CN110090156B - Preparation process and device of vitamin AD microbeads - Google Patents
Preparation process and device of vitamin AD microbeads Download PDFInfo
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Abstract
The invention discloses a preparation process of vitamin AD microbeads, which comprises the steps of conveying vitamin A, vitamin D and vitamin AD microbead matrixes to a vacuum emulsifying machine for emulsification, and then conveying materials to a granulator for granulation, wherein a dripper outlet in the granulator is arranged below the liquid level of cooling liquid, and dripping pills and cooling solidification are completed in one step; then the dropping pill is conveyed to a pill washing and deoiling machine and rinsed by cold water and the refrigerated organic solvent; then feeding the material into a fluidized dryer to enable the material to form a fluidized state, starting a high-speed shearing machine, and drying the material through three stages of low-temperature drying, medium-temperature drying and high-temperature drying in sequence to achieve the effect of drying and scattering agglomerated vitamin AD microbeads; in the whole preparation flow, each process step is designed in a refined mode, the preparation efficiency is high in production, the drying effect is good, and the vitamin AD microbeads with high uniformity can be prepared efficiently. The invention also discloses a device special for the process, which has delicate structure and high utilization rate.
Description
Technical Field
The invention belongs to the field of pharmacy, and particularly relates to a preparation process and a device of vitamin AD microbeads.
Background
The vitamin A and vitamin D microbeads (AD microbeads) are solid medicinal micropellet beads containing vitamin A and vitamin D with diameter of 3mm, preferably 0.6 mm to 1.2 mm, and are prepared from one or more of gelatin, agar, pectin, carrageenan, gum arabic, curdlan, sucrose, fructose, and vegetable oil as main matrix. The AD micro-beads are mainly used for supplementing vitamins A and D of a human body, are necessary substances for growth and development of the human body, and particularly have important effects on fetal development, epithelial tissue stereotyped property, vision, reproductive function, bone growth, blood calcium regulation and the like.
Two main ways for supplementing human vitamin AD which are commonly adopted at home and abroad are mainly provided, wherein one way is to eat food rich in vitamin A and vitamin D; the other is taking granules or capsules containing vitamin AD; for taking vitamin AD granules, the common preparation method of the medicine is to prepare vitamin AD into micro-pellet beads, and can mix and supplement AD micro-beads and other types of vitamin micro-beads; in the preparation process, how to ensure that the preparation process cannot damage the vitamin AD microbeads is a problem to be considered; most importantly, how to ensure high production efficiency of the AD microbeads and uniformity of effective components of the AD microbeads are the problems which need to be solved urgently.
At present, in specific industrial production, firstly dripping is generally adopted in a dripping pill making process, and then solidification forming is carried out by utilizing solidification liquid; when the oil is removed from the pills, the pills are directly washed in a washing and hot air drying mode; in the drying step, a conveyor belt heater is usually used for drying, so that the agglomeration phenomenon is easy to occur; therefore, the preparation of the vitamin AD microbeads has more problems:
1) the pill forming process efficiency of the AD microbeads is low;
2) the deoiling process of the AD microspheres is incomplete; the AD micro-beads have agglomeration phenomenon in the deoiling process;
3) and the drying process of the AD micro-beads has low drying efficiency and frequent agglomeration.
The application of products containing vitamin AD microbeads is always restricted by the problems, and the phenomenon of short supply and demand appears in the market; therefore, it is urgent to solve the above-mentioned problems and to broaden the market of vitamin AD microbead products.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides the preparation process and the device for preparing the vitamin AD microbeads, which have the advantages of good drying effect and high preparation efficiency.
In order to achieve the above object, the present invention provides a process for preparing vitamin AD microbeads, comprising the steps of:
a preparation process of vitamin AD microbeads is characterized by comprising the following steps:
s1 weighing materials and vacuum emulsification: emulsifying the vitamin A, the vitamin D and the vitamin AD microsphere matrix after weighing to obtain an emulsified material;
s2 dropping and pelletizing: conveying the emulsified material obtained in the step S1 to a granulator, and dripping a plurality of discharging drippers arranged below the liquid level of the cooling liquid in the granulator to prepare pills to obtain the vitamin AD microbeads;
deoiling S3 pellets: conveying the vitamin AD microbeads prepared by the S2 to a pill washing and deoiling machine for deoiling and cleaning;
drying S4 pellets: and conveying the vitamin AD microbeads subjected to deoiling cleaning in the S3 to a fluidized drying machine for drying.
In step S1, the vitamin AD microbead substrate is one or a mixture of gelatin, agar, pectin, carrageenan, gum acacia, curdlan, sucrose, fructose, and vegetable oil, the solvent is purified water, and the emulsification temperature is 10-95 ℃.
In step S2, the method includes: and (3) defoaming the emulsified material obtained in the step S1 through standing and negative pressure, and then conveying the material into a granulator to drip vitamin AD microbeads through a plurality of discharging drippers below the liquid level of the cooling liquid at the temperature of 4-30 ℃.
In step S3, the method includes: and (4) conveying the vitamin AD microbeads obtained in the step S2 to a pill washing and deoiling machine for cleaning and deoiling, starting a stirring paddle, and firstly rinsing with cold water and then cleaning with an organic solvent.
Wherein the organic solvent comprises one of gasoline, alcohol and isopropanol, and the cleaning and deoiling conditions are as follows:
temperature of cold water: 2-30 ℃; rinsing flow rate: 20-2000L/MIN; rinsing time: 2-60 min;
temperature of the organic solvent: 2-30 ℃; organic solvent cleaning time: 10-600S; organic solvent cleaning times: 1-10 times;
rotating speed of a stirring paddle: 20-1000 RPM; the positive and negative rotation switching period of the stirring paddle: 2 to 20S.
In step S4, the method includes: and (4) conveying the vitamin AD microbeads obtained in the step S3 to a fluidized dryer for drying, starting an induced draft fan to introduce air flow to the bottom of the fluidized dryer so that the vitamin AD microbeads are blown up to form a fluidized state, and then starting a high-speed shearing machine.
