CN107353611A - The preparation technology of slow released ClO 2 microcapsule antibacterial film - Google Patents
The preparation technology of slow released ClO 2 microcapsule antibacterial film Download PDFInfo
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- CN107353611A CN107353611A CN201710527194.4A CN201710527194A CN107353611A CN 107353611 A CN107353611 A CN 107353611A CN 201710527194 A CN201710527194 A CN 201710527194A CN 107353611 A CN107353611 A CN 107353611A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a kind of preparation technology of slow released ClO 2 microcapsule antibacterial film, this method includes following operating procedure：1) microscapsule powder is prepared：By Gelatin in stability chlorine dioxide water solution, aqueous phase solution is obtained；PLA is dissolved in dichloromethane, obtains oil-phase solution；The emulsifying agent of Span 80 is added in oil-phase solution, aqueous phase solution and atoleine stirring is added, vacuum filtration, is freeze-dried to obtain chlorine dioxide microscapsule powder；2) antibacterial film is prepared：Into chlorine dioxide microscapsule powder, activator and plasticizer was added in film base material PLA, after stirring, 60min is stood, bubble is eliminated, with flat board coating machine coating film forming.Antibacterial film is prepared using the inventive method, has raw material sources wide, safety and sanitation, the advantages that biodegradable, and there is strong antibacterial action, the sustained release cycle is grown, and is had broad application prospects in fresh food fresh-keeping aspect.
Description
Technical field
The present invention relates to a kind of preparation method of edible film, specifically a kind of slow released ClO 2 microcapsule antibacterial film
Preparation technology.
Technical background
Chlorine dioxide (ClO2) it is that the safe efficient, wide spectrum that confirms of World Health Organization (WHO), strength are nontoxic
Bactericide, its effective chlorine are 2.63 times of chlorine, and sterilizing ability is 5 times of chlorine, is more than 50 times of sodium hypochlorite, due to it
Chlorine alternative reaction will not occur, thus carcinogenic, aberration inducing organic chloro-product will not be produced, being classified as A1 level securities by WHO disappears
Toxic agent.Microcapsules technology is that one kind utilizes filmogen solid, liquid or gas entrapment into functional core shell structure bag
The technology of compound.Prepared inclusion compound is referred to as microcapsules, the particle diameter of microcapsules generally at several microns to thousands of microns, wherein,
The wrapped material in inside is referred to as core, is also guest molecule, outside capsulating material is referred to as wall material, is also host molecule, wall
Material is generally natural or synthetic high polymer material, and core can be liquid, solid, may also be gas, can be one or more of
The mixture of material.Microcapsules have protection, barrier, the core material by shell protection had not both been invaded by external environment
Enter to influence, while there is the barrier property that will not outwardly escape again, product made from microcapsules technology has good feature
And storage-stable.Stable ClO 2 solution has the advantages that water white transparency, property is stable, and chlorine dioxide content is high, but
Meet in illumination, acid, high content carbon dioxide and high humidity environment and easily react, ineffective effect.
The patent document for preparing packaging film using chlorine dioxide at present also has following several technical schemes：
1) a kind of fresh-keeping packaging material of slowly-releasing chlorine dioxide bactericide has been invented by Beijing Printing Institute.The fresh-keeping packaging material
Material is cast in the modified highly-breathable curtain coating polyethylene of polyethylene outer membrane, ethylene-vinyl acetate copolymer (EVA) by highly-breathable
Film, the laminated film being prepared by the adhesive dry laminating of the powder of releasing agent containing chlorine dioxide, the film are exhaled using fruits and vegetables
Vapor caused by suction effect induces film release low concentration gas phase chlorine dioxide bactericide, extends the shelf life of fruits and vegetables, improves
The quality of fruits and vegetables.
2) a kind of oyster shell-stealthy chlorine dioxide anti-biotic material has been invented by University Of Qingdao.This anti-biotic material is existed by particle diameter
Less than 50 μm of oyster shell powder mixes with sodium chlorite powder, niter cake powder, obtains a kind of mixture.
3) a kind of chlorine dioxide slow-release tin foil has been invented by Northeast Forestry University.Using sodium chlorite as antistaling agent, with winestone
Acid is activator, and poromeric material is base material；Sodium chlorite and sodium hydroxide are scattered in oxidized starch glue masking liquid is made, then
Masking liquid is coated on base material A；Tartaric acid solution is obtained by tartaric acid is soluble in water, tartaric acid solution is applied on base material B,
A, B, which is bonded, produces chlorine dioxide slow-release tin foil.
