Fluidized bed granulation process and device for online regulation and control of particle size and moisture of particles

Abstract

The invention provides a fluidized bed granulation process and device for online regulation and control of particle size and moisture of particles, and belongs to the technical field of fluidized bed granulation. The fluidized bed granulation process specifically comprises the following steps: firstly, presetting a material target particle size, a material control temperature and a minimum material temperature, adopting a four-stage granulation process, and realizing online regulation and control on the material particle size and moisture by controlling the air inlet volume and the air inlet temperature; the process is realized by installing an anemograph behind an air inlet valve on an air inlet pipe of an existing fluidized bed granulation drying device, installing a near-infrared probe on a material tank window and installing a temperature probe in the middle, the transformation difficulty is small, air volume and temperature control in the whole granulation process can be achieved, and online monitoring of the particle size and moisture of particles in the whole process can be achieved. The obtained products are small in batch difference and good in reproducibility, the stability of the product quality is further guaranteed, the purpose of saving energy can be achieved by monitoring the air inlet volume and the temperature, and the method is suitable for actual production.

Description

Technical Field

[0001] The invention belongs to the technical field of fluidized bed granulation, and relates to a fluidized bed granulation process and a device for online regulating particle size and moisture. Background Art

[0002] Fluidized bed granulation is also called one-step granulation. The traditional fluidized bed granulation process is feeding → material heating → spraying → drying → discharging. The whole process is carried out in a closed container and granulation is completed in one step. Its principle is: in the fluidized bed granulator, compressed air and adhesive solution are atomized by the nozzle in a certain proportion and sprayed onto the material powder in the fluidized state on the fluidized bed. First, the droplets wet the contacted powder and agglomerate around it to form particle nuclei. At the same time, the droplets that continue to be sprayed fall on the surface of the particle nucleus to produce a bonding bridging effect, so that the particle nuclei and the particle nuclei, and the particle nuclei and the particles are combined with each other, gradually forming larger particles.

[0003] In the field of drug granulation, especially traditional Chinese medicine granulation, the fluidized bed granulation process generally has the problem of "bed collapse", that is, during the granulation process, powders and small particles, small particles and small particles stick to each other due to high moisture content, first sticking into large particles or large agglomerates, and the fluidization state gradually slows down, or they stick together due to preheating and softening, eventually leading to "bed collapse", resulting in large differences between batches of preparation particles, uneven particle quality and other problems.

[0004] Chinese utility model patent CN211358737U discloses a fluidized bed top spray granulation system, including an air intake treatment device, a fluidized bed boiling granulation dryer, a negative pressure fan and a positive pressure fan. The system adopts positive pressure air supply, which can effectively make up for the uneven air flow at the bottom of the existing fluidized bed hopper, avoid the defects of caking and bed collapse at the position of slow flow rate, reduce the blockage of filter bags due to the large amount of fine powder flying upward under negative pressure, improve product quality and production efficiency, and avoid product scrapping. However, the device needs to adjust the positive pressure delivery or negative pressure air supply according to the state of the particles in the fluidized bed granulation process, requires manual monitoring, and has certain difficulties in operation.

[0005] Chinese utility model patent CN20986594U discloses a top spray granulation fluidized bed with anti-collapse bed, in which a powder spraying device is connected to the material chamber of the tank body, and lubricants and anti-sticking agents such as talcum powder, magnesium stearate, silicon dioxide, starch, etc. are sprayed into the powder inlet of the powder spraying device to eliminate the adhesion between powders or particles, thereby preventing the occurrence of bed collapse. However, during the granulation process, it is still necessary to determine what kind of powder to add to eliminate the adhesion between particles according to the state of the particles.

[0006] In addition, the transformation of the above-mentioned device also has certain difficulties. Chinese invention patent application CN115957256A discloses a method for preparing Shaoyao Gancao Decoction granules, in which an excipient is placed in a fluidized bed chamber as a solid material, and Shaoyao Gancao Decoction extract or a mixed clear paste prepared from Shaoyao Gancao Decoction extract is used as a liquid material for fluidized bed granulation, and fluidized granulation is performed in a fluidized bed granulator through a compression spray gun. The obtained granule particle size meets the standard of the Chinese Pharmacopoeia particle size, and the quality is uniform and stable. When the mixed clear paste is used as the liquid material for fluidized bed granulation, granules with consistent quality between batches can be obtained; and by the ratio of the amount of the mixed clear paste to the amount of the solid material, the particle size and yield can be guaranteed, and the collapse of the pot and adhesion will not occur. This process requires the extract to be made into a clear paste, which increases the operation steps and is less efficient.

[0007] Based on the above defects of fluidized bed granulation technology, in order to improve the "bed collapse" problem in the fluidized bed granulation process, it is urgent to develop a device or process that can monitor online and adjust the particle state in real time. Summary of the invention

[0008] In view of the above-mentioned problems existing in the prior art, the present invention provides a fluidized bed granulation process and device for online regulation of particle size and moisture content. By regulating the wind speed, temperature and spraying process during the fluidized bed granulation process, the particle moisture content, particle size and bulk density are adjusted online, thereby achieving batch-to-batch particle consistency and process reproducibility, thereby ensuring product quality.