Wherein, the drying step conditions are as follows:
1) and (3) low-temperature stage: the air inlet temperature is 5-25 ℃; air inlet volume of 200-2000M3H; lasting for 0.5-3 h, and shearing at the rotating speed of 100-2000 RPM;
2) a medium temperature stage: the air inlet temperature is 25-40 ℃; air inlet volume of 200-2000M3H; lasting for 0.5-4 h, and shearing at the rotating speed of 1000-3000 RPM;
3) and (3) high-temperature stage: the air inlet temperature is 40-100 ℃; air inlet volume of 200-2000M3H; lasting for 0.5-3 h.
The invention also provides a device for preparing the vitamin AD microspheres by adopting the process, which comprises a vacuum emulsifying machine, a granulator, a pill washing and deoiling machine and a fluidized drying machine;
a vacuum emulsifying machine: for emulsifying the material; and is conveyed to a granulator through a material conveying pump and a material conveying pipe;
a granulator: comprises a discharge dripper and a vertical runner pipe; a discharge dripper is arranged in the vertical flow channel pipe; the number of the discharging drippers is multiple, and the outlets of the discharging drippers are positioned below the liquid level of the cooling liquid; the vitamin AD micro-beads dripped by the discharge drippers are conveyed to a pill washing and deoiling machine;
a pill washing and deoiling machine: cleaning the vitamin AD micro-beads dripped by the discharge dripper; conveying the cleaned vitamin AD microbeads into a fluidized dryer;
fluidized drying machine: and the vitamin AD micro-beads are used for drying the washed vitamin AD micro-beads by the pill washing and deoiling machine.
The vacuum emulsifying machine comprises a material tank, and the material tank is also provided with an interlayer which divides the material tank into an emulsifying cavity and a heat preservation cavity; the emulsification chamber is used for emulsifying the material, but the heat preservation chamber holding liquid for control emulsification chamber temperature.
The grain discharging drippers are accommodated in the vertical flow channel pipes, and a plurality of grain dripping needle pipes are arranged in each grain discharging dripper; the vertical flow channel pipe is internally provided with cooling liquid, and the discharging dripper is positioned below the liquid level of the cooling liquid.
The pill washing and deoiling machine comprises a cleaning pot, a cleaning agent switching part and a stirring paddle arranged in the cleaning pot, wherein the cleaning agent switching part comprises a cold water channel, an organic solvent channel and a switching valve, and the cold water channel and the organic solvent channel are communicated with the cleaning pot; the switching valve is used for switching the cold water channel and the organic solvent channel.
The fluidized drying machine comprises a material pot, a fluidizing cylinder, a blower and a high-speed shearing machine; the two ends of the material pot are opened, one end of the material pot is connected with the blower, and the other end of the material pot is connected with the fluidizing barrel; the inner wall of the fluidization cylinder is coated with an anti-sticking wall material; the high-speed shearing machine is accommodated in the material pot.
The invention has the advantages that: compared with the prior art, the preparation process and the device of the vitamin AD micro-beads can emulsify materials through a vacuum emulsifying machine, then convey the materials into a granulator, and improve the discharging efficiency by adopting a mode that a discharging dripper is directly positioned below the liquid level of a cooling liquid; then conveying the prepared microbeads into a pill washing and deoiling machine, and washing by adopting a cold water washing mode and then by adopting an organic solute washing mode; and (3) putting the cleaned vitamin AD microbeads into a fluidized dryer for drying, wherein the whole drying process is divided into an early low-temperature stage, a middle heating stage and a later high-temperature stage to finish the preparation. Through the special process of each step and the matched device, the method has the following advantages:
(1) the process for preparing the AD micro-beads by dripping pills is different from the common dripping pill mode: the solidified liquid is singly pelletized and then cooled; the invention adopts a plurality of discharging drippers to continuously discharge under the cooling liquid level, and dripping pills and cooling are simultaneously carried out, thereby improving the dripping pill efficiency;
(2) the deoiling process of the AD microspheres adopts the steps of rough washing with cold water and then washing with the refrigerated organic solvent, and stirring and scattering large blocks of the AD microspheres by using a paddle during washing, so that the deoiling of the AD microspheres is more thorough; the refrigerated cleaning agent can prevent the AD microspheres from being melted due to overhigh temperature in the general deoiling process;
(3) the drying process of the AD microbeads adopts a fluidized dryer for drying, and special materials are coated on the inner wall of the fluidized cylinder, so that the AD microbeads are effectively prevented from being adhered to the wall; the shearing equipment is added in the material pot, so that the phenomenon of agglomeration in the drying process is prevented, and the drying effect is effectively improved by adopting the process of firstly carrying out low temperature and then gradually heating;
(4) the preparation of the AD micro-beads has the advantages that the production efficiency is improved, the drying efficiency of the AD micro-beads is ensured, and the vitamin AD micro-beads can be obtained through the process with the characteristics.
Drawings
FIG. 1 is a first flowchart of the present invention;
FIG. 2 is a second flowchart of the present invention;
FIG. 3 is a third flowchart of the present invention;
FIG. 4 is a fourth flow chart of the present invention;
FIG. 5 is a fifth flow chart of the present invention;
FIG. 6 is a schematic view of a vacuum emulsification machine and granulator according to the present invention;
FIG. 7 is a schematic view of the granulation section of the present invention;
FIG. 8 is a schematic structural view of a pill-washing and oil-removing machine of the present invention;
fig. 9 is a schematic structural view of the fluidized dryer of the present invention.
