CN104548113B - A kind of production technology of film coating agent - Google Patents

A kind of production technology of film coating agent Download PDF

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Publication number
CN104548113B
CN104548113B CN201410763878.0A CN201410763878A CN104548113B CN 104548113 B CN104548113 B CN 104548113B CN 201410763878 A CN201410763878 A CN 201410763878A CN 104548113 B CN104548113 B CN 104548113B
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coating agent
production technology
rotating speed
plasticizer
filmogen
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CN104548113A (en
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赵永建
邵广川
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Tianjin Bokelin Medicine Packaging Technology Co Ltd
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Tianjin Bokelin Medicine Packaging Technology Co Ltd
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Abstract

The present invention relates to a kind of production technology of film coating agent, the production method is mainly crushed using high pressure draught to material.The problem of heavy metal and raw material particle size in film coating agent producing process be present in prior art.The method good crushing effect of the present invention, product cut size are thin and uniform;High velocity air can avoid material heated denaturalization;Coating agent finished product heavy metal analysis meets the control requirement of food, health products trade;Production efficiency is higher.

Description

A kind of production technology of film coating agent
Technical field:
The present invention relates to a kind of preparation method of medicament clothing sheet material, more particularly to a kind of production technology of film coating agent
Background technology:
Film coating is a kind of new art for coating, is that polymer solution or suspension are ejected into piece wicking surface to be formed A few micrometers of one layer of thick more stable plastic thin film layers, make up to certain Expected Results, this technical process is referred to as thin Film coating.When Swertia Tablet operates in seed-coating machine, the superfine small drop of Coating Solution or suspension is ejected into the outer of label Table, when these drops reach label, by contacting, hitting, sprawling, coalescing, dry, one layer of clothing is formed on the surface of label Film.
Film coating procedure can be divided into aqueous coatings technique and organic solvent art for coating according to the difference of solvent.Film Being coated purpose is mainly:Improve outward appearance and be easy to identify, cover bad smell, facilitate patients, mitigate gastrointestinal reaction, control Insoluble drug release, change drug release patterns, protection against the tide, lucifuge, completely cut off air to increase the stability of medicine.
Film coating process is critical that with excellent film coating agent.Film coating agent generally by high polymer material, Plasticizer, colouring agent etc. form, have strict compatibility in kind and quantity, with ensure medicine core surface energy formed one layer or Several layers of clothing film continuous, fine and close, lasting and with specific function.So superior in quality film coating agent should meet operation side Just, quick dissolving, be suspended uniformly, atomization is good, film forming is rapid, unilateral attractive in appearance, colour stable and moisture resistance height etc. require.
The existing frequently-used coating agent mode of production is generally divided into ball-milling method, comminuting method etc..Ball-milling method is relatively simple:In ball milling In tank operation process, porcelain ball or metal ball phase mutual friction are mixed and disperseed to material, and this mode by equipment rotating speed due to being limited System, ball operating linear velocity is not high, the limited strength of application, need to obtain the scattered of coloring agent particle by extending milling time, when Between be up to 3-5 hours, low production efficiency, and due to the scattered not up to thinner state of colouring agent, colour stable between product batches Property can not ensure.
Rule is crushed to hit material by weight or weight, mechanical force is enough to overcome the cohesiveness between colouring agent, Reach required fineness, but surface area increases after colouring agent refinement, surface free energy rise, because surface energy is made after cancellation external force With, still have the generation of reunion situation, cause product colour is uneven, in operation phenomena such as sedimentation, stifled rifle;Moreover, high-speed impact Part high polymer material molecular chain rupture or denaturation can be caused with overheat, influences the filming performance of product.
In my company (Tianjin Bokelin Medicine Packaging Technology Co., Ltd.) patent (Patent No. authorized in 2011 ZL200910069076.9 in), although overcoming some shortcomings in ball-milling method and comminuting method, many technological problemses are solved, But when coating agent is applied in food, health products coating, it is possible to cause indivedual batch heavy metals exceeding standards;This is due to divide at a high speed During dissipating, collision and friction are produced between material and equipment blade, bucket wall, very small amount metal ingredient is likely to result in and comes off, It is blended in material.Because amount is larger, compared with medicine, food, health products heavy metal require tightened up:For example curing In medicine product, heavy metal limit should be generally less than 10-20ppm, and the limitation of lead is no more than 0.5ppm in food and health products, arsenic Limitation be no more than 0.3ppm, control is strict, only has very small amount metal ingredient also to have exceeded risk even if in product.And And with the use of new material, when the larger filmogen of indivedual particle diameters is applied to coating agent, the slow-speed of revolution can not provide enough Energy is crushed, and because particle diameter is different between different material, is likely to result in and is mixed uneven situation, influence color and production Moral character energy.
In order to solve asking for prior art heavy metal present in film coating agent producing process and raw material particle size Topic, we have developed new coating agent producing process, its cardinal principle is that material is crushed using high pressure draught.
The content of the invention
The present invention provides a kind of film coating agent producing process, and the technique solves film coating present in prior art The problem of content of beary metal is more in agent and particle diameter is uneven.