[0009] To achieve the above object, the technical solution of the present invention is as follows:

[0010] The present invention provides a fluidized bed granulation process for online regulating the moisture content and particle size of particles, comprising the following steps:

[0011] (1) Slurrying: Add the binder into water and fully dissolve it to obtain a binder slurry;

[0012] (2) Feeding: placing the plant extract and filler in the material trough of the fluidized bed and introducing air to make the materials in a fluidized state;

[0013] (3) Material heating: Set the air volume and air temperature to heat the material;

[0014] (4) Granulation: Granulation is performed through a four-stage granulation process, specifically: the target particle size range of the material for each stage of granulation, the material control temperature and the minimum material temperature during the granulation process are preset; the air volume and air temperature are set at the same time, and when the material temperature reaches the preset material control temperature range, spraying is started for granulation, and when the particle size of the material reaches the preset material target particle size range of the stage, the next stage of granulation is started until the four-stage granulation is completed;

[0015] (5) After granulation, the material is dried, granulated and sieved to obtain the product.

[0016] Those skilled in the art should understand that step (1) pulping and step (2) feeding are relatively independent steps and there is no order of precedence. Pulping can be performed first and then feeding, or feeding can be performed first and then pulping, or pulping can be performed while feeding.

[0017] Those skilled in the art should understand that step (2) feeding and step (3) material preheating are interconnected steps. In principle, step (2) feeding should be implemented first, and step (3) material preheating should be started after the feeding is completed. Of course, in the fluidized bed granulation process of the present invention, step (3) material preheating can also be implemented at the same time as step (2) feeding.

[0018] Furthermore, in step (2), the air volume is 2800-6500m 3 / h, preferably 3000-6500m 3 / h.

[0019] Furthermore, step (2) also includes: setting the inlet air moisture content ≤ 8%, the bag shaking time to 5-20s, and the bag shaking interval time to 20-60s; the inlet air moisture content, bag shaking time and bag shaking interval time are continuously executed until the granulation is completed.

[0020] Furthermore, in step (3), the air volume is 3000-4500m 3 / h, preferably 3200-4500m 3 / h; the inlet air temperature is 75-90℃, preferably 80-85℃.

[0021] Furthermore, during the granulation process of step (4), when the material temperature is lower than the minimum material temperature, the spraying is stopped; when the material temperature reaches the material control temperature again, the spraying is started until the particle size of the material reaches the target particle size range preset in this stage, and then the next stage of granulation is started.

[0022] Furthermore, in step (4), the target particle size range of the material particles in the four-stage granulation is:

[0023] Stage 1: The proportion of materials passing through 80 mesh is less than 90% and the proportion of materials passing through 200 mesh is less than 85%;

[0024] The second stage: the proportion of materials passing through 80 mesh is less than 80% and the proportion of materials passing through 200 mesh is less than 45%;

[0025] The third stage: the proportion of materials passing through 80 mesh is less than 50% and the proportion of materials passing through 200 mesh is less than 30%;

[0026] Stage 4: The proportion of materials passing through 80 mesh is less than 35% and the proportion of materials passing through 200 mesh is ≤ 25%.

[0027] Through the reasonable control of the four-stage particle size range, combined with the adjustment of air volume and temperature, the granulation requirements can be met more quickly, the entire process time can be shortened, and the preparation efficiency can be greatly improved.

[0028] Furthermore, in step (4), the air inlet temperature is 80-90°C; the material control temperature is 45-55°C; and the minimum material temperature is 35-37°C.

[0029] Furthermore, step (4) also includes setting the atomization pressure to 3.0-4.0 bar.

[0030] In some specific embodiments of the present invention, in the four-stage granulation process, the initial air volume of the spraying is 4000-5400m 3 / h and 150-250m per stage 3 / h increases in gradient, the initial slurry speed is 100-150rpm and decreases in gradient by 8-15rpm per stage. The purpose of setting the lowest air volume and the highest slurry speed in the first stage of granulation is that under this condition, the material in the material tank can be in a good fluidized state and the material is all at the bottom of the spray gun and will not be higher than the spray gun so that the slurry cannot contact the material, which eventually leads to uneven granulation; at the same time, the granulation efficiency can also be improved under this process condition.

[0031] In some preferred embodiments of the present invention, in the four-stage granulation process, the initial air volume of the spraying is 4500m 3 / h and 200m per stage 3 The initial rotation speed of the slurry was 150 rpm and then decreased by 10 rpm in each stage.

[0032] Furthermore, in step (5), the air inlet temperature is set to 80-85°C and the air inlet volume is set to 4000-4800m 3 / h, so that the material is in a good fluidized state and heated to 45-55℃ for drying, and the drying is stopped after the moisture content of the material reaches 2.0-3.5%.

[0033] In some embodiments of the present invention, the granulation and screening in step (5) is to screen the dry granules through a 1.0-2.5 mm cone granulator.

[0034] The plant extracts applicable to the fluidized bed granulation process of the present invention include, but are not limited to, kudzu root extract, milk thistle extract, schisandra extract, calendula extract, scutellaria extract, salvia extract, sanguisorba officinalis extract, centella asiatica extract, honeysuckle extract, polygonum multiflorum extract, chamomile extract, rutin extract, eucommia extract, poria extract, forsythia extract, ginseng extract, codonopsis extract, aloe extract, sophora flavescens extract, ganoderma lucidum extract, evodia rutaecarpa extract, lotus seed extract, phellodendron extract, atractylodes macrocephala extract, American ginseng extract, Cistanche deserticola extract, safflower extract , saffron extract, purslane extract, fangfeng extract, qinjiao extract, notopterygium extract, angelica extract, angelica extract, wormwood extract, achyranthes bidentata extract, chuanxiong extract, red peony root extract, cinnamon bark extract, peony extract, eucommia extract, wolfberry extract, Panax notoginseng extract, rhubarb extract, knotweed extract, saffron extract, angelica extract, radix spatholobi extract, agave extract, licorice extract, gentian extract, sophora flavescens extract, cnidium monnieri extract, artemisia annua extract, ginger extract, mint extract, turmeric extract, rhubarb extract, lily extract one or more of.