The main element symbols are as follows:
1. vacuum emulsifying machine 2 and granulator
21. Discharge dripper 22 and vertical flow channel pipe
23. Dripping pill collecting assembly 24, bubble filter basket
3. Pellet-washing and deoiling machine 33 and explosion-proof exhaust assembly
31. Cleaning pot 311 and cleaning agent switching part
3111. Cold water channel 3112 and organic solvent channel
32. Wash ball collection subassembly 4, fluidized drying machine
41. Drier 411, material pot
412. Fluidizing drum 42 and blower
43. A high speed shearer 44, a dry pill collection assembly.
Detailed Description
In order to more clearly describe the present invention, the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1-2, the present invention provides a process for preparing vitamin AD microbeads, which comprises the following steps:
s1 weighing materials and vacuum emulsification: weighing vitamin A, vitamin D and vitamin AD microsphere matrixes, and then putting the weighed vitamin A, vitamin D and vitamin AD microsphere matrixes into a vacuum emulsifying machine for emulsification;
s2 dropping and pelletizing: conveying the emulsified material obtained in the step S1 to a granulator, and dripping the emulsified material into pills through a plurality of drippers arranged below the liquid level of the cooling liquid;
deoiling S3 pellets: conveying the vitamin AD microbeads prepared by the S2 to a pill washing and deoiling machine for deoiling and cleaning;
drying S4 pellets: and conveying the vitamin AD microbeads subjected to deoiling cleaning in the S3 to a fluidized drying machine for drying.
Specifically, referring to fig. 1, in step S1, the vitamin AD microbead matrix is selected from one or more of gelatin, agar, pectin, carrageenan, gum acacia, curdlan, sucrose, fructose, vegetable oil, etc.; purified water is selected as a solvent; putting the weighed materials and pure water into a material tank according to a certain proportion, wherein the material concentration is preferably 10-80% in the embodiment; emulsifying at 10-95 deg.c, preferably 50 deg.c; and then starting a motor at the top of the material tank to drive an emulsifying head to emulsify the material, controlling the emulsifying rotating speed to be between 100 and 3000RPM, and reducing the air pressure in the tank to be between-5 and-90 KPa through a vacuum pump. The purpose of this treatment is: the components of each layer of the material are uniformly mixed by a vacuum emulsification process, in particular to uniformly mix vitamin A, vitamin D and other auxiliary materials.
Specifically, referring to fig. 1-2, in step S2, the emulsified material obtained in step S1 is defoamed for 10-60 min, and is conveyed to a splitter by a material conveying pump and a pipeline, and is split into a plurality of material channels, and the material channels are respectively conveyed to a plurality of discharging drippers; wherein, a plurality of discharging drippers are provided, and the outlet of the discharging dripper is positioned below the liquid level of the cooling liquid; naturally forming round pills by surface tension and directly solidifying in cooling liquid; the temperature of the optional cooling liquid is 4-30 ℃, and preferably 6 ℃. The mode of continuously discharging the outlet of the discharging dripper below the liquid level of the cooling liquid is different from the mode that common drippers are dripped one by one and then the cooling liquid is solidified into pills; the method of the invention directly combines the dripping pill and the cooling solidification in one step, and the material naturally forms the pill and solidifies in the vertical cooling liquid flow passage tube by surface tension, thereby shortening the preparation time in time, improving the space utilization rate in space and improving the pill forming efficiency. In the prior art, the common method for preparing the microbeads is to firstly drip and then put into cooling liquid to be solidified into pills, namely, the pills are naturally formed by means of gravity, but under the condition of forming the pills by means of gravity, materials are condensed into pills with larger diameters at a dripping head part and then drip, so that the pills with the diameters within 3mm cannot be obtained, and the preparation requirements (the diameters of 0.6-2.2 mm) of the invention cannot be met.
Specifically, referring to fig. 3, please refer to step S3, the vitamin AD microbeads obtained in step S2 are transported to a pill washing and deoiling machine, and are washed with cold water and then with an organic solvent; simultaneously starting a stirring paddle; the organic solvent adopts one of gasoline, alcohol and isopropanol, wherein alcohol is preferably used as the cleaning organic solvent, and the specific cleaning and deoiling conditions are as follows:
temperature of cold water: 2-30 ℃; rinsing flow rate: 20-2000L/MIN; rinsing time: 2-60 min;
temperature of the organic solvent: 2-30 ℃; organic solvent cleaning time: 10-600S; organic solvent cleaning times: 1-10 times;
rotating speed of a stirring paddle: 20-1000 RPM; the positive and negative rotation switching period of the stirring paddle: 2 to 20S. The process has the advantages that: the vitamin AD micro-beads are rinsed by cold water, most of the cooling oil adhered to the surfaces of the vitamin AD micro-beads in the step S2 is removed, most of the pills can be broken up, then the pills are cleaned by the refrigerated organic solvent, the cooling oil can be basically removed, the rest of the small pills can be broken up, and part of moisture of the vitamin AD micro-beads can be taken away.
Specifically, referring to fig. 4, in step S4, the vitamin AD microbeads obtained in step S3 are transported to a fluidized dryer, and an induced draft fan is started to introduce air flow to the bottom of the fluidized dryer, so that the vitamin AD microbeads are blown up to form a fluidized state; after 10-15 minutes, starting a high-speed shearing machine, and performing a drying step, wherein the specific conditions of the drying step are as follows:
1) and (3) low-temperature stage: the air inlet temperature is 5-25 ℃; air inlet volume of 200-2000M3H; lasting for 0.5-3 h, and shearing at the rotating speed of 100-2000 RPM;
2) a medium temperature stage: the air inlet temperature is 25-40 ℃; air inlet volume of 200-2000M3H; lasting for 0.5-4 h, and shearing at the rotating speed of 1000-3000 RPM;
3) and (3) high-temperature stage: the air inlet temperature is 40-100 ℃; air inlet volume of 200-2000M3H; and (5) continuing for 0.5-3 h, and stopping the shearing rotating speed. The three temperature stages are carried out in sequence, the moisture of the material can be reduced in the low temperature stage, the hardness of the material pills can be gradually improved, the air flow is gradually improved after the certain hardness is achieved, namely, the material pills enter the medium temperature stage to promote the moisture of the material to be further reduced, and then the material pills enter the high temperature stage to ensure the drying degree of the materialThe drying standard is met; meanwhile, the high-speed shearing machine is opened in the drying process, the agglomerated materials are scattered, and the drying effect and the drying speed of the materials are guaranteed.