The present invention is achieved by the following technical solutions:
A kind of production technology of film coating agent, the production method comprise the following steps:
Step 1, filmogen is put into the mixer for having blade, start mixer, blade rotating speed is controlled in 200- 1000r/min, plasticizer is slowly added into, operates 6-15min;
Step 2, colouring agent is added, the control of blade rotating speed is in 200-1000r/min, operating 10-20min;Obtain three kinds into The mixture divided;
Step 3, mixture are crushed with airslide disintegrating mill, and the Stress control of compressed air is in 0.7-1.0MPa, size controlling In 1-20 μ ms, produce.
Film coating agent in the above method, the composition of each component are as follows:
The parts by weight of filmogen 30~85;
The parts by weight of plasticizer 6~22;
The parts by weight of colouring agent 9~50.
Preferably, the composition of each component is as follows:
The parts by weight of filmogen 44~82;
The parts by weight of plasticizer 10~18;
The parts by weight of colouring agent 17~38.
Described film forming agent is in hydroxypropyl methyl cellulose, methylcellulose, hydroxypropyl cellulose, polyacrylic resin It is one or more of.
Described plasticizer is one or more of in glycerine, castor oil, triethyl citrate.
Described colouring agent is sunset yellow lake, erythrosine color lake, light blue color lake, iron oxide red, iron oxide yellow, titanium dioxide One of which is several.It is preferred that titanium dioxide, this area is referred to as titanium dioxide.
Above-mentioned raw materials are pharmaceutical grade marketable material.
The model high shear mixers such as SRL, SHR, GH can be selected in mixer of the present invention, and (such as thin close Krona in river is public Take charge of the mixer prepared);Airslide disintegrating mill (such as Jiangsu close friend group system of the models such as QYF, YQ, QW can be used in airslide disintegrating mill Standby airslide disintegrating mill).
Preferably, the production technology of film coating agent of the invention, comprises the following steps:
Step 1, filmogen is put into the mixer for having blade, mixer selects SRL, SHR or GH model high speed shear Mixer, starts mixer, and the control of blade rotating speed is slowly added into plasticizer in 500-800r/min, equipment operation 6-15min, Plasticizer is set to be fully infiltrated into filmogen;
Step 2, into mixer, input colouring agent is further mixed again, and blade rotating speed is controlled in 500-800r/min, if Received shipment turns 10-20min, is well mixed three;
Step 3, the material input air flow pulverizer mixed, airslide disintegrating mill use the air-flow powder of QYF, YQ or QW model Broken machine, the Stress control of compressed air is in 0.7-1.0MPa, and for material by after air-flow crushing in crushing chamber, its particle diameter is most of Concentrate in 5-10 μ ms, obtain that color is uniform and the satisfactory coating agent finished product of particle diameter.
Test example
The process conditions such as rotating speed of the present invention, mixing time, air pressure etc. are obtained by screening, and screening process is such as Under:
The rotating speed of test example 1 and the screening of time
The rotating speed of mixing paddle is set to 150r/min, 300r/min, 900r/min, 1100r/min by us, is added Enter the incorporation time after colouring agent and be also set to 5min, 11min, 19min, 23min, carry out the plasticising and mixing of material, effect is shown in Table 1 below
The rotating speed of table 1. and the screening of time
It can be seen that when the rotating speed of mixing paddle is relatively low, dispersion mixing is poor, and plasticizer is not completely dispersed into film forming Material internal, material still some be moist agglomerate, colouring agent also disperses uneven, and time lengthening does not reach effect yet; When the rotating speed of mixing paddle is increased to 200-1000r/min, contribute to material dispersion, powder color is substantially uniform;But after The long-time that renews effect changes unobvious;But when the rotating speed of blade is more than 1000r/min, powder at a high speed with pot wall collide by rotation Heating, material have ruckbildung.So it is determined that the process range effect of this patent selection is preferable.
The screening of the pressure of test example 2
The good material of above-mentioned preparation effect is crushed using airslide disintegrating mill, the pressure of compressed air is respectively 0.6MPa, 0.7MPa, 1.0MPa, 1.2MPa, crushing effect see the table below 2:
The screening of the pressure of table 2
0.6MPa 0.7MPa 1.0MPa 1.2MPa
Finished product grain size 10—30μm 1—20μm 1—20μm 1—20μm
Due to crushing the pressure relied primarily in air-flow, the low crushing effect to material of air pressure is bad so that finished product grain size It is larger, it is unsatisfactory for the requirement of our processing;And more than air pressure 1.0MPa finished product grain sizes and be not apparent from diminishing, more preferable effect is not played Fruit, so Stress control is more suitable in 0.7-1.0MPa.
The gas flow crushing process of test example 3 and common process performance comparison
Common process:Method disclosed in ZL200910069076.9
Present invention process gas flow crushing process:Embodiment 1
Table 3 is gas flow crushing process and common process performance comparison
The advantages of the present invention
1st, plasticization effect is good.Liquid plasticizer can not be uniformly distributed using being added by the way of drenching in powder, can be in office Portion forms the agglomerate of humidity, and other parts are still dry powder.Powder is set to produce motion, liquid using low velocity shear hybrid mode When plasticizer sprays, reach preliminary with the powder of motion and mix, then penetrated into by the frictional impact of blade inside filmogen, Form good plasticization effect.The slow-speed of revolution of blade will not also cause materials from spattering simultaneously.
2nd, product quality is more guaranteed.Colouring agent can shape using the mixing compared with the slow-speed of revolution in mixer with filmogen Into preferable mixed effect, do not use high rotating speed to disperse, material can be avoided to introduce metal to blade and the power friction of pot wall miscellaneous The situation of matter.And the further scattered and refinement in color lake uses air-flow crushing mode, because material is in high velocity air condition Mutually collide down and crush, equipment surface will not be impacted, also free from admixture enters.After testing, the coating agent produced into Product lead content is less than 0.5ppm, and the content of arsenic is less than 0.3ppm, and the heavy metal analysis of product meets the control of food, health products trade System requires.
