negative pressure unit, the negative pressure unit comprises an exhaust fan and a negative pressure pipeline, and the top of the spouted bed is connected with the exhaust fan through the negative pressure pipeline; the atomized gas supply unit comprises an air compressor, a gas storage tank and a gas heater which are sequentially connected through a high-pressure gas pipeline; the atomization unit comprises a two-fluid nozzle arranged at the bottom of the spouted bed, and a high-pressure gas pipeline is connected to the two-fluid nozzle at the bottom of the spouted bed from the gas outlet of the heater; the molten grease supply unit comprises a water bath and a peristaltic pump which are sequentially connected through a feed pipe, and the feed pipe is connected to a two-fluid nozzle of the spouted bed after passing through the peristaltic pump.
And, a layer of heating tape and heat preservation cotton twine outside the inlet tube.
Furthermore, the spouted bed is provided with a temperature sensor.
A hot melt spouted bed granulation apparatus comprising the steps of:
1) heating wall materials: the method comprises the following steps of putting a grease wall material which is solid at normal temperature into a water bath kettle, heating and melting the grease wall material into liquid, and conveniently spraying, wherein the temperature of the water bath kettle is set to be 10-15 ℃ higher than the melting point of the wall material, and keeping the temperature constant, so that the wall material is fully melted, and a feeding pipe is prevented from being blocked by a solidification phenomenon in a granulation process;
2) preheating a spouted bed: when the wall material of the oil and fat is fully molten, adjusting the temperature of a bed layer of the spouted bed to be 10-15 ℃ lower than the melting point of the wall material, and preheating the spouted bed;
3) adding a core material at the bottom of the spouted bed: adopting powder as a core material, and placing the core material into the bottom of the spouted bed when the interior of the spouted bed reaches a stable temperature;
4) core material fluidization: starting an exhaust fan, and adjusting the frequency of the fan to enable the core material to enter a fluidization state;
5) wall material atomization: starting a peristaltic pump, feeding the molten grease wall material into a two-fluid nozzle at a feed liquid flow rate of 4-8mL/min, mixing the molten grease wall material with fluidizing gas in a high-pressure gas pipeline in the two-fluid nozzle, and adjusting the atomizing pressure to be 0.2MPa to atomize the molten grease into liquid drops to be sprayed onto the fluidized core material;
6) and (4) completing granulation: and (4) the fluidized core material and the atomized liquid drops of the wall material are collided, wetted and coated to complete granulation.
The invention has the advantages and beneficial effects that:
1. according to the hot-melting spouted bed granulation device, the spouted bed is fluidized in a negative pressure manner, and the exhaust fan exhausts air to the spouted bed to enable the inside of the spouted bed to be in a negative pressure state; the atomizing air required by the two-fluid nozzle is provided by an air compressor, the oil wall material for spraying is heated and melted by adopting a water bath kettle, and the oil wall material is conveyed to the two-fluid nozzle by a feed pipe through a peristaltic pump for atomizing and spraying.
2. The hot-melt spouted bed granulation device provided by the invention has the advantages that the heating belt and the heat insulation cotton are wound on the outer side of the feeding pipe, so that the material is kept at a certain temperature before entering the two-fluid nozzle, and the feeding pipe and the nozzle are prevented from being blocked by oil solidification.
3. The hot-melt spouted bed granulation device is connected with a heater on an atomizing gas pipeline to heat atomizing air.
4. The hot-melting spouted bed granulation device provided by the invention performs granulation by using a physical method, does not add any emulsifier, reduces the solvent evaporation process, reduces the process energy consumption, has high product purity, and is not easy to damage nutritional ingredients.
5. According to the hot-melting spouted bed granulation method, the spouted bed with bottom spraying is adopted for granulation of the wall material and the powder core material after melting, the atomized wall material is directly contacted with the fluidized core material, the wall material is prevented from being solidified before contacting the core material, and the controllability of the product form is realized by controlling the particle diameter ratio of the wall material to the core material.
Drawings
FIG. 1 is a schematic flow diagram of a hot melt spouted bed granulation apparatus of the present invention;
FIG. 2 is an SEM photograph of particles obtained from 98-154 μm citric acid;
FIG. 3 is an SEM photograph of particles obtained from 250-315 μm citric acid
FIG. 4 is an SEM photograph of particles obtained from 400-500 μm citric acid
FIG. 5 is an SEM photograph of particles obtained from 500-630 μm citric acid
FIG. 6 is an SEM photograph (left) of particles obtained from 630-800 μm citric acid
FIG. 7 is an SEM photograph of an intra-particle section of the resulting particles of 630-800 μm citric acid (right)
Description of the reference numerals
The method comprises the following steps of 1-a water bath kettle, 2-an exhaust fan, 3-a flow meter, 4-a spouted bed, 5-a temperature controller, 6-a gas heater, 7-an air inlet, 8-an air storage tank, 9-an air compressor, 10-a pressure gauge, 11-a two-fluid nozzle and 12-a peristaltic pump.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
A hot-melting spouted bed granulation device comprises a spouted bed, a negative pressure unit, an atomized gas supply unit, an atomization unit and a molten grease supply unit, wherein the top of the spouted bed is connected with the negative pressure unit, the negative pressure unit comprises an exhaust fan and a negative pressure pipeline, and the top of the spouted bed is connected with the exhaust fan through the negative pressure pipeline; the atomized gas supply unit comprises an air compressor, a gas storage tank and a gas heater which are sequentially connected through a high-pressure gas pipeline; the atomization unit comprises a two-fluid nozzle arranged at the bottom of the spouted bed, and a high-pressure gas pipeline is connected to the two-fluid nozzle at the bottom of the spouted bed from the gas outlet of the heater; the molten grease supply unit comprises a water bath and a peristaltic pump which are sequentially connected through a feed pipe, and the feed pipe is connected to a two-fluid nozzle of the spouted bed after passing through the peristaltic pump.