[0035] The fillers used in the fluidized bed granulation process of the present invention include, but are not limited to, one or more of dextrin and its derivatives, microcrystalline cellulose and its derivatives, lactose, corn starch and potato starch.

[0036] The binder used in the fluidized bed granulation process of the present invention includes, but is not limited to, one or more of pregelatinized starch, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, povidone, copovidone, ethyl cellulose and methyl cellulose.

[0037] Furthermore, the mass concentration of the adhesive slurry is 3.0-3.8%.

[0038] The present invention also provides a device for any of the above-mentioned fluidized bed granulation processes, comprising: an air inlet cabinet, an air inlet pipe, a fluidized bed, an exhaust pipe, an air inlet fan and a muffler connected in sequence; the end of the air inlet cabinet away from the air inlet pipe is an air inlet, and the air inlet cabinet is provided with a surface cooler and a heater; the air inlet pipe is provided with an air inlet valve and an air inlet anemometer; an air flow distribution plate, a material trough and a spray gun are built into the bottom of the fluidized bed, a near-infrared probe is installed in the side window, and a temperature probe for measuring the material temperature is installed in the middle.

[0039] Furthermore, the air inlet anemometer is installed at a distance of ≥1 meter from the air inlet valve.

[0040] In the present invention, the near-infrared probe is combined with a chemometric algorithm to establish an online quantitative model of particle size and moisture content, and then the key quality attributes in the granulation and drying process are quantitatively measured and monitored in real time, and the accuracy and effectiveness of the near-infrared model monitoring are analyzed and evaluated.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] (1) The present invention can preset the target particle size and moisture content according to actual production needs during the fluidized bed granulation process, and achieve this through a four-stage granulation process. In this process, the air volume and air temperature as well as the spraying slurry speed are mainly controlled, and the material temperature and the minimum material temperature can be preset. The spraying is controlled by these two temperatures, thereby controlling the granulation process, making the material in a good fluidized state, and realizing online adjustment of parameters such as particle size and moisture content, achieving batch-to-batch particle consistency and process reproducibility, thereby ensuring product quality.

[0043] (2) The present invention further improves the preparation efficiency by reasonably setting the particle size range of each stage in the four-stage granulation process and coordinating the inlet air volume and the inlet air temperature. The preparation of particles with target particle size and moisture content can be achieved in the shortest time. Moreover, by monitoring the inlet air volume and temperature, energy saving can be achieved, and the practical value is higher.

[0044] (3) The fluidized bed granulation process of the present invention is to introduce an air velocity meter, a temperature probe and a near-infrared probe into the existing fluidized bed granulation drying device, which is easy to transform, but can ensure the air volume control of the entire granulation process and realize online monitoring of particle size and moisture in the whole process. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 It is a schematic diagram of a fluidized bed granulation device;

[0046] Figure 2 The particle size distribution result of the intermediate product prepared in Example 1;

[0047] Figure 3 The particle size distribution result of the intermediate product prepared in Example 2;

[0048] Figure 4 The particle size distribution result of the intermediate product prepared in Example 3;

[0049] Figure 5 The particle size distribution result of the intermediate product prepared in Comparative Example 1;

[0050] Figure 6 The particle size distribution result of the intermediate product prepared in Comparative Example 2;

[0051] Description of reference numerals:

[0052] 1- Surface cooler; 2- heater; 3- air inlet cabinet; 4- air inlet valve; 5- air inlet pipe; 6- anemometer; 7- air flow distribution plate; 8- temperature probe; 9- near infrared probe; 10- material trough; 11- spray gun; 12- fluidized bed; 13- exhaust pipe; 14- air inlet fan; 15- muffler. DETAILED DESCRIPTION

[0053] The embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings and examples, but it will be appreciated by those skilled in the art that the following examples are only used to illustrate the present invention and should not be construed as limiting the scope of the present invention. If specific conditions are not specified in the examples, conventional conditions are used. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0054] The fluidized bed granulation device of the present invention is as follows Figure 1 As shown, it includes: an air inlet cabinet 3, an air inlet pipe 5, a fluidized bed 12, an exhaust pipe 13, an air inlet fan 14 and a muffler 15 connected in sequence; the end of the air inlet cabinet 3 away from the air inlet pipe 5 is an air inlet, and the air inlet cabinet 3 is provided with a surface cooler 1 and a heater 2; the air inlet pipe 5 is provided with an air inlet valve 4 and an air inlet anemometer 6; the bottom of the fluidized bed 12 is built-in with an air flow distribution plate 7, a material trough 10 and a spray gun 11, a near-infrared probe 9 is installed in the side window, and a temperature probe 8 for measuring the material temperature is installed in the middle.

[0055] In the present invention, the near-infrared probe 9 can be combined with a chemometric algorithm to establish an online quantitative model for the moisture content and particle size of the particles, and then to perform real-time quantitative measurement and monitoring of key quality attributes in the granulation and drying process, and to analyze and evaluate the accuracy and effectiveness of the near-infrared model monitoring.

[0056] The specific steps of the fluidized bed granulation process for online controlling of particle moisture and particle size of the present invention are as follows:

[0057] (1) Slurry preparation: Take an appropriate amount of purified water into a slurry preparation tank, add a binder under stirring, and fully dissolve it to obtain a binder slurry;

[0058] (2) Feeding: Place the formulated amount of plant extracts and fillers in the material trough of the fluidized bed, and let air in from the bottom of the fluidized bed so that the materials in the material trough are in a good fluidized state;

[0059] (3) Material heating: Set the air volume and air temperature to heat the material;

[0060] (4) Granulation: Granulation is performed through a four-stage granulation process, specifically: the target particle size range of the material for each stage of granulation, the material control temperature and the minimum material temperature during the granulation process are preset; the air volume and air temperature are set at the same time, and when the material temperature reaches the preset material control temperature range, spraying is started for granulation, and when the particle size of the material reaches the preset material target particle size range of the stage, the next stage of granulation is started until the four-stage granulation is completed;

[0061] (5) After the spraying is completed, the material is dried, granulated and sieved.

