CN109535496A - A kind of preparation method of degradable water penetration coating membrane - Google Patents
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a kind of preparation methods of degradable water penetration coating membrane, belong to granule coating fields.The preparation method of chitosan film of the invention includes the following steps: for chitosan (relative molecular mass 110000), glycerol and 2% acetic acid solution to be uniformly mixed according to the ratio of 1g, 4g, 90mL, centrifugation is debubblized, chitosan film liquid is obtained, chitosan film liquid obtains chitosan film in 50 DEG C of drying.Chitosan film of the invention can be used as granule coating for food, medicine field, by the way that granule to be dipped into chitosan film liquid, or chitosan film liquid is sprayed at granule surface can be coated to granule.Chitosan film water penetration of the invention is high, it is coated granule, substantially improves the appearance of granule, weakens the stimulation to the sense of taste；Its high temperature resistant and stability is strong, can be brewed repeatedly.
Description
Technical field
The present invention relates to granule coating fields, and in particular to a kind of preparation method of degradable water penetration coating membrane.
Background technique
Chitosan is by the deacetylated gained of chitin, and in living nature, chitosan is unique a large amount of existing natural alkalinity
Polysaccharide is widely present in shell, rudimentary plant and the cell of algae, the shell of shellfish and the cartilage, higher plant of shrimp crab insect
Cell wall in, possess good biological degradability.Chitosan has been applied to medicine, food, cosmetics, water process at present
Etc., as chitosan is using more and more extensive, people also pay attention to chitosan further.
Chitosan has excellent film forming, and strong will is refined to be waited with the chitosan of different relative molecular weights and different deacetylations
Prepare chitosan film, the results showed that, the pure water flux of chitosan film is reduced with the increase of molecular weight of chitosan, and water is cut
Rate is stayed to increase with the increase of deacetylation.Wu Guojie etc. has studied the optimised process of chitosan film forming, with 3.5 × 10-5mol/L
Chitosan solution, 0.52mol/L acetic acid, 0.40mol/L ethyl alcohol, the chitosan film tension of 0.25mol/L sodium hydroxide preparation are strong
Degree is 749.235N/m.Wu You is excellent using natural macromolecular material chitosan as raw material, is prepared for chitosan film using the tape casting,
Research shows that crosslinking and acetylation can increase the tensile strength of chitosan film, to improve the performance of film.Wang Yafen etc. is to film
Performance such as elongation, moisture-vapor transmission, gas permeation rate, tensile strength, folding line etc. analyzed, with chitosan be at
Film is configured to chitosan solution as solvent using the acetic acid aqueous solution that volume ratio is 1%, and stearic acid is added at film liquid, uses
Chitosan edible packing membrane made of casting method can be used for the packaging of varieties of food items.
The coating material of granule has versatility, is broadly divided into water-soluble material, enteric as common coating material
Property material, insoluble material it is these three types of, current widely used coating material has hydroxypropyl methyl cellulose (HPMC), poly-
Ethylene glycol (PEG), cellulose acetate phthalate (CAP), polyethylene acetal diethylamine acetate (AEA), ethyl cellulose
(EC) not yet it is widely used on coating material with crylic acid resin, chitosan.The factor for influencing film-coated technique is main
There are Preparation Technology of Granules and film-forming process.It is Preparation Technology of Granules by the smoothness of enwrapped granule agent, hardness, aridity
Influence factor, the factor for influencing film-forming process are more.Granule is coated using film coating procedure, can achieve cover
Peculiar smell, the purpose for improving stability.
Prepare water penetration Chitosan Coating, it would be desirable to be able to the preferable and not soluble in water material of high temperature resistant, water penetration；That chooses is molten
Agent, it is necessary to have higher chemical stability and thermal stability, but also should have lower toxicity and edibility, have source
Broadness, lower-price characteristic.Various solvents have certain advantage and disadvantage, and acetic acid is volatile, and sodium hydroxide has corrosivity, give
Experimental implementation brings difficulty.In addition, air humidity when experiment is difficult to control, drying temperature value range, which is difficult to determination, is all
Test problem encountered.
Summary of the invention
It is an object of the invention to solve shortcoming and deficiency of the existing technology, a kind of degradable good water permeability is provided
Chitosan film preparation method.