The invention also provides a device suitable for the process, which comprises a vacuum emulsifying machine 1, a granulator 2, a pill washing and deoiling machine 3 and a fluidized dryer 4;
vacuum emulsifying machine 1: for emulsifying the material; and is conveyed to a granulator 2 through a material conveying pump and a material conveying pipe;
and (3) granulating machine 2: comprises a discharge dripper 21, a vertical flow passage pipe 22 and a dripping pill collecting component 23; a discharge dripper 21 is arranged in the vertical flow channel pipe 22; a plurality of discharging drippers 21 are arranged, and the outlets of the discharging drippers 21 are positioned below the liquid level of the cooling liquid;
and (3) a pill washing and deoiling machine 3: comprises a cleaning pot 31 and a pill-cleaning collecting component 32; the cleaning pot 31 is provided with a cleaning agent switching part 311, a stirring paddle 312 and a water filtering port 313, wherein the cleaning agent switching part 311 comprises a cold water channel 3111, an organic solvent channel 3112 and a switching valve 3113; the dropping pills produced by the granulator are conveyed into a cleaning pot 31, a cleaning solvent is selected through a cold water channel 3111 and an organic solvent channel 3112, and the cleaned dropping pills are conveyed into a pill cleaning collection assembly 32;
fluidized drying machine 4: comprises a drier body 41, a blower 42, a high-speed shearing machine 43 and a dried pill collecting component 44; the dryer 41 includes a material pan 411 and a fluidizing drum 412; the material pot 411 is open at two ends, one end is connected with the blower 42, and the other end is connected with the fluidization cylinder 412; the inner wall of the fluidization cylinder 412 is coated with an anti-sticking wall material; the high-speed shearing machine 43 is accommodated in the material pot 411;
referring to fig. 6, the material is emulsified and conveyed to a granulator for granulation through a vacuum emulsifying machine, and then the granules are conveyed to a pill washing and deoiling machine for cleaning, and then conveyed to a fluidized drying machine for drying.
The vacuum emulsifying machine 1 further comprises a material tank 11, the material tank 11 is further provided with an interlayer, the interlayer of the material tank divides the material tank into a material cavity and a heat preservation cavity, and the heat preservation cavity stores water or oil with a certain temperature and is used for adjusting the temperature of the material.
Please refer to fig. 6-7; the length of the vertical flow channel pipe 22 is preferably 0.5-1.5 m; the granule discharging drippers 21 are accommodated in the vertical flow channel pipe 22, the inner diameter of each granule discharging dripper is preferably 0.2-3 mm, each dripper can accommodate a plurality of needle tubes, 1-8 needle tubes are preferably accommodated, and the arrangement is that on the premise that the diameter of the dripping pills is within 3mm, the space is utilized as much as possible to improve the production efficiency; the granulator has still included coolant liquid reflux unit, and has installed bubble filter basket 24 additional in the coolant liquid reflux unit, eliminates the influence of the bubble that the coolant liquid flows the production to vitamin AD microballon.
Wherein, the organic solvent and the large blade are adopted for rinsing; please refer to fig. 8; therefore, the pill washing and deoiling machine is also additionally provided with an explosion-proof air exhaust assembly 33; the cleaning efficiency is ensured, and meanwhile, the production safety is emphasized. Wherein, the stirring paddle is a big blade paddle, and the big blade paddle can rotate forwards and backwards, and can break up the agglomerated pills.
Please refer to fig. 9; the two ends of the material pot 411 are open, the smaller end of the opening is connected with the air blower 42, the larger end of the opening is connected with the fluidization cylinder 412, and the side wall of the material pot 411 and the horizontal plane form an inclination angle of 45-65 degrees; under the long-term debugging of the inventor, the inventor finds that when the inclined angle of the pot wall of the fluidized material pot 411 is designed to be 45-65 degrees, the vitamin AD microbeads can be effectively prevented from being adhered to the inner wall of the material pot in the early stage of drying.
The following examples illustrate the preparation process of vitamin AD microbeads and the beneficial effects of the preparation process of the invention:
example 1
After the materials are weighed, putting the materials and purified water into a material tank of a vacuum emulsifying machine according to the proportion of 4:6, emulsifying the materials at 50 ℃, starting a motor at the top of the material tank to drive an emulsifying head to emulsify the materials, and reducing the air pressure in the tank to-30 KPa through a vacuum pump to obtain the materials in an emulsified state, wherein the emulsifying speed is 1500 RPM;
standing the emulsified material, and defoaming under negative pressure for 40 min; then the mixture is conveyed into a flow divider of a granulator through a material conveying pump and a pipeline, the flow divider is divided into a plurality of material channels and respectively conveyed into 6 discharging drippers, each discharging dripper is provided with 6 dripping needle tubes, and the total 36 needle tubes simultaneously operate, so that the dripping flow can reach 215 g/min; the temperature of the cooling liquid is adjusted to 8 ℃; dripping into a cooling oil flow passage to form pills, then flowing into a collecting filter basket, separating the dripping pills from the cooling oil by the filter basket, refluxing the cooling liquid into a bubble filter basket in a liquid storage tank, and collecting the dripping pills in the filter basket to obtain the AD pills to be washed. Particularly, the outlet of the discharging dripper is positioned below the liquid level of the cooling liquid for continuous discharging, and the material naturally forms round pills and is solidified into pills in the vertical cooling liquid flow passage pipe by surface tension, which is different from the common way that drippers are dripped one by one and then the cooling liquid is solidified into pills; in this example, the inventors counted the diameters of the vitamin AD microbeads that were prepared by dripping, and found that the yield was 92% and that the defective materials were mostly ultrafine particles.