[0062] Those skilled in the art should understand that step (1) pulping and step (2) feeding are relatively independent steps and there is no order of precedence. Pulping can be performed first and then feeding, or feeding can be performed first and then pulping, or pulping can be performed while feeding.

[0063] Those skilled in the art should understand that step (2) feeding and step (3) material preheating are interconnected steps. In principle, step (2) feeding should be implemented first, and step (3) material preheating should be started after the feeding is completed. Of course, in the fluidized bed granulation process of the present invention, step (3) material preheating can also be implemented at the same time as step (2) feeding.

[0064] In some specific embodiments of the present invention, in step (2), the air volume is 2800-6500m 3 / h, including but not limited to 2800, 3000, 3200, 3500, 4000, 4500, 5000, 5500, 6000, 6500m 3 / h; preferably 3000, 3200, 3500, 4000, 4500, 5000m 3 / h; more preferably 3000, 3200, 3500m 3 / h.

[0065] In some specific embodiments of the present invention, step (2) also includes: setting the inlet air moisture content to ≤8%, the bag shaking time to 5-20s, and the bag shaking interval time to 20-60s, and the inlet air moisture content, bag shaking time and bag shaking interval time are continuously executed until the granulation is completed.

[0066] In some specific embodiments of the present invention, in step (3), the air volume is 3000-4500m 3 / h, including but not limited to 3000, 3200, 3500, 3750, 4000, 4250, 4500m 3 / h; preferably 3200, 3500, 3750, 4000, 4250m 3 / h; more preferably 3200, 3500, 4000m 3 / h; the inlet air temperature is 75-90℃, including but not limited to 75-80℃, 80-85℃, 85-90℃, 75-85℃, 80-90℃; preferably 80-85℃, 85-90℃, 80-90℃; further preferably 80-85℃.

[0067] In some specific embodiments of the present invention, during the granulation process of step (4), when the material temperature is lower than the minimum material temperature, spraying is stopped; when the material temperature reaches the material control temperature again, spraying is started until the particle size of the material reaches the set material particle size control range of the granulation at this stage, and then the next stage of granulation is started.

[0068] In some specific embodiments of the present invention, in step (4), the target particle size range of the material particles in the four-stage granulation is:

[0069] Stage 1: The proportion of materials passing through 80 mesh is less than 90% and the proportion of materials passing through 200 mesh is less than 85%;

[0070] The second stage: the proportion of materials passing through 80 mesh is less than 80% and the proportion of materials passing through 200 mesh is less than 45%;

[0071] The third stage: the proportion of materials passing through 80 mesh is less than 50% and the proportion of materials passing through 200 mesh is less than 30%;

[0072] Stage 4: The proportion of materials passing through 80 mesh is less than 35% and the proportion of materials passing through 200 mesh is ≤ 25%.

[0073] In some specific embodiments of the present invention, in step (4), the inlet air temperature is 80-90°C; the material control temperature is 45-55°C; and the minimum material temperature is 35-37°C.

[0074] In some specific embodiments of the present invention, step (4) further comprises setting the atomization pressure to 3.0-4.0 bar.

[0075] In some specific embodiments of the present invention, in the four-stage granulation process, the initial air volume of the spraying is 4000-5400m 3 / h and 150-250m / h per stage 3 / h increases in gradient, the initial slurry speed is 100-150rpm and decreases in gradient by 8-15rpm per stage. The purpose of setting the lowest air volume and the highest slurry speed in the first stage of granulation is that under this condition, the material in the material tank can be in a good fluidized state and the material is all at the bottom of the spray gun and will not be higher than the spray gun so that the slurry cannot contact the material, which ultimately leads to uneven granulation.

[0076] In some specific embodiments of the present invention, in step (5), the inlet air temperature is set to 80-85°C, and the inlet air volume is set to 4000-4800m 3 / h, so that the material is in a good fluidized state and heated to 45-55℃ for drying, and the drying is stopped after the moisture content of the material reaches 2.0-3.5%.

[0077] In some embodiments of the present invention, the granulation and screening in step (5) is to screen the dry granules through a 1.0-2.5 mm cone granulator.

[0078] The plant extracts applicable to the fluidized bed granulation process of the present invention include, but are not limited to, kudzu root extract, milk thistle extract, schisandra extract, calendula extract, scutellaria extract, salvia extract, sanguisorba officinalis extract, centella asiatica extract, honeysuckle extract, polygonum multiflorum extract, chamomile extract, rutin extract, eucommia extract, poria extract, forsythia extract, ginseng extract, codonopsis extract, aloe extract, sophora flavescens extract, ganoderma lucidum extract, evodia rutaecarpa extract, lotus seed extract, phellodendron extract, atractylodes macrocephala extract, American ginseng extract, Cistanche deserticola extract, safflower extract , saffron extract, purslane extract, fangfeng extract, qinjiao extract, notopterygium extract, angelica extract, angelica extract, wormwood extract, achyranthes bidentata extract, chuanxiong extract, red peony root extract, cinnamon bark extract, peony extract, eucommia extract, wolfberry extract, Panax notoginseng extract, rhubarb extract, knotweed extract, saffron extract, angelica extract, radix spatholobi extract, agave extract, licorice extract, gentian extract, sophora flavescens extract, cnidium monnieri extract, artemisia annua extract, ginger extract, mint extract, turmeric extract, rhubarb extract, lily extract one or more of.