The purpose of the invention is achieved by the following technical solution:
A kind of preparation method of chitosan film includes the following steps: chitosan, glycerol and 2% (percentage by volume) second
Acid solution is uniformly mixed according to the ratio of 1g, 4g, 90mL, and centrifugation is debubblized, and obtains chitosan film liquid, chitosan film liquid is in 50 DEG C
Drying obtains chitosan film.Wherein, the relative molecular mass of chitosan is 110000.
Chitosan film of the invention can be used for food, medicine field, be coated as granule.
A kind of method that granule is coated, includes the following steps: for granule to be dipped into and is obtained by the above method
Chitosan film liquid, or chitosan film liquid is sprayed at granule surface, 50 DEG C of drying；It repeats to impregnate or spray, baking step
Three to five times, film liquid obtains the granule of coating after parching.
The invention has the advantages that and the utility model has the advantages that
(1) chitosan film water penetration of the invention is high, it is coated granule, substantially improves the outer of granule
It sees, weakens the stimulation to the sense of taste；Its high temperature resistant and stability is strong, can also be brewed repeatedly.
(2) chitosan film of the invention can be used as being coated in Chinese medicine, and Chinese medicine can be greatly increased after Chinese medicine is granulated again
The dissolution of interior nutriment, but wash out scattered since its powder after being granulated is easy to water, it then can solve this using Chitosan Coating
Problem.Chitosan Coating can both maintain the form of Chinese medicine after being granulated, and water penetration can guarantee the nutriment in Chinese medicine again
Dissolution.
(3) present invention provides theoretical foundation to the exploitation of water penetration Chitosan Coating and the research of profound level.
Detailed description of the invention
Fig. 1 is influence result figure of the relative molecular weight of chitosan to chitosan film performance.
Fig. 2 is influence result figure of the acetic acid concentration to chitosan film performance.
Fig. 3 is influence result figure of the acetic acid solution volume to chitosan film performance.
Fig. 4 is influence result figure of the glycerol additive amount to chitosan film performance.
Fig. 5 is influence result figure of the drying temperature to chitosan film performance.
Specific embodiment
Following embodiment should not be construed as limiting the invention for further illustrating the present invention.If not referring in particular to
Conventional means bright, that technological means used in embodiment is well known to those skilled in the art.
Material used in following embodiments and reagent are mainly as follows:
Chitosan (food grade): Sinopharm Chemical Reagent Co., Ltd.；Glacial acetic acid (analysis is pure): Chinese medicines group chemistry examination
Agent Co., Ltd；Edible glycerol (food grade): Zhengzhou Bo Yan Biotechnology Co., Ltd；Sodium hydroxide (analysis is pure): traditional Chinese medicines collection
Chemical reagent Co., Ltd, group；Anhydrous calcium chloride (analysis is pure): Sinopharm Chemical Reagent Co., Ltd..
Acetic acid solution: the liquid-transfering gun for being 1.000mL with specification draw respectively 1.000mL, 2.000mL, 3.000mL,
The glacial acetic acid of 4.000mL, 5.000mL use distilled water constant volume in the constant volume bottle of 100mL, obtain 1%, 2%, 3%, 4%, 5%
Acetic acid solution.
The single factor experiment of 1 chitosan film preparation condition of embodiment
(1) influence of the relative molecular weight of chitosan to film properties
It is respectively 110000,150000,400000,800000 chitosan using relative molecular mass, it is poly- according to 1g shell
Sugar is put into chitosan and acetic acid solution into beaker with the ratio that volume fraction is 2% acetic acid solution 90mL, and it is edible to add 4g
Glycerol is sufficiently mixed the bubble that rear 4000r/min is centrifuged in 10 minutes removal film liquids, obtains chitosan film liquid.The film that will be made
Liquid pours into culture dish, dries on 50 DEG C of thermostat water bath, and cooling is stood after film forming, pours into dilute solution of sodium hydroxide
(0.5mol/L) impregnates 10min, takes off film, natural air drying after washing obtains chitosan film.Chitosan film is measured by the following method
Water vapo(u)r transmission and water solubility.