But preparation of the studies above person to chlorine dioxide anti-biotic material, be mostly direct addition sodium chlorite powder and
Organic acid.Sodium chlorite is the presoma for producing chlorine dioxide, is blended directly in material, under illumination, high temperature, super-humid conditions
It is unstable, it is extremely easy in decomposition, this limits the yield of chlorine dioxide and action time to a certain extent.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation of slow released ClO 2 microcapsule antibacterial film
Technique, it is short that the technique can solve chlorine dioxide action time, the problems such as antibacterial effect difference.
The present invention solves above-mentioned technical problem with following technical scheme：
The preparation technology of slow released ClO 2 microcapsule antibacterial film of the present invention, including following operating procedure：
1) microscapsule powder is prepared：By Gelatin in stability chlorine dioxide water solution, in 40 DEG C of thermostat water baths
Middle dissolving 60min, gelatin concentration is 1-100g/L in obtained aqueous phase solution；PLA is dissolved in dichloromethane, stirred in machinery
120min is stirred under the conditions of mixing, PLA concentration is 1-200g/L in obtained oil-phase solution；Oil-phase solution is placed in mechanical agitator
Upper stirring, the emulsifying agent of Span 80 is added while stirring, is stirring evenly and then adding into aqueous phase solution, then at 300-2000r/min at a high speed
The lower atoleine that adds of stirring continues to stir, and then uses magnetic stirring apparatus with 200r/min stirring at low speed 120-240min, volatilization
Fall dichloromethane, be filtered by vacuum, be freeze-dried to obtain chlorine dioxide microscapsule powder；
2) antibacterial film is prepared：PLA is dissolved in the film forming base that PLA mass concentration is configured in dichloromethane as 5-30%
Material PLA, then added the chlorine dioxide microscapsule powder, activator tartaric acid and plasticizer acetyl tributyl citrate three of 400 mesh
Butyl ester, the addition of chlorine dioxide microscapsule powder are the 20% of PLA dry weights, and the addition of activator tartaric acid presses formula：
5ClO2 -+4H+=4ClO2+Cl-+2H2O is calculated, and the addition of plasticizer tributyl 2-acetylcitrate is the 5-30% of PLA dry weights,
After stirring, 60min is stood, bubble is eliminated, with flat board coating machine coating film forming.
In step 1), the volume ratio of aqueous phase solution and oil-phase solution is 1:The addition of 1~20,80 emulsifying agents is oil phase
The 1-20% of liquor capacity；The addition of atoleine is the 2/3 of oil-phase solution volume.
The inventive method uses microcapsules technology, and precursors cladding is got up, and reduces influence of the environment to it, and will
Microcapsules are added in film, PLA film is had strong antibacterial action, and extend its antibacterial term of validity, and this has to fresh food
Important meaning.
The antibacterial film that the inventive method is prepared has the characteristics that：
1) the antibacterial film tensile strength is 15.82-21.20MPa, elongation at break 6.80-24.00%, to large intestine bar
The bacteriostasis rate of bacterium and staphylococcus aureus is all in more than 90%-99%.
2) antibacterial film extends the release time of chlorine dioxide, its low amounts is persistently discharged, and has Durability of antimicrobial effect.
3) antibacterial film is naturally degradable, green, is a kind of preferable antibiotic packaging material.
Embodiment
The inventive method utilizes microcapsules technology, with PLA (PLA) for wall material, with gelatin/stability chlorine dioxide water
Solution (aqueous phase solution) is core, and stability chlorine dioxide water solution is prepared into chlorine dioxide microcapsules, and chlorine dioxide is micro-
Capsule and organic acid are added in PLA films, and slow released ClO 2 antibacterial film is made with spread plate.
The preparation technology of the chlorine dioxide microcapsules is：By Gelatin in stability chlorine dioxide water solution,
60min is dissolved in 40 DEG C of thermostat water baths, gelatin concentration is 1-100g/L in obtained aqueous phase solution；PLA is dissolved in dichloro
In methane, 120min is stirred under mechanical agitation, PLA concentration is 1-200g/L in obtained oil-phase solution；Oil phase is molten
Liquid is placed on mechanical agitator and stirred, and adds the emulsifying agent of Span 80 while stirring, is stirring evenly and then adding into aqueous phase solution, then at
Atoleine is added under 300-2000r/min high-speed stirreds to continue to stir, and is then stirred with magnetic stirring apparatus with 200r/min low speed
120-240min is mixed, vapors away dichloromethane, is filtered by vacuum, is freeze-dried to obtain chlorine dioxide microscapsule powder.