[0079] The fillers used in the fluidized bed granulation process of the present invention include, but are not limited to, one or more of dextrin and its derivatives, microcrystalline cellulose and its derivatives, lactose, corn starch and potato starch.

[0080] The binder used in the fluidized bed granulation process of the present invention includes, but is not limited to, one or more of pregelatinized starch, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, povidone, copovidone, ethyl cellulose and methyl cellulose.

[0081] Furthermore, the mass concentration of the adhesive slurry is 3.0-3.8%.

[0082] The present invention also provides a device for any of the above-mentioned fluidized bed granulation processes, comprising: an air inlet cabinet, an air inlet pipe, a fluidized bed, an exhaust pipe, an air inlet fan and a muffler connected in sequence; the end of the air inlet cabinet away from the air inlet pipe is an air inlet, and the air inlet cabinet is provided with a surface cooler and a heater; the air inlet pipe is provided with an air inlet valve and an air inlet anemometer; an air flow distribution plate, a material trough and a spray gun are built into the bottom of the fluidized bed, a near-infrared probe is installed in the side window, and a temperature probe for measuring the material temperature is installed in the middle.

[0083] Furthermore, the air inlet anemometer is installed at a distance of ≥1 meter from the air inlet valve.

[0084] Furthermore, the near-infrared probe is combined with a chemometric algorithm to establish an online quantitative model for particle size and moisture content, and then to perform real-time quantitative measurement and monitoring of key quality attributes in the granulation and drying process, and to analyze and evaluate the accuracy and effectiveness of the near-infrared model monitoring.

[0085] Those skilled in the art should understand that other physical and chemical parameters of the target particles, such as bulk density, can also be controlled by adjusting the air volume and air temperature during the fluidized bed preparation process of the present invention. Therefore, without any creative work, it can also be achieved by the fluidized bed granulation process and device of the present invention.

[0086] Example 1

[0087] An extract product, the formula of which is: 43kg of kudzu root extract, 43kg of milk thistle extract, 43kg of schisandra chinensis extract, 35kg of dextrin, 40kg of microcrystalline cellulose and 1.3kg of povidone K30.

[0088] The fluidized bed granulation process of the extract product comprises the following steps:

[0089] (1) Slurry preparation: weigh an appropriate amount of purified water into a slurry preparation tank, start the slurry preparation and stirring, then slowly pour the corresponding povidone K30 into the slurry preparation tank, stirring while adding, and after the povidone K30 is fully dissolved, prepare a slurry with a concentration of 3.0%;

[0090] (2) Feeding: Place the formulated amount of Pueraria extract, Milk thistle extract, Schisandra chinensis extract, dextrin, and microcrystalline cellulose in the material tank of the fluidized bed, and set the air volume to 3000m 3 / h, so that the material is in a good fluidized state, the bag shaking time is 10s, the bag shaking interval is 30s, and the inlet air moisture content is ≤8.0% (the inlet air moisture content and bag shaking parameters are continuously implemented, covering the entire one-step granulation process);

[0091] (3) Material heating: Set the air volume to 3200m 3 / h, the inlet air temperature is 80℃, so that the material is in a good fluidized state and the material is heated to 50℃;

[0092] (4) Granulation: The target particle size range of the four-stage spraying is as follows: first stage: the proportion of materials passing through 80 mesh is less than 90% and the proportion of materials passing through 200 mesh is less than 85%; second stage: the proportion of materials passing through 80 mesh is less than 80% and the proportion of materials passing through 200 mesh is less than 45%; third stage: the proportion of materials passing through 80 mesh is less than 50% and the proportion of materials passing through 200 mesh is less than 30%; fourth stage: the proportion of materials passing through 80 mesh is less than 35% and the proportion of materials passing through 200 mesh is ≤25%; set the material control temperature to 50°C and the minimum material temperature to 36°C; and set the initial air volume to 5400m 3 / h, the inlet air temperature is 80°C, the atomization pressure is 3.0 bar, so that the material is in a good fluidized state. When the material temperature reaches the preset material control temperature range, start the spraying for granulation (the initial speed of the spraying liquid supply is 150rpm), spray the slurry prepared in step (1), and when the particle size of the material reaches the preset material target particle size range of this stage, start the next stage of granulation until the fourth stage of granulation is completed; in this process, when the material temperature is lower than 36°C, stop spraying; when the material temperature reaches 50°C again, start spraying until the particle size of the material reaches the set material particle size control range of this stage of granulation, then start the next stage of granulation, and after the fourth stage reaches the particle size, continue to spray all the slurry and end the spraying; the specific spraying parameter settings are as follows:

[0093] Phase 1: Set the air volume to 5400m 3 / h, the spraying liquid supply speed is 150rpm;

[0094] Stage 2: Set the air volume to 5600m 3 / h, the spraying liquid supply speed is 140rpm;

[0095] Stage 3: Set the air volume to 5800m 3 / h, the spraying liquid supply speed is 130rpm;

[0096] Stage 4: Set the air volume to 6000m 3 / h, the spraying liquid supply speed is 120rpm;

[0097] (5) Drying: After the spraying is completed, the material is dried and the air volume is set to 4500m 3 / h, the inlet air temperature is 80℃, so that the material is in a good fluidized state, and the material is heated to 45℃. When the moisture content of the material reaches 3.2%, the drying is stopped and the material is discharged;

[0098] (6) Granulation and sieving: The dry granules are sieved through a 2.5 mm conical granulator to obtain an intermediate product with uniform color and particle size.