The water vapo(u)r transmission of chitosan film measures: it is about that 4g is done that the chitosan film sample made, which is sealed in equipped with quality,
On the taper bottleneck of drying prescription (anhydrous calcium chloride), conical flask is placed in the environment that relative humidity is 50%, results of regular determination taper
The quality of bottle.Steam penetrating capacity (g/m is calculated as follows2H):
In formula (1), WVT is steam penetrating capacity, g/m2·h；Δ m is the incrementss of conical flask quality, g；When T is interval
Between, h；A is effectively to measure area, m2。
The water-soluble measurement of chitosan film: chitosan film is cut into the membrane sample that specification is 15mm × 15mm, membrane sample
It is put into the beaker for filling 50mL distilled water, beaker rim of a cup is sealed with preservative film, with anti-gray after drying at room temperature to constant weight
Dirt enters and the evaporation of distilled water.After 80 DEG C of dissolution 6h (stirring 30s every 0.5h), remaining undissolved film is taken out, is stood
Drying is to constant weight, according to the water solubility of poor quality for calculating chitosan film of film dissolution front and back.Water-soluble property coefficient is calculated as follows
(%):
In formula (2), S is water-soluble property coefficient, %；m0For the quality for dissolving preceding chitosan membrane sample, g；M is that dissolution rear shell is poly-
The quality of sugared membrane sample, g.
Use the water vapo(u)r transmission and water solubility of the chitosan film that the chitosan of different relative molecular masses is prepared
It the results are shown in Table 1 and Fig. 1.
Influence of 1 relative molecular weight of chitosan of table to chitosan film performance
Note: in table, a, b, c etc. indicate that 0.05 level difference is significant, and one or more letters are not identical then significant.Such as: if
One letter processing be a, then with all include a without significant difference and it is all not comprising a have significant difference；If more
A letter had not both included c with all then or had not included the processing of d there were significant differences such as cd, and contain c or d nothing it is significant
Difference.Similarly hereinafter.
With the increase of relative molecular weight of chitosan, the steam penetrating capacity of chitosan film is lower and lower, and reduces width
It spends larger.In addition from the point of view of the water-soluble rate of chitosan film, in the chitosan for the use of relative molecular mass being 110000, film water is molten
Rate is lower.With the increase of relative molecular mass, molecules align is closer, bigger to the interception of vapor, and water-soluble rate is low,
Therefore selecting the relative molecular mass of chitosan is 110000.
(2) influence of the acetic acid concentration to film properties
The chitosan for the use of relative molecular mass being 110000, be respectively divided into 1% according to 1g chitosan and volume fraction,
2%, the ratio of 3%, 4%, 5% acetic acid solution 90mL is put into chitosan and acetic acid solution into beaker, add 4g eat it is sweet
Oil is sufficiently mixed rear 4000r/min and is centrifuged 10 minutes, obtains chitosan film liquid.The film liquid made is poured into culture dish, in 50 DEG C
Thermostat water bath on dry, cooling is stood after film forming, dilute solution of sodium hydroxide is poured into and impregnates 10min, take off film, it is natural after washing
It air-dries, obtains chitosan film.According to the water vapo(u)r transmission and water solubility of the method measurement chitosan film in above-mentioned (1), as a result
It is shown in Table 2 and Fig. 2.
Influence of 2 acetic acid concentration of table to chitosan film performance
The steam penetrating capacity of chitosan film first increases as acetic acid concentration increases, when acetic acid concentration reaches 2%, with
The rising of acetic acid concentration and reduce.The water-soluble rate of chitosan film is reduced with the increase of acetic acid concentration, when acetic acid concentration reaches 5%
When, water-soluble rate curve levels off to gently.The too low chitosan that will lead to of acetic acid concentration dissolves insufficient, the excessively high then film liquid of acetic acid concentration
Penetrating odor can be had, and is possible to destroy the constituent of granule, therefore selects acetic acid concentration for 2%.