Then putting the AD pellets to be washed into a pellet washing filter basket of a pellet washing and deoiling machine; and (3) allowing 18 ℃ cold water to enter the cleaning pot from the cold water channel through the switching valve, wherein the rinsing flow of the cold water is 120L/MIN, simultaneously starting the stirring paddle to stir in a mode of repeatedly switching forward rotation and reverse rotation, wherein the forward rotation period and the reverse rotation period are 10 seconds, stopping stirring after 18MIN cold water rinsing, adjusting a valve pipeline system, discharging the cold water in the cleaning pot from the bottom, and finishing the cold water rinsing process after water is discharged. After the cold water rinsing is finished, the valve is switched to allow the organic solvent to enter the cleaning pot, the valve is closed after the organic solvent at 18 ℃ completely submerges the pills in the cleaning basket, so that the organic solvent is kept in the cleaning pot, and the stirrer is started again, wherein the stirring mode is the same as that of water washing. After 160s, the requirement of the cleaning and deoiling process is met, the valve is opened to discharge the organic solvent from the bottom, and the organic solvent cleaning process is completed after the organic solvent is discharged. The organic solvent can be reused for cleaning and deoiling according to the process requirements, and the cleaning can be carried out for multiple times. The inventor researches specific temperatures of cold water and an organic solvent, and finds that the AD micro-beads are easy to freeze if the cold water with the temperature lower than 2 ℃ is used for rinsing the AD micro-beads, and if the temperature is higher than 30 ℃, some AD micro-beads with smaller diameters are melted in a cleaning process, so that the preparation requirements cannot be met.
After the washing is finished, filling the vitamin AD micro-beads to be dried into a fluidized drying material pot, and sealingClosing the material pot, starting an induced draft fan to introduce air flow to the bottom of the material pot to force the material to be blown up to form a fluidized state, and gradually taking away residual organic solvent and moisture in the material by the air flow; the hardness of the material pellets can be improved along with the reduction of the moisture of the material, after the material pellets reach a certain hardness, the temperature of the air flow is gradually increased and the high-speed shearing machine is started after 2 hours in the specific production process, so that the moisture of the material is further reduced, the initial air temperature is 18 ℃, and the air volume is 300M3H, the duration is 2 hours, and the shearing rotating speed is 600 RPM; then the drying is carried out in the middle stage, the air temperature is adjusted to 40 ℃, and the air quantity is adjusted to 400M3H, duration 0.5 hours, high shear adjusted to 2800 RPM; finally, the later drying stage is carried out, the high-speed shearing machine is firstly closed, the air temperature is synchronously adjusted to 50 ℃, and the air quantity is adjusted to 300M3H, for 1 hour.
Example 2
After the materials are weighed, putting the materials and purified water into a material tank of a vacuum emulsifying machine according to the proportion of 4:6, emulsifying the materials at 82 ℃, starting a motor at the top of the material tank to drive an emulsifying head to emulsify the materials, wherein the emulsifying speed is 2200RPM, and simultaneously reducing the air pressure in the tank to-30 KPa through a vacuum pump to obtain the materials in an emulsified state;
and standing the emulsified material, and defoaming under negative pressure for 55 min. Then the mixture is conveyed into a flow divider of a granulator through a material conveying pump and a pipeline, the flow divider is divided into a plurality of material channels and respectively conveyed into 6 discharging drippers, each discharging dripper is provided with 6 dripping needle tubes, and the total 36 needle tubes simultaneously operate, so that the dripping flow can reach 215 g/min; the temperature of the cooling liquid is adjusted to 10 ℃; the material is dripped into the cooling oil flow channel through the needle tube to form pills and then flows into the collecting and filtering basket, the filtering basket separates the pill pills from the cooling oil, the cooling oil flows back to the bubble filtering basket in the liquid storage tank, and the pill pills are collected in the filtering basket to obtain the AD pills to be washed. In this example, the inventor makes statistics on the diameter of the vitamin AD microbeads subjected to dripping, and the statistical finding shows that the qualified rate is 82%, and the unqualified materials are mostly ultrafine particles and materials with bubble pits on the surface.
Then putting the AD pellets to be washed into a pellet washing filter basket of a pellet washing and deoiling machine; and (3) allowing 16 ℃ cold water to enter the cleaning pot from the cold water channel through the switching valve, wherein the rinsing flow of the cold water is 180L/MIN, simultaneously starting the stirring paddle to stir in a mode of repeatedly switching forward rotation and reverse rotation, wherein the period of the forward rotation and the reverse rotation is 8 seconds, stopping stirring after 20MIN cold water rinsing, adjusting a valve pipeline system, discharging the cold water in the cleaning pot from the bottom, and finishing the cold water rinsing process after water is discharged. After the cold water rinsing is finished, the valve is switched to allow the organic solvent to enter the cleaning pot, the valve is closed after the organic solvent with the temperature of 16 ℃ completely submerges the pills in the cleaning basket, so that the organic solvent is kept in the cleaning pot, and the stirrer is started again, wherein the stirring mode is the same as that of water washing. After 200s, the requirement of the cleaning and deoiling process is met, the valve is opened to discharge the organic solvent from the bottom, and the organic solvent cleaning process is completed after the organic solvent is discharged. The step of cleaning and deoiling by using an organic solvent can be repeated according to the process requirements, and the cleaning is carried out for multiple times;
after cleaning, filling vitamin AD microbeads to be dried into a fluidized drying material pot, sealing the material pot, starting an induced draft fan to introduce air flow to the bottom of the material pot, so that the material is blown up to form a fluidized state, and the residual organic solvent and moisture in the material are gradually taken away by the air flow; along with the reduction of the moisture of the material, the hardness of the material pellets can be improved, after the material pellets reach a certain hardness, the temperature of the air flow is gradually increased and the high-speed shearing machine is started after 2 hours in the specific production process, so that the moisture of the material is further reduced, the initial air temperature is 15 ℃, and the air volume is 330M3H, the duration is 2 hours, and the shearing rotating speed is 600 RPM; then entering a middle-stage drying interval, performing high-speed shearing for 0.5 hour at 2500RPM, adjusting the air temperature to 25 ℃ and the air volume to 420M3H, for 0.5 hours; finally, the later drying stage is carried out, the high-speed shearing machine is firstly closed, the air temperature is synchronously adjusted to 65 ℃, and the air quantity is adjusted to 300M3H, for 1 hour.