[0099] Example 2

[0100] An extract product, the formula of which is: 43kg of kudzu root extract, 43kg of milk thistle extract, 43kg of schisandra chinensis extract, 35kg of dextrin, 40kg of microcrystalline cellulose and 1.3kg of povidone K30.

[0101] The fluidized bed granulation process of the extract product comprises the following steps:

[0102] (1) Slurry preparation: weigh an appropriate amount of purified water into a slurry preparation tank, start the slurry preparation and stirring, then slowly pour the corresponding povidone K30 into the slurry preparation tank, stirring while adding, and after the povidone K30 is fully dissolved, a slurry with a concentration of 3.8% is prepared;

[0103] (2) Feeding: Place the formulated amount of Pueraria extract, Milk thistle extract, Schisandra chinensis extract, dextrin, and microcrystalline cellulose in the material tank of the fluidized bed, and set the air volume to 3000m 3 / h, the inlet air temperature is 80℃, so that the material is in a good fluidized state, the bag shaking time is 15s, the bag shaking interval is 40s, and the inlet air moisture content is ≤8.0% (the inlet air moisture content and bag shaking parameters are continuously implemented, covering the entire one-step granulation process);

[0104] (3) Material heating: Set the air volume to 3200m 3 / h, the inlet air temperature is 85℃, so that the material is in a good fluidized state and the material is heated to 50℃;

[0105] (4) Granulation: The target particle size range of the four-stage spraying is as follows: first stage: the proportion of materials passing through 80 mesh is less than 90% and the proportion of materials passing through 200 mesh is less than 85%; second stage: the proportion of materials passing through 80 mesh is less than 80% and the proportion of materials passing through 200 mesh is less than 45%; third stage: the proportion of materials passing through 80 mesh is less than 50% and the proportion of materials passing through 200 mesh is less than 30%; fourth stage: the proportion of materials passing through 80 mesh is less than 35% and the proportion of materials passing through 200 mesh is ≤25%; set the material control temperature to 50°C and the minimum material temperature to 37°C; and set the initial air volume to 4750m 3 / h, the inlet air temperature is 90°C, the atomization pressure is 4.0 bar, so that the material is in a good fluidized state. When the material temperature reaches the preset material control temperature range, start the spraying for granulation (the initial speed of the spraying liquid supply is 120rpm), spray the slurry prepared in step (1), and when the particle size of the material reaches the preset material target particle size range of this stage, start the next stage of granulation until the fourth stage of granulation is completed; in this process, when the material temperature is lower than 37°C, stop spraying; when the material temperature reaches 50°C again, start spraying until the particle size of the material reaches the set material particle size control range of this stage of granulation, then start the next stage of granulation, and after the fourth stage reaches the particle size, continue to spray all the slurry and end the spraying; the specific spraying parameter settings are as follows:

[0106] Phase 1: Set the air volume to 4750m 3 / h, the spraying liquid supply speed is 120rpm;

[0107] Stage 2: Set the air volume to 4900m 3 / h, the spraying liquid supply speed is 110rpm;

[0108] Stage 3: Set the air volume to 5050m 3 / h, the spraying liquid supply speed is 100rpm;

[0109] Stage 4: Set the air volume to 5200m 3 / h, the spraying liquid supply speed is 90rpm;

[0110] (5) Drying: After the spraying is completed, the material is dried and the air volume is set to 4500m 3 / h, the inlet air temperature is 85℃, so that the material is in a good fluidized state, the material is heated to 45℃, and the drying is stopped when the moisture content of the material reaches 3.2%, and the material is discharged;

[0111] (6) Granulation and sieving: The dry granules are sieved through a 2.5 mm conical granulator to obtain an intermediate product with uniform color and particle size.

[0112] Example 3

[0113] An extract product, the formula of which is: 43kg of kudzu root extract, 43kg of milk thistle extract, 43kg of schisandra chinensis extract, 35kg of dextrin, 40kg of microcrystalline cellulose and 1.3kg of povidone K30.

[0114] The fluidized bed granulation process of the extract product comprises the following steps:

[0115] (1) Slurry preparation: Weigh an appropriate amount of purified water into a slurry preparation tank, start the slurry preparation and stirring, then slowly pour the corresponding povidone K30 into the slurry preparation tank, stirring while adding, and after the povidone K30 is fully dissolved, prepare a slurry with a concentration of 3.5%.

[0116] (2) Feeding: Place the formulated amount of Pueraria extract, Milk thistle extract, Schisandra chinensis extract, dextrin, and microcrystalline cellulose in the material tank of the fluidized bed, and set the air volume to 3000m 3 / h, so that the material is in a good fluidized state, the bag shaking time is 6s, the bag shaking interval is 20s, and the inlet air moisture content is ≤8.0% (the inlet air moisture content and bag shaking parameters are continuously implemented, covering the entire one-step granulation process).

[0117] (3) Material heating: Set the air volume to 3200m 3 / h, the inlet air temperature is 83℃, which puts the material in a good fluidized state and heats the material to 50℃.