(3) influence of the acetic acid solution volume to film properties
The chitosan for the use of relative molecular mass being 110000, the second for being respectively 2% with volume fraction according to 1g chitosan
The ratio of acid solution volume 70mL, 80mL, 90mL, 100mL, 110mL are put into chitosan and acetic acid solution into beaker, add
4g edible glycerol is sufficiently mixed rear 4000r/min and is centrifuged 10 minutes, obtains chitosan film liquid.The film liquid made is poured into culture
Ware is dried on 50 DEG C of thermostat water bath, and cooling is stood after film forming, is poured into dilute solution of sodium hydroxide and is impregnated 10min, takes off film,
Natural air drying after washing, obtains chitosan film.According to the water vapo(u)r transmission and water of the method measurement chitosan film in above-mentioned (1)
Dissolubility the results are shown in Table 3 and Fig. 3.
Influence of the 3 acetic acid solution volume of table to chitosan film performance
When acetic acid solution volume is 90mL, the steam penetrating capacity of chitosan film is maximum, and the water-soluble rate of chitosan film is most
It is low.The too low film forming that will lead to of chitosan concentration is uneven, and the easy fragmentation of film, and tensile strength is too low, and chitosan concentration is excessively high then
Film liquid is sticky, and manufactured film thickness is too high.Therefore select acetic acid solution volume for 90mL.
(4) influence of the glycerol additive amount to film properties
The chitosan for the use of relative molecular mass being 110000 is 2% acetic acid solution according to 1g chitosan and volume fraction
The ratio of 90mL is put into chitosan and acetic acid solution into beaker, then is separately added into 1g, 2g, 3g, 4g, 5g edible glycerol, sufficiently
4000r/min is centrifuged 10 minutes after mixing, obtains chitosan film liquid.The film liquid made is poured into culture dish, in 50 DEG C of constant temperature
It is dried on water-bath, cooling is stood after film forming, poured into dilute solution of sodium hydroxide and impregnate 10min, take off film, natural air drying after washing,
Obtain chitosan film.According to the water vapo(u)r transmission and water solubility of the method measurement chitosan film in above-mentioned (1), it the results are shown in Table 4
And Fig. 4.
Influence of the 4 glycerol additive amount of table to chitosan film performance
The steam penetrating capacity of chitosan film increases with the increase of glycerol ratio, and increment becomes after glycerol additive amount is 4g
It is close gentle.The water-soluble rate of chitosan film is increased with the increase of glycerol additive amount, and when glycerol additive amount is excessive, chitosan film is easy
It absorbs water and easily tears, therefore select glycerol additive amount for 4g.
(5) influence of the drying temperature to film properties
The chitosan for the use of relative molecular mass being 110000 is 2% acetic acid solution according to 1g chitosan and volume fraction
The ratio of 90mL is put into chitosan and acetic acid solution into beaker, adds 4g edible glycerol, be sufficiently mixed rear 4000r/min from
The heart 10 minutes, obtain chitosan film liquid.The film liquid made is poured into culture dish, respectively at 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C
Thermostat water bath on dry, cooling is stood after film forming, dilute solution of sodium hydroxide is poured into and impregnates 10min, take off film, it is natural after washing
It air-dries, obtains chitosan film.According to the water vapo(u)r transmission and water solubility of the method measurement chitosan film in above-mentioned (1), as a result
It is shown in Table 5 and Fig. 5.
Influence of 5 drying temperature of table to chitosan film performance
The steam penetrating capacity of chitosan film and the water-soluble rate of chitosan film are reduced with the rising of drying temperature, work as baking
Two curves start to be decreased obviously when dry temperature is 50 DEG C.When drying temperature is low, the time of baking needed is greatly increased, drying
When the temperature is excessively high, it is easily broken after chitosan film is dry and is in faint yellow, therefore select drying temperature for 50 DEG C.
The orthogonal test of 2 chitosan film preparation condition of embodiment
Using the single factor experiment result of embodiment 1 as foundation, the relative molecular mass of chitosan is chosen, (shell is poly- for solid-to-liquid ratio
Sugar quality and 2% acetic acid solution volume ratio, g:mL), amounts of glycerol, drying temperature be factor of evaluation, with the water of chitosan film
Vapor permeation amount is tested with the quadrature analysis of 3 level, 4 factor of orthogonal software design as test result, carries out test knot
The analysis of fruit, experimental design factor and horizontal such as table 6, the results are shown in Table 7,8.