The preparation technology of the slow released ClO 2 antibacterial film is：PLA is dissolved in dichloromethane and is configured to PLA's
Mass concentration be 5-30% into film base material PLA, then added chlorine dioxide microscapsule powder, the activator winestone of 400 mesh
Acid and plasticizer tributyl 2-acetylcitrate, the addition of chlorine dioxide microscapsule powder are the 20% of PLA dry weights, activator
The addition of tartaric acid presses formula： 5ClO2 -+4H+=4ClO2+Cl-+2H2O is calculated, and plasticizer tributyl 2-acetylcitrate adds
Enter the 5-30% that amount is PLA dry weights, after stirring, stand 60min, bubble is eliminated, with flat board coating machine coating film forming.
Above-mentioned formula：5ClO2 -+4H+=4ClO2+Cl-+2H2In O, ClO2 -Represent NaClO2(included in microcapsules
NaClO2),H+Represent organic acid (such as tartaric acid), NaClO2Occupy certain proportion (being referred to as embedding rate) in microcapsules, according to
The content of embedding rate and addition microcapsules can draw NaClO2Quality, according to NaClO2Quality and above-mentioned formula drawn
Machine acid quality.
In step 1), the volume ratio of aqueous phase solution and oil-phase solution is 1:The addition of 1~20,80 emulsifying agents is oil phase
The 1-20% of liquor capacity；The addition of atoleine is the 2/3 of oil-phase solution volume.
Antibacterial film of the present invention passes through the effect of moisture, PLA generation corrosions, chlorine dioxide microcapsules and organic acid utilization water
Shunt excitation is lived, and the behavior such as diffusive migration, which reacts, in PLA film generates antibiotic property Chlorine Dioxide Gas to reach the purpose of antibacterial.
It is the embodiment of the inventive method below, but protection scope of the present invention is not limited to following instance：
Embodiment 1, the preparation technology of antibacterial film are as follows：
1) preparation of chlorine dioxide microcapsules：0.1g Gelatins are taken in 100ml, the stability that concentration is 37000mg/L
In aqueous solution of chlorine dioxide, 60min is dissolved in 40 DEG C of thermostat water baths, obtains aqueous phase solution, it is standby.0.1g PLA are taken to dissolve
In 100ml dichloromethane, 120min is stirred under mechanical agitation, is allowed to be completely dissolved, obtains oil-phase solution.Measure
30ml oil-phase solutions are placed on mechanical agitator and stirred, and add the emulsifying agent of 0.3ml Spans 80 while stirring, are stirring evenly and then adding into
30ml aqueous phase solutions, after 300r/min stirs 5min, 20ml atoleines are added, continued after stirring 1min, transfer magnetic
Power agitator vapors away dichloromethane with 200r/min stirring at low speed 180min.Vacuum filtration, is freeze-dried to obtain microcapsule powder
End.
2) preparation of antibacterial film：5g PLA are taken, 5% (w/v) PLA/ dichloromethane solution 100g are prepared, in mechanical agitator
Upper stirring 120min, is allowed to be completely dissolved, added the chlorine dioxide microcapsules 1g of 400 mesh, activator tartaric acid 0.005g,
Plasticizer tributyl 2-acetylcitrate 0.25g, after stirring, 60min is stood, bubble is eliminated, is coated into flat board coating machine
Film.20 DEG C are placed in, 120min is dried in RH50% climate box.
Antibacterial film tensile strength prepared by the embodiment 1 is 15.82MPa, elongation at break 24.00%, to large intestine
The bacteriostasis rate of bacillus and staphylococcus aureus is all more than 90%.