And, a layer of heating tape and heat preservation cotton twine outside the inlet tube.
Furthermore, the spouted bed is provided with a temperature sensor.
A hot melt spouted bed granulation apparatus comprising the steps of:
1) heating wall materials: the method comprises the following steps of putting a grease wall material which is solid at normal temperature into a water bath kettle, heating and melting the grease wall material into liquid, and conveniently spraying, wherein the temperature of the water bath kettle is set to be 10-15 ℃ higher than the melting point of the wall material, and keeping the temperature constant, so that the wall material is fully melted, and a feeding pipe is prevented from being blocked by a solidification phenomenon in a granulation process;
2) preheating a spouted bed: when the wall material of the oil and fat is fully molten, adjusting the temperature of a bed layer of the spouted bed to be 10-15 ℃ lower than the melting point of the wall material, and preheating the spouted bed;
3) adding a core material at the bottom of the spouted bed: adopting powder as a core material, and placing the core material into the bottom of the spouted bed when the interior of the spouted bed reaches a stable temperature;
4) core material fluidization: starting an exhaust fan, and adjusting the frequency of the fan to enable the core material to enter a fluidization state;
5) wall material atomization: starting a peristaltic pump, feeding the molten grease wall material into a two-fluid nozzle at a feed liquid flow rate of 4-8mL/min, mixing the molten grease wall material with fluidizing gas in a high-pressure gas pipeline in the two-fluid nozzle, and adjusting the atomizing pressure to be 0.2MPa to atomize the molten grease into liquid drops to be sprayed onto the fluidized core material;
6) and (4) completing granulation: and (4) the fluidized core material and the atomized liquid drops of the wall material are collided, wetted and coated to complete granulation.
Example 1:
in this embodiment, the wall material is selected from: stearic acid, core material: and (4) citric acid.
The results of experiments performed with cores of 98-154 μm and 250-315 μm in FIGS. 1 and 2, respectively, are shown in SEM photographs. It can be seen from the figure that the particle growth resulting from both core/wall material ratios is an agglomeration mechanism. The proportion of the core material/the wall material is small, the core material and the wall material are combined in a fluidized bed in a random collision manner, the core material particles infiltrated by the wall material adhesive collide with surrounding particles, the wall material is used as a 'liquid bridge' to enable the particles to be adhered together, the 'liquid bridge' is solidified along with the increase of the fluidization time, and the particles are connected together through the 'solid bridge' to form irregular agglomerated particles as shown in the figure.
The results of experiments using 400-500 μm and 500-630 μm core materials in FIGS. 3 and 4 are shown in SEM photographs. It can be seen from the figure that the particles obtained by the two core material/wall material ratios are mixed with the coating, and the growth mechanism of the particles at the ratio is mixed with the aggregation and distribution. SEM photographs taken with core particles of larger particle size (630-. The proportion of the core material to the wall material is larger, the wall material binder is distributed on the surface of larger core material particles, the wetted particles are fluidized and collided in the fluidized bed, the binder is gradually solidified, new binder is distributed on the surface of the solidified particles again, and the binder coats the particles layer by layer to form compact and regular particles. SEM cross-sectional photographs of the particles are shown in fig. 6 (right), and it is apparent that the liquid binder is coated on the surface of the fluidized particles layer by layer.
Although the embodiments of the present invention and the accompanying drawings have been disclosed for illustrative purposes, those skilled in the art will appreciate that various substitutions, alterations, and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and thus the scope of the invention is not limited to the embodiments and drawings disclosed.
Claims (4)
1. The utility model provides a hot melt spouted bed prilling granulator which characterized in that: the device comprises a spouted bed, a negative pressure unit, an atomized gas supply unit, an atomization unit and a molten grease supply unit, wherein the top of the spouted bed is connected with the negative pressure unit, the negative pressure unit comprises an exhaust fan and a negative pressure pipeline, and the top of the spouted bed is connected with the exhaust fan through the negative pressure pipeline; the atomized gas supply unit comprises an air compressor, a gas storage tank and a gas heater which are sequentially connected through a high-pressure gas pipeline; the atomization unit comprises a two-fluid nozzle arranged at the bottom of the spouted bed, and a high-pressure gas pipeline is connected to the two-fluid nozzle at the bottom of the spouted bed from the gas outlet of the heater; the molten grease supply unit comprises a water bath and a peristaltic pump which are sequentially connected through a feed pipe, and the feed pipe is connected to a two-fluid nozzle of the spouted bed after passing through the peristaltic pump.