Example 3
After the materials are weighed, putting the materials and purified water into a material tank of a vacuum emulsifying machine according to the proportion of 4:6, emulsifying the materials at 50 ℃, starting a motor at the top of the material tank to drive an emulsifying head to emulsify the materials, wherein the emulsifying speed is 2200RPM, and simultaneously reducing the air pressure in the tank to-80 KPa through a vacuum pump to obtain the materials in an emulsified state;
and standing the emulsified material, and defoaming under negative pressure for 55 min. Then the mixture is conveyed into a flow divider of a granulator through a material conveying pump and a pipeline, the flow divider is divided into a plurality of material channels and respectively conveyed into 6 discharging drippers, each discharging dripper is provided with 6 dripping needle tubes, and the total 36 needle tubes simultaneously operate, so that the dripping flow can reach 215 g/min; the temperature of the cooling liquid is adjusted to 8 ℃; the material is dripped into the cooling oil flow channel through the needle tube to form pills and then flows into the collecting and filtering basket, the filtering basket separates the pill pills from the cooling oil, the cooling oil flows back to the bubble filtering basket in the liquid storage tank, and the pill pills are collected in the filtering basket to obtain the AD pills to be washed. In this embodiment, the inventor makes statistics on the diameter of the vitamin AD microbeads subjected to dripping, and finds that the qualified rate is 86% and that the unqualified materials are mostly ultrafine particles and materials with bubbles on the surface.
Then putting the AD pellets to be washed into a pellet washing filter basket of a pellet washing and deoiling machine; and (3) allowing 18 ℃ cold water to enter the cleaning pot from the cold water channel through the switching valve, wherein the rinsing flow of the cold water is 180L/MIN, simultaneously starting the stirring paddle to stir in a mode of repeatedly switching forward rotation and reverse rotation, wherein the period of the forward rotation and the reverse rotation is 10 seconds, stopping stirring after 40MIN cold water rinsing, adjusting a valve pipeline system, discharging the cold water in the cleaning pot from the bottom, and finishing the cold water rinsing process after water is discharged. And after the cold water rinsing is finished, switching the valve to allow the organic solvent to enter the cleaning pot, closing the valve after the 25 ℃ organic solvent completely submerges the pills in the cleaning basket, keeping the organic solvent in the cleaning pot, and starting the stirrer again in the same stirring mode as the water washing. After 200s, the requirement of the cleaning and deoiling process is met, the valve is opened to discharge the organic solvent from the bottom, and the organic solvent cleaning process is completed after the organic solvent is discharged. The step of cleaning and deoiling by using an organic solvent can be repeated according to the process requirements, and the cleaning is carried out for multiple times;
after cleaning, filling vitamin AD microbeads to be dried into a fluidized drying material pot, sealing the material pot, starting a draught fan to introduce air flow to the bottom of the material pot to force the material to be blown up to form a fluidized state, wherein the vitamin AD microbeads are in the materialThe residual organic solvent and moisture are gradually carried away by the air flow; along with the reduction of the moisture of the material, the hardness of the material pellets can be improved, after the material pellets reach a certain hardness, the temperature of the air flow is gradually increased and the high-speed shearing machine is started after 2 hours in the specific production process, so that the moisture of the material is further reduced, the initial air temperature is 15 ℃, and the air volume is 330M3H, the duration is 2 hours, and the shearing rotating speed is 600 RPM; then entering a middle-stage drying interval, performing high-speed shearing for 0.5 hour at 2500RPM, adjusting the air temperature to 40 ℃ and the air volume to 420M3H, for 0.5 hours; finally, the later drying stage is carried out, the high-speed shearing machine is firstly closed, the air temperature is synchronously adjusted to 80 ℃, and the air quantity is adjusted to 300M3H, for 1 hour.
Example 4
After the materials are weighed, putting the materials and purified water into a material tank of a vacuum emulsifying machine according to the proportion of 4:6, emulsifying the materials at 82 ℃, starting a motor at the top of the material tank to drive an emulsifying head to emulsify the materials, wherein the emulsifying speed is 2200RPM, and simultaneously reducing the air pressure in the tank to-80 KPa through a vacuum pump to obtain the materials in an emulsified state;
and standing the emulsified material for vacuum defoaming for 12 min. Then the mixture is conveyed into a flow divider of a granulator through a material conveying pump and a pipeline, the flow divider is divided into a plurality of material channels and respectively conveyed into 6 discharging drippers, each discharging dripper is provided with 6 dripping needle tubes, and the total 36 needle tubes simultaneously operate, so that the dripping flow can reach 215 g/min; the temperature of the cooling liquid is adjusted to 10 ℃; the material is dripped into the cooling oil flow channel through the needle tube to form pills and then flows into the collecting and filtering basket, the filtering basket separates the pill pills from the cooling oil, the cooling oil flows back to the bubble filtering basket in the liquid storage tank, and the pill pills are collected in the filtering basket to obtain the AD pills to be washed. In this embodiment, the inventor makes statistics on the diameter of the vitamin AD microbeads subjected to dripping, and finds that the qualified rate is 90% to 92%, and most of the unqualified materials are ultrafine particles and materials with bubbles on the surface.