[0118] (4) Granulation: The target particle size range of the four-stage spraying is as follows: the first stage: the proportion of materials passing through 80 mesh is less than 90% and the proportion of materials passing through 200 mesh is less than 85%; the second stage: the proportion of materials passing through 80 mesh is less than 80% and the proportion of materials passing through 200 mesh is less than 45%; the third stage: the proportion of materials passing through 80 mesh is less than 50% and the proportion of materials passing through 200 mesh is less than 30%; the fourth stage: the proportion of materials passing through 80 mesh is less than 35% and the proportion of materials passing through 200 mesh is ≤25%; the material control temperature is set to 50°C, the minimum material temperature is 35°C, and the initial air volume is set to 4000m 3 / h and at a gradient of 250m 3 / h is increased step by step, the inlet air temperature is 85°C, the atomization pressure is 3.5 bar, so that the material is in a good fluidized state. When the material temperature reaches the preset material control temperature range, the spraying is started for granulation (the initial speed of the spraying liquid supply is 100rpm and is reduced step by step by 8rpm), and the slurry prepared in step (1) is sprayed. When the particle size of the material reaches the preset material target particle size range of this stage, the next stage of granulation is started until the fourth stage of granulation is completed; during this process, when the material temperature is lower than 35°C, the spraying is stopped; when the material temperature reaches 50°C again, the spraying is started until the particle size of the material reaches the set material particle size control range of this stage of granulation, the next stage of granulation is started, and after the fourth stage reaches the particle size, the slurry is continued to be sprayed completely and the spraying is ended; the specific spraying parameter settings are as follows:

[0119] Stage 1: Set the air volume to 4000m 3 / h, the spraying liquid supply speed is 100rpm;

[0120] Stage 2: Set the air volume to 4250m3 / h, the spraying liquid supply speed is 92rpm;

[0121] Stage 3: Set the air volume to 4500m 3 / h, the spraying liquid supply speed is 84rpm;

[0122] Stage 4: Set the air volume to 4750m 3 / h, the spraying liquid supply speed is 76rpm;

[0123] (5) Drying: After the spraying is completed, the material is dried and the air volume is set to 3500m 3 / h, the inlet air temperature is 83℃, so that the material is in a good fluidized state, the material is heated to 45℃, and the drying is stopped when the moisture content of the material is 3.2%, and the material is discharged.

[0124] (6) Granulation and sieving: The dry granules were sieved through a 2.5 mm conical granulator to obtain an intermediate product with uniform color and particle size.

[0125] An extract product, the formula of which is: 43kg of kudzu root extract, 43kg of milk thistle extract, 43kg of schisandra chinensis extract, 35kg of dextrin, 40kg of microcrystalline cellulose and 1.3kg of povidone K30.

[0126] The fluidized bed granulation process of the extract product comprises the following steps:

[0127] (1) Slurry preparation: weigh an appropriate amount of purified water into a slurry preparation tank, start the slurry preparation and stirring, then slowly pour the corresponding povidone K30 into the slurry preparation tank, stirring while adding, and after the povidone K30 is fully dissolved, a slurry with a concentration of 3.5% is prepared;

[0128] (2) Feeding: Place the formulated amount of Pueraria extract, Milk thistle extract, Schisandra chinensis extract, dextrin, and microcrystalline cellulose in the material tank of the fluidized bed, and set the air volume to 3000m 3 / h, so that the material is in a good fluidized state, the bag shaking time is 10s, the bag shaking interval is 30s, and the inlet air moisture content is ≤8.0% (the inlet air moisture content and bag shaking parameters are continuously implemented, covering the entire one-step granulation process);

[0129] (3) Heating: air volume is 3200m 3 / h, set the air inlet temperature to 80℃, make the material in a good fluidized state, and heat the material to 50℃;

[0130] (4) One-step granulation: Set the air volume to 5400m 3 / h, the inlet air temperature is 85°C, the atomization pressure is 3.5 bar, so that the material is in a good fluidized state, the material temperature is controlled to 50°C, the minimum material temperature is 36°C, and the slurry prepared in step (1) is sprayed in, the spraying liquid supply speed is 150rpm, and the slurry is completely sprayed, and the spraying is completed;

[0131] (5) Drying: After the spraying is completed, the material is dried and the air volume is set to 4500m 3 / h, the inlet air temperature is 83℃, so that the material is in a good fluidized state, the material is heated to 45℃, and the drying is stopped when the moisture content of the material reaches 3.2%, and the material is discharged;

[0132] (6) Granulation and sieving: The dry granules are sieved through a 2.5 mm cone granulator to obtain an intermediate product with larger particle size and more coarse particles.

[0133] Comparative Example 2

[0134] An extract product, the formula of which is: 43kg of kudzu root extract, 43kg of milk thistle extract, 43kg of schisandra chinensis extract, 35kg of dextrin, 40kg of microcrystalline cellulose and 1.3kg of povidone K30.

[0135] The fluidized bed granulation process of the extract product comprises the following steps:

[0136] (1) Slurry preparation: weigh an appropriate amount of purified water into a slurry preparation tank, start the slurry preparation and stirring, then slowly pour the corresponding povidone K30 into the slurry preparation tank, stirring while adding, and after the povidone K30 is fully dissolved, prepare a slurry with a concentration of 3.5%;

[0137] (2) Feeding: Place the formulated amount of Pueraria extract, Milk thistle extract, Schisandra chinensis extract, dextrin, and microcrystalline cellulose in the material tank of the fluidized bed, and set the air volume to 3000m 3 / h, so that the material is in a good fluidized state, the bag shaking time is 10s, the bag shaking interval is 30s, and the inlet air moisture content is ≤8.0% (the inlet air moisture content and bag shaking parameters are continuously implemented, covering the entire one-step granulation process);

[0138] (3) Material heating: Set the air volume to 3200m 3 / h, the inlet air temperature is 80℃, so that the material is in a good fluidized state and the material is heated to 50℃;

[0139] (4) One-step granulation: Set the air volume to 4000m 3 / h, the inlet air temperature is 85°C, the atomization pressure is 3.5 bar, so that the material is in a good fluidized state, and the material control temperature is set to 50°C, the minimum material temperature is 36°C, and the slurry prepared in step (1) is sprayed in, the spraying liquid supply speed is 120rpm, and the spraying is completed after all the slurry is sprayed;

[0140] (5) Drying: After the spraying is completed, the material is dried and the air volume is set to 4500m 3 / h, the inlet air temperature is 83℃, so that the material is in a good fluidized state, the material is heated to 45℃, and the drying is stopped when the moisture content of the material reaches 3.2%, and the material is discharged;

[0141] (6) Granulation and sieving: The dry granules are sieved through a 2.5 mm conical granulator to obtain an intermediate product with a smaller particle size and a larger proportion of fine powder.