6 chitosan film orthogonal test level of table and factor
7 chitosan film preparation condition quadrature analysis experimental design of table and result
The variance analysis of each factor of table 8
Note: (*) indicates significant under 0.05 level, and (-) indicates without significant.
Influence of each factor to steam penetrating capacity, by 1g chitosan in terms of, by quadrature analysis it is found that working as chitosan phase
When being 110000 to molecular mass, steam penetrating capacity is maximum；When relative molecular mass is 400000, steam penetrating capacity is most
It is small.When acetic acid solution volume is 90mL, steam penetrating capacity is maximum；When acetic acid solution volume is 80mL, steam penetrating capacity is most
It is small.When glycerol additive amount is 4g, steam penetrating capacity is maximum；When glycerol additive amount is 3g, steam penetrating capacity is minimum.When film forming
Drying temperature when being 50 DEG C, steam penetrating capacity is maximum；When drying temperature is 60 DEG C, steam penetrating capacity is minimum.
Variance analysis, influence of the relative molecular mass to steam penetrating capacity are carried out to the steam penetrating capacity of chitosan film
Extremely significant, the influence of amounts of glycerol and drying temperature to steam penetrating capacity is more significant.
Therefore, combination A is primarily determined by orthogonal test1B2C2D2For Optimizing Technical, the system of water penetration Chitosan Coating
Standby process conditions are the chitosan that relative molecular mass is 110000, and acetic acid solution volume is 90mL, and glycerol additive amount is 4g, at
Drying temperature when film is 50 DEG C.
The reliability for examining orthogonality analysis method acquired results needs to carry out chitosan using the determination condition of above-mentioned optimization
The test of the steam penetrating capacity of film.In view of the condition of measurement is modified to using relative molecular mass by actual operational circumstances
For 110000 chitosan 1g, volume fraction is 2% acetic acid solution, and acetic acid solution volume is 90mL, and glycerol additive amount is 4g, is dried
Dry temperature is 50 DEG C.With this condition carry out 3 parallel tests, obtain chitosan film steam penetrating capacity (7.396 ±
0.203)g/m2·h.The relative error of actual value and theoretical value is 1.13%.
Application of 3 chitosan film of embodiment in granule coating
It will according to the ratio of 1g chitosan (relative molecular mass 110000), 4g edible glycerol, 2% acetic acid solution of 90mL
Chitosan and edible glycerol are dissolved in dilute acetic acid solutions, are uniformly mixed, and 4000r/min is centrifuged 10 minutes, obtain chitosan film liquid.
Chitosan film liquid is sprayed at water-soluble colored granule surface, 50 DEG C of drying (drying 10min) in vacuum oven is put into, repeats
Three times, it is placed again into vacuum oven and dries, until film liquid parches, obtain the granule of coating.There to be the particle of coating
Agent is brewed twice using boiled water, and particle is complete, boiled water discoloration；Particle has disintegration after brewing three times.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (4)
1. a kind of preparation method of chitosan film, characterized by the following steps: chitosan, glycerol and 2% acetic acid is molten
Liquid is uniformly mixed according to the ratio of 1g, 4g, 90mL, and centrifugation is debubblized, and obtains chitosan film liquid, and chitosan film liquid is dried in 50 DEG C
Obtain chitosan film；Wherein, the relative molecular mass of chitosan is 110000.
2. application of the chitosan film that preparation method according to claim 1 obtains in food, medicine field.
3. application according to claim 2, it is characterised in that: the chitosan film is coated as granule.
4. a kind of method that granule is coated, characterized by the following steps: be dipped into granule and pass through right
It is required that the chitosan film liquid that preparation method described in 1 obtains, or chitosan film liquid is sprayed at granule surface, 50 DEG C of drying；
It repeats to impregnate or spray, baking step three to five times, film liquid obtains the granule of coating after parching.
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Cited By (2)
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| CN110384214A (en) * | 2019-08-09 | 2019-10-29 | 云南大学 | A kind of method that coating method prepares ham |
| CN114716710A (en) * | 2022-03-21 | 2022-07-08 | 江南大学 | Method for improving physical property and oxidation resistance of chitosan film |
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