2. A hot melt spouted bed granulation device as defined in claim 1, wherein: and a layer of heating tape and heat insulation cotton are wound outside the feeding pipe.
3. A hot melt spouted bed granulation device as defined in claim 1, wherein: the spouted bed is provided with a temperature sensor.
4. The utility model provides a hot melt spouted bed prilling granulator which characterized in that: the method comprises the following steps:
1) heating wall materials: the method comprises the following steps of putting a grease wall material which is solid at normal temperature into a water bath kettle, heating and melting the grease wall material into liquid, and conveniently spraying, wherein the temperature of the water bath kettle is set to be 10-15 ℃ higher than the melting point of the wall material, and keeping the temperature constant, so that the wall material is fully melted, and a feeding pipe is prevented from being blocked by a solidification phenomenon in a granulation process;
2) preheating a spouted bed: when the wall material of the oil and fat is fully molten, adjusting the temperature of a bed layer of the spouted bed to be 10-15 ℃ lower than the melting point of the wall material, and preheating the spouted bed;
3) adding a core material at the bottom of the spouted bed: adopting powder as a core material, and placing the core material into the bottom of the spouted bed when the interior of the spouted bed reaches a stable temperature;
4) core material fluidization: starting an exhaust fan, and adjusting the frequency of the fan to enable the core material to enter a fluidization state;
5) wall material atomization: starting a peristaltic pump, feeding the molten grease wall material into a two-fluid nozzle at a feed liquid flow rate of 4-8mL/min, mixing the molten grease wall material with fluidizing gas in a high-pressure gas pipeline in the two-fluid nozzle, and adjusting the atomizing pressure to be 0.2MPa to atomize the molten grease into liquid drops to be sprayed onto the fluidized core material;
6) and (4) completing granulation: and (4) the fluidized core material and the atomized liquid drops of the wall material are collided, wetted and coated to complete granulation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010356023.1A CN111644122A (en) | 2020-04-29 | 2020-04-29 | Hot-melting spouted bed granulation device and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010356023.1A CN111644122A (en) | 2020-04-29 | 2020-04-29 | Hot-melting spouted bed granulation device and method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113304050A (en) * | 2021-06-07 | 2021-08-27 | 南京望知星医药科技有限公司 | Production equipment and method of roxithromycin microcapsules |
| CN115153022A (en) * | 2022-05-25 | 2022-10-11 | 无锡利必多生物科技有限公司 | Completely-coated fish oil microcapsule and preparation method thereof |
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| US4353709A (en) * | 1979-11-28 | 1982-10-12 | Mitsui Toatsu Chemicals, Incorporated | Granulation process |
| CN2406721Y (en) * | 2000-01-22 | 2000-11-22 | 邹龙贵 | Granulating and dressing apparatus |
| CN1293175A (en) * | 2000-09-29 | 2001-05-02 | 泸天化（集团）有限责任公司 | Fluidized gramulating process of heterogeneous urea-base compound fertilizer |
| CN201124091Y (en) * | 2007-11-30 | 2008-10-01 | 山东建筑大学材料科学研究所 | Negative-pressure fluidized-bed for experiment |
| CN101462907A (en) * | 2009-01-13 | 2009-06-24 | 北京市农林科学院 | Coated compound fertilizer and preparation thereof |
| CN206045962U (en) * | 2016-08-03 | 2017-03-29 | 中山市易美尔纺织助剂有限公司 | High tower grit blast crystal system |
| CN107321276A (en) * | 2017-06-16 | 2017-11-07 | 天津科技大学 | A kind of controllable heat fusing fluid bed microcapsules preparation system of product quality and preparation method |
-
2020
- 2020-04-29 CN CN202010356023.1A patent/CN111644122A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4353709A (en) * | 1979-11-28 | 1982-10-12 | Mitsui Toatsu Chemicals, Incorporated | Granulation process |
| CN2406721Y (en) * | 2000-01-22 | 2000-11-22 | 邹龙贵 | Granulating and dressing apparatus |
| CN1293175A (en) * | 2000-09-29 | 2001-05-02 | 泸天化（集团）有限责任公司 | Fluidized gramulating process of heterogeneous urea-base compound fertilizer |
| CN201124091Y (en) * | 2007-11-30 | 2008-10-01 | 山东建筑大学材料科学研究所 | Negative-pressure fluidized-bed for experiment |
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| CN206045962U (en) * | 2016-08-03 | 2017-03-29 | 中山市易美尔纺织助剂有限公司 | High tower grit blast crystal system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113304050A (en) * | 2021-06-07 | 2021-08-27 | 南京望知星医药科技有限公司 | Production equipment and method of roxithromycin microcapsules |
| CN115153022A (en) * | 2022-05-25 | 2022-10-11 | 无锡利必多生物科技有限公司 | Completely-coated fish oil microcapsule and preparation method thereof |
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