[0142] Test Case

[0143] The particle size of the products prepared in the above-mentioned Examples 1 to 3 and Comparative Examples 1 and 2 was tested by a laser particle size analyzer. The test process was as follows: Samples 001 to 014 were sampled in the one-step granulation process of step (4) at a time gradient of 2 min, wherein sample 001 was the sample before spraying, and sample 014 was the sample after spraying. The results are shown in FIG. Figure 2-Figure 6 .

[0144] As can be seen from the figure, through the fluidized bed granulation process of the present invention, a product with a uniform particle size consistent with the target particle size can be obtained, that is, an intermediate product in which 35-45% of the material passes through 60 mesh, 25-30% of the material passes through 80 mesh, 10-15% of the material passes through 200 mesh, and <10% of the material passes through 300 mesh.

[0145] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.

Claims

1. A fluidized bed granulation process for online control of particle size and moisture content, characterized in that: The following steps are involved: (1) Slurrying: Add the binder into water and fully dissolve it to obtain a binder slurry; (2) Feeding: placing the plant extract and filler in the material trough of the fluidized bed and introducing air to make the materials in a fluidized state; (3) Material heating: Set the air volume and air temperature to heat the material; (4) Granulation: Granulation is performed through a four-stage granulation process, specifically: the target particle size range of the material for each stage of granulation, the material control temperature and the minimum material temperature during the granulation process are preset; the air volume and air temperature are set at the same time, and when the material temperature reaches the preset material control temperature range, spraying is started for granulation, and when the particle size of the material reaches the preset material target particle size range of the stage, the next stage of granulation is started until the four-stage granulation is completed; (5) After granulation, the material is dried, granulated and sieved to obtain the product.

2. The fluidized bed granulation process according to claim 1, characterized in that: In step (2), the air volume is 2800-6500m 3 / h, preferably 3000-6500m 3 / h.

3. The fluidized bed granulation process according to claim 1, characterized in that: Step (2) also includes: setting the inlet air moisture content to ≤8%, the bag shaking time to 5-20s, and the bag shaking interval time to 20-60s; the inlet air moisture content, bag shaking time and bag shaking interval time are continuously executed until the granulation is completed.

4. The fluidized bed granulation process according to claim 1, characterized in that: In step (3), the air volume is 3000-4500m 3 / h, preferably 3200-4500m 3 / h; the inlet air temperature is 75-90℃, preferably 80-85℃.

5. The fluidized bed granulation process according to claim 1, characterized in that: In the four-stage granulation process of step (4), when the material temperature is lower than the minimum material temperature, the spraying is stopped; when the material temperature reaches the material control temperature again, the spraying is started until the particle size of the material reaches the target particle size range preset in this stage, and then the next stage of granulation is started.

6. The fluidized bed granulation process according to claim 1, characterized in that: In step (4), the target particle size range of the material particles in the four-stage granulation is: Stage 1: The proportion of materials passing through 80 mesh is less than 90% and the proportion of materials passing through 200 mesh is less than 85%; The second stage: the proportion of materials passing through 80 mesh is less than 80% and the proportion of materials passing through 200 mesh is less than 45%; The third stage: the proportion of materials passing through 80 mesh is less than 50% and the proportion of materials passing through 200 mesh is less than 30%; Stage 4: The proportion of materials passing through 80 mesh is less than 35% and the proportion of materials passing through 200 mesh is ≤ 25%.

7. The fluidized bed granulation process according to claim 1, characterized in that: In step (4), the air inlet temperature is 80-90°C; the material control temperature is 45-55°C; and the minimum material temperature is 35-37°C.

8. The fluidized bed granulation process according to claim 1, characterized in that: In step (4), in the four-stage granulation process, the initial air volume of the spraying is 4000-5400m 3 / h and 150-250m / h per stage 3 / h increases gradually, the initial slurry speed is 100-150rpm and decreases gradually by 8-15rpm in each stage; preferably, in the four-stage granulation process, the initial air volume of the spraying is 4500m 3 / h and 200m per stage 3 The initial rotation speed of the slurry was 150 rpm and then decreased by 10 rpm in each stage.

9. A device for the fluidized bed granulation process according to any one of claims 1 to 8, characterized in that: include: An air inlet cabinet (3), an air inlet pipe (5), a fluidized bed (12), an exhaust pipe (13), an air inlet fan (14) and a muffler (15) are connected in sequence; the end of the air inlet cabinet (3) away from the air inlet pipe (5) is an air inlet, and the air inlet cabinet (3) is provided with a surface cooler (1) and a heater (2); the air inlet pipe (5) is provided with an air inlet valve (4) and an air inlet anemometer (6); an air flow distribution plate (7), a material trough (10) and a spray gun (11) are built into the bottom of the fluidized bed (12), a near-infrared probe (9) is installed in the side window, and a temperature probe (8) for measuring the material temperature is installed in the middle.

10. The device according to claim 9, characterized in that The air inlet anemometer (6) is installed at a distance of ≥1 meter from the air inlet valve (4).

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