3rd, product cut size is thin and uniform.Airslide disintegrating mill is coated the principle that agent is processed:Compressed air is through crushing Multiple nozzles of intracavitary inject disintegrating area after being accelerated into supersonic airstream, material is suspended in fluidized state and seethe with excitement and mutually collide Hit, accelerated particle mutually clashes crushing in each nozzle joint, is fully opened the coloring agent particle of reunion, into membrane material Bulky grain in material, which can also crush, to attenuate.Material after crushing is raised air-flow and is delivered to graded region, reaches the thin of granularity requirements Powder is collected, and not up to the coarse powder of granularity requirements returns to disintegrating area and continues to crush.The method good crushing effect, particle diameter distribution are equal Even, coating agent fineness can reach 1-20 μm, and the particle of wherein 5-10 μm particle diameter reaches more than 85%, illustrate to obtain using air-flow crushing The material obtained has good fineness and the size distribution concentrated, the product cut size obtained better than original high shear process, and Solves the problems, such as the heavy metal in product.Finished product grain size is uniform so that coating agent is in coating in use, solution dissolves rapid, face Color is uniform, unilateral bright and clean after coating, no piebald and color dot.
4th, material heated denaturalization is avoided.Carried out using the mode of production in crushing process, high velocity air can take away material and hit Caused heat is hit, so temperature of charge can be maintained at less than 30 DEG C all the time in production, there will not be the phenomenon of hot-spot, it is right The situation that will not be melted or be denatured in the relatively low materiel machining of some fusing points.
5th, production efficiency is higher.Continuous work can be realized when being crushed using the mode of production, it is high without frequently charging discharging Pressure gas stream can reach fast-crushing to material, and its speed of production than other production technologies faster, saves the production time.
Under
Embodiment
The present invention is further illustrated by the following examples, but not as limitation of the present invention.
Embodiment 1
1st, 850g hydroxypropyl methyl celluloses are added in mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min Clock, slowly plus 60g enters glycerine, and equipment is run 6 minutes, reaches the plasticising to material.
2nd, 90g titanium dioxide is put into mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min, to cladding Colouring agent afterwards carries out the mixing of 10 minutes, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 0.7MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.
Embodiment 2
1st, 610g methylcellulose is added in mixer, the blade rotating speed for controlling mixing apparatus is 600 revs/min, is delayed Slow to add 160 castor oil, equipment is run 10.5 minutes, reaches the plasticising to material.
2nd, put into 190g titanium dioxide into mixer and 40g sunset yellow lakes, the blade rotating speed for controlling mixing apparatus are 600 revs/min, the mixing of 15 minutes is carried out to the colouring agent after cladding, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 0.85MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.
Embodiment 3
1st, 300g hydroxypropyl celluloses being added in mixer, the blade rotating speed for controlling mixing apparatus is 1000 revs/min, 200 triethyl citrates are slowly added into, equipment is run 15 minutes, reaches the plasticising to material.
2nd, put into 150g titanium dioxide into mixer and 350g medicinal iron oxides, the blade rotating speed for controlling mixing apparatus are 1000 revs/min, the mixing of 20 minutes is carried out to the colouring agent after cladding, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 1.0MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.
Embodiment 4
1st, 300g hydroxypropyl methyl celluloses are added in mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min Clock, slowly plus 60g enters glycerine, and equipment is run 6 minutes, reaches the plasticising to material.
2nd, 90g titanium dioxide is put into mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min, to cladding Colouring agent afterwards carries out the mixing of 10 minutes, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 0.7MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.
Embodiment 5
1st, 850g hydroxypropyl methyl celluloses are added in mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min Clock, slowly plus 220g enters glycerine, and equipment is run 6 minutes, reaches the plasticising to material.
2nd, 500g titanium dioxide is put into mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min, to bag Colouring agent after covering carries out the mixing of 10 minutes, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 0.7MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.
Embodiment 6
1st, 440g hydroxypropyl methyl celluloses are added in mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min Clock, slowly plus 100g enters glycerine, and equipment is run 6 minutes, reaches the plasticising to material.
2nd, 170g titanium dioxide is put into mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min, to bag Colouring agent after covering carries out the mixing of 10 minutes, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 0.7MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.
Embodiment 7
1st, 820g hydroxypropyl methyl celluloses are added in mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min Clock, slowly plus 180g enters glycerine, and equipment is run 6 minutes, reaches the plasticising to material.
2nd, 380g titanium dioxide is put into mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min, to bag Colouring agent after covering carries out the mixing of 10 minutes, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 0.7MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.
Embodiment 8
1st, 600g hydroxypropyl methyl celluloses are added in mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min Clock, slowly plus 140g enters glycerine, and equipment is run 6 minutes, reaches the plasticising to material.
2nd, 280g titanium dioxide is put into mixer, the blade rotating speed for controlling mixing apparatus is 200 revs/min, to bag Colouring agent after covering carries out the mixing of 10 minutes, forms mixture.
3rd, the material input air flow pulverizer mixed, compressed air pressure 0.7MPa, material is in crushing chamber by air-flow After crushing, discharging obtains that color is uniform and the satisfactory coating agent finished product of particle diameter.