Then putting the AD pellets to be washed into a pellet washing filter basket of a pellet washing and deoiling machine; and (3) allowing 18 ℃ cold water to enter the cleaning pot from the cold water channel through the switching valve, wherein the rinsing flow of the cold water is 120L/MIN, simultaneously starting the stirring paddle to stir in a mode of repeatedly switching forward rotation and reverse rotation, wherein the period of the forward rotation and the reverse rotation is 8 seconds, stopping stirring after 40MIN cold water rinsing, adjusting a valve pipeline system, discharging the cold water in the cleaning pot from the bottom, and finishing the cold water rinsing process after water is discharged. And after the cold water rinsing is finished, switching the valve to allow the organic solvent to enter the cleaning pot, closing the valve after the 25 ℃ organic solvent completely submerges the pills in the cleaning basket, keeping the organic solvent in the cleaning pot, and starting the stirrer again in the same stirring mode as the water washing. After the requirement of the cleaning and deoiling process is met after 220 seconds, the valve is opened to discharge the organic solvent from the bottom, and the organic solvent cleaning process is finished after the organic solvent is discharged. The step of cleaning and deoiling by using an organic solvent can be repeated according to the process requirements, and the cleaning is carried out for multiple times;
after cleaning, filling vitamin AD microbeads to be dried into a fluidized drying material pot, sealing the material pot, starting an induced draft fan to introduce air flow to the bottom of the material pot, so that the material is blown up to form a fluidized state, and the residual organic solvent and moisture in the material are gradually taken away by the air flow; the hardness of the material pellets can be improved along with the reduction of the moisture of the material, after the material pellets reach a certain hardness, the temperature of the air flow is gradually increased and the high-speed shearing machine is started after 2 hours in the specific production process, so that the moisture of the material is further reduced, the initial air temperature is 18 ℃, and the air volume is 300M3H, the duration is 2 hours, and the shearing rotating speed is 600 RPM; then entering a middle-stage drying interval, performing high-speed shearing for 0.5 hour at 2500RPM, adjusting the air temperature to 30 ℃ and the air volume to 420M3H, for 0.5 hours; finally, the later drying stage is carried out, the high-speed shearing machine is firstly closed, the air temperature is synchronously adjusted to 65 ℃, and the air quantity is adjusted to 300M3H, for 1 hour.
The following table is a process flow chart of the above examples 1 to 4:
TABLE 1 Process flow sheet
In addition to the above-listed examples, the inventors have made many attempts in exploring the process, for example, adjusting only the temperature of cold water in the washing and deoiling process to 35 ℃ on the process conditions of example 1, and found that too high temperature causes the vitamin AD microbeads to melt; only adjusting the fluidized drying process is tried, the drying is always carried out by using wind with the temperature of 18 ℃ and the wind rate of 300M3/H, and the drying effect of the embodiment 1 needs 38 hours; of course, the inventor obviously does not make more than these attempts in the process of developing the technology, and only selects a few representative examples to illustrate; before the process provided by the invention is developed, the prior art always adopts direct dripping, then simple washing and hot air drying are carried out, and finally the microbeads are put on dry cloth with a certain vibration frequency for wiping, so that the invention is pioneering in all aspects of preparation efficiency, preparation qualification rate and the like.
Then, the inventor judges the qualification rate of the whole preparation process through a drying weight loss experiment in the preparation production process. Loss on drying: weighing dried vitamin AD microbeads, putting the vitamin AD microbeads into an experimental environment at 110 ℃, and weighing after 4 hours, wherein the difference between the front weight and the rear weight is the weight percentage of water evaporation within 4 hours; and the drying weight loss can not exceed 7.0 percent, and the drying reaches the standard.
Data statistics of the qualified rate and the loss on drying of the dropping pills for the above 4 examples are as follows:
TABLE 2 example qualification rate and loss on drying of dropping pills
In summary, in the above embodiments 1 to 4, the preparation process of the present invention can meet the requirement of the vitamin AD microbeads on the particle size (0.6 to 2.2mm), and the qualified rate of the particle size can be maintained at 82 to 92%, the dropping method in the prior art usually has a particle size of 3 to 5mm, which cannot meet the requirement of the vitamin AD microbeads prepared by the present invention on high uniformity mixing, and the effect is not as good as the vitamin AD microbeads prepared by the present invention; meanwhile, the inventor verifies through a drying weight loss experiment after fluidized drying, and finds that the percentage of drying weight loss is between 4.90% and 6.70%, and the percentage of drying weight loss does not exceed 7.0%, so that a good drying effect is achieved.
The invention has the advantages that:
(1) the dropping pill forming process of the AD micro-beads adopts a plurality of discharging drippers to continuously discharge materials under the cooling liquid level, and is different from a common dropping pill mode: the solidified liquid is singly pelletized and then cooled; the dripping pill and the cooling are carried out simultaneously, and the dripping pill efficiency is improved;
(2) the deoiling process of the AD microspheres adopts the steps of rough washing with cold water and then washing with the refrigerated organic solvent, and stirring and scattering large blocks of the AD microspheres by using a paddle during washing, so that the deoiling of the AD microspheres is more thorough; the refrigerated cleaning agent can prevent the AD microspheres from being melted due to overhigh temperature in the general deoiling process;
(3) the drying process of the AD microbeads adopts a fluidized dryer for drying, and special materials are coated on the inner wall of the fluidized cylinder, so that the AD microbeads are effectively prevented from being adhered to the wall; the shearing equipment is added in the material pot, so that the phenomenon of agglomeration in the drying process is prevented, and the drying effect is effectively improved by adopting the process of firstly heating at low temperature and then heating gradually.