Claims (5)

1. a kind of production technology of film coating agent, comprises the following steps:
(1) take in filmogen input mixing apparatus and stir, rotating speed is in 500-800r/min, addition plasticizer operating 6-15min;
(2) colouring agent is added into mixing apparatus again, continues to stir, rotating speed in 500-800r/min, equipment operation 10-20min, Obtain mixed material;
(3) mixed material is put into and crushed into airslide disintegrating mill, wherein pressure is 0.7-1.0MPa, and the particle diameter after crushing is 1-20μm;
Described plasticizer is selected from:It is one or more of in glycerine, castor oil, triethyl citrate;
The colouring agent is selected from:In sunset yellow lake, erythrosine color lake, light blue color lake, iron oxide red, iron oxide yellow, titanium dioxide One or more;
Described mixer is with paddle mixer.
2. production technology as claimed in claim 1, it is characterised in that the filmogen described in step (1) is selected from:Hydroxypropyl Methylcellulose, methylcellulose, hydroxypropyl cellulose, the one of which of polyacrylic resin.
3. production technology as claimed in claim 1, it is characterised in that the particle diameter described in step (3) is 5-10 μm.
4. the production technology as described in claim any one of 1-3, it is characterised in that described filmogen:Plasticizer:Coloring Agent weight ratio is 30~85:6~22:9~50.
5. production technology as claimed in claim 4, it is characterised in that described filmogen:Plasticizer:Colourant weights ratio For 44~82:10~18:17~38.
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