The above disclosure is only for a few specific embodiments of the present invention, but the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (7)
1. A preparation process of vitamin AD microbeads is characterized by comprising the following steps:
s1 weighing materials and vacuum emulsification: emulsifying the vitamin A, the vitamin D and the vitamin AD microsphere matrix after weighing to obtain an emulsified material;
s2 dropping and pelletizing: the emulsified material obtained in the step S1 is subjected to standing and negative pressure defoaming, and then conveyed into a granulator to be dripped into vitamin AD microbeads through a plurality of discharging drippers below the liquid level of the cooling liquid at the temperature of 4-30 ℃;
deoiling S3 pellets: conveying the vitamin AD microbeads prepared by the S2 to a pill washing and deoiling machine for deoiling and cleaning; the conditions are as follows: temperature of cold water: 18 ℃; rinsing flow rate: 120L/MIN; rinsing time: 18 min;
temperature of the organic solvent: 18 ℃; organic solvent cleaning time: 10S; organic solvent cleaning times: 1-10 times; rotating speed of a stirring paddle: 20-1000 RPM; the positive and negative rotation switching period of the stirring paddle: 2-20S;
drying S4 pellets: conveying the vitamin AD microbeads obtained in the step S3 to a fluidized dryer for drying, starting an induced draft fan to introduce air flow to the bottom of the fluidized dryer so that the vitamin AD microbeads are blown up to form a fluidized state, and then starting a high-speed shearing machine;
the conditions of the drying step are as follows:
1) and (3) low-temperature stage: the air inlet temperature is 18 ℃; air inlet quantity 300M3H; lasting for 2h, and the shearing rotating speed is 600 RPM;
2) a medium temperature stage: the air inlet temperature is 40 ℃; air inlet quantity 400M3H; the duration is 0.5h, and the shearing rotating speed is 2800 RPM;
3) and (3) high-temperature stage: the air inlet temperature is 50 ℃; air inlet quantity 300M3H; lasting for 1 h.
2. The process for preparing vitamin AD microbeads according to claim 1, wherein in step S1, said vitamin AD microbead matrix is one or more of gelatin, agar, pectin, carrageenan, gum acacia, curdlan, sucrose, fructose, and vegetable oil; the solvent is purified water, and the emulsifying temperature is 10-95 ℃.
3. An apparatus for adopting the preparation process of any one of claims 1-2, which comprises a vacuum emulsifying machine, a granulator, a pill washing and deoiling machine and a fluidized drying machine;
a vacuum emulsifying machine: for emulsifying the material; and is conveyed to a granulator through a material conveying pump and a material conveying pipe;
a granulator: comprises a discharge dripper and a vertical runner pipe; a discharge dripper is arranged in the vertical flow channel pipe; the number of the discharging drippers is multiple, and the outlets of the discharging drippers are positioned below the liquid level of the cooling liquid; the vitamin AD micro-beads dripped by the discharge drippers are conveyed to a pill washing and deoiling machine;
a pill washing and deoiling machine: cleaning the vitamin AD micro-beads dripped by the discharge dripper; conveying the cleaned vitamin AD microbeads into a fluidized dryer;
fluidized drying machine: and the vitamin AD micro-beads are used for drying the washed vitamin AD micro-beads by the pill washing and deoiling machine.
4. The vitamin AD microbead preparation apparatus according to claim 3, wherein the vacuum emulsifying machine comprises a material tank, the material tank is further provided with an interlayer, and the interlayer divides the material tank into an emulsifying cavity and a heat preservation cavity; the emulsification chamber is used for emulsifying the material, but the heat preservation chamber holding liquid for control emulsification chamber temperature.
5. The vitamin AD microbead preparation apparatus according to claim 3, wherein the discharge drippers are accommodated in the vertical flow passage pipes, and a plurality of dripping needle pipes are arranged in each discharge dripper; the vertical flow channel pipe is internally provided with cooling liquid, and the discharging dripper is positioned below the liquid level of the cooling liquid.
6. The vitamin AD microbead preparation device as claimed in claim 3, wherein the pill-washing and deoiling machine comprises a cleaning pot, a cleaning agent switching part and a stirring paddle arranged in the cleaning pot, the cleaning agent switching part comprises a cold water channel, an organic solvent channel and a switching valve, and the cold water channel and the organic solvent channel are communicated with the cleaning pot; the switching valve is used for switching the cold water channel and the organic solvent channel.
7. The vitamin AD microbead preparation apparatus according to claim 3, wherein the fluidized dryer comprises a material pot, a fluidizing cylinder, a blower and a high-speed shearing machine; the two ends of the material pot are opened, one end of the material pot is connected with the blower, and the other end of the material pot is connected with the fluidizing barrel; the inner wall of the fluidization cylinder is coated with an anti-sticking wall material; the high-speed shearing machine is accommodated in the material pot.
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| CN202096469U (en) * | 2011-03-11 | 2012-01-04 | 天津天士力制药股份有限公司 | Pill deoiling and drying machine |
| CN204147278U (en) * | 2014-07-11 | 2015-02-11 | 天士力制药集团股份有限公司 | Air cooling dripping pill production line |
| CN109044839A (en) * | 2018-10-10 | 2018-12-21 | 南京正宽医药科技有限公司 | Medicinal pill dripping machine in one kind |
| CN208405391U (en) * | 2018-03-05 | 2019-01-22 | 江西天之海药业股份有限公司 | A kind of vitaminAD capsule and pill pill dripping machine of accurate measurement feed |
| CN109432070A (en) * | 2018-11-09 | 2019-03-08 | 深圳万和制药有限公司 | The preparation method and vitaminAD pellet of high uniformity vitaminAD pellet |
| CN109692126A (en) * | 2019-03-01 | 2019-04-30 | 深圳万和制药有限公司 | The equipment for preparing the method for high evenness dripping pill and using |
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2019
- 2019-06-19 CN CN201910532276.7A patent/CN110090156B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202096469U (en) * | 2011-03-11 | 2012-01-04 | 天津天士力制药股份有限公司 | Pill deoiling and drying machine |
| CN204147278U (en) * | 2014-07-11 | 2015-02-11 | 天士力制药集团股份有限公司 | Air cooling dripping pill production line |
| CN208405391U (en) * | 2018-03-05 | 2019-01-22 | 江西天之海药业股份有限公司 | A kind of vitaminAD capsule and pill pill dripping machine of accurate measurement feed |
| CN109044839A (en) * | 2018-10-10 | 2018-12-21 | 南京正宽医药科技有限公司 | Medicinal pill dripping machine in one kind |
| CN109432070A (en) * | 2018-11-09 | 2019-03-08 | 深圳万和制药有限公司 | The preparation method and vitaminAD pellet of high uniformity vitaminAD pellet |
| CN109692126A (en) * | 2019-03-01 | 2019-04-30 | 深圳万和制药有限公司 | The equipment for preparing the method for high evenness dripping pill and using |
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