Embodiment 2, the preparation technology of antibacterial film are as follows：
1) prepared by chlorine dioxide microcapsules：5g Gelatins are taken in 100ml, the stability dioxy that concentration is 37000mg/L
Change in chlorine water solution, dissolve 60min in 40 DEG C of thermostat water baths, obtain aqueous phase solution, it is standby.10gPLA is taken to be dissolved in
In 100ml dichloromethane, 120min is stirred under mechanical agitation, is allowed to be completely dissolved, obtains oil-phase solution.Measure
30ml oil-phase solutions are placed on mechanical agitator and stirred, and add the emulsifying agent of 3ml Spans 80 while stirring, are stirring evenly and then adding into
3ml aqueous phase solutions, after 1200r/min high-speed stirreds 2min, 20ml atoleines are added, continued after stirring 1min, transfer is used
Magnetic stirring apparatus vapors away dichloromethane with 200r/min stirring at low speed 180min.Vacuum filtration, is freeze-dried to obtain microcapsule powder
End.
2) preparation of antibacterial film：15g PLA are taken, 25% (w/v) PLA/ dichloromethane solution 100ml is prepared, is stirred in machinery
Mix and 120min is stirred on device, be allowed to be completely dissolved, added chlorine dioxide microcapsules 3g, the activator tartaric acid of 400 mesh
0.02g and plasticizer tributyl 2-acetylcitrate 5g, after stirring, 60min is stood, eliminates bubble, is applied with flat board coating machine
Cloth film forming.20 DEG C are placed in, 120min is dried in RH50% climate box.
Antibacterial film tensile strength prepared by the embodiment 2 is 21.20MPa, elongation at break 7.1%, to large intestine bar
The bacteriostasis rate of bacterium and staphylococcus aureus is all more than 99%.
Embodiment 3, the preparation technology of antibacterial film are as follows：
1) prepared by chlorine dioxide microcapsules：10g Gelatins are taken in 100ml, the stability two that concentration is 37000mg/L
In the chlorine monoxid aqueous solution, 60min is dissolved in 40 DEG C of thermostat water baths, obtains aqueous phase solution, it is standby.20gPLA is taken to be dissolved in
In 100ml dichloromethane, 120min is stirred under mechanical agitation, is allowed to be completely dissolved, obtains oil-phase solution.Measure
30ml oil-phase solutions are placed on mechanical agitator and stirred, and add the emulsifying agent of 6ml Spans 80 while stirring, are stirring evenly and then adding into
1.5ml obtains aqueous phase solution, after 2000r/min high-speed stirreds 3min, adds 20ml atoleines, continues after stirring 1min, turns
Magnetic stirring apparatus is diverted from one use to another with 200r/min stirring at low speed 180min, vapors away dichloromethane.Vacuum filtration, is freeze-dried to obtain micro- glue
Capsule powder.
2) preparation of antibacterial film：30g PLA are taken, 30% (w/v) PLA/ dichloromethane solution 100g are prepared, in mechanical agitation
120min is stirred on device, is allowed to be completely dissolved, added the chlorine dioxide microcapsules 6g of 400 mesh, activator tartaric acid 0.04g,
Plasticizer tributyl 2-acetylcitrate 9g, after stirring, 60min is stood, bubble is eliminated, with flat board coating machine coating film forming.
20 DEG C are placed in, 120min is dried in RH50% climate box.
Antibacterial film tensile strength prepared by the embodiment 3 is 16.86MPa, elongation at break 6.8%, to large intestine bar
The bacteriostasis rate of bacterium and staphylococcus aureus is all more than 95%.
Claims (3)
1. the preparation technology of slow released ClO 2 microcapsule antibacterial film, it is characterised in that it includes following operating procedure：
1) microscapsule powder is prepared：It is molten in 40 DEG C of thermostat water baths by Gelatin in stability chlorine dioxide water solution
60min is solved, gelatin concentration is 1-100g/L in obtained aqueous phase solution；PLA is dissolved in dichloromethane, in mechanical agitation bar
120min is stirred under part, PLA concentration is 1-200g/L in obtained oil-phase solution；Oil-phase solution is placed on mechanical agitator and stirred
Mix, add the emulsifying agent of Span 80 while stirring, aqueous phase solution is stirring evenly and then adding into, then at 300-2000r/min high-speed stirreds
Lower addition atoleine continues to stir, and then vapors away two with magnetic stirring apparatus with 200r/min stirring at low speed 120-240min
Chloromethanes, vacuum filtration, is freeze-dried to obtain chlorine dioxide microscapsule powder；
2) antibacterial film is prepared：It is 5-30% into film base material PLA to be dissolved in PLA mass concentration is configured in dichloromethane
PLA, then added the chlorine dioxide microscapsule powder, activator tartaric acid and the fourth of plasticizer acetyl tributyl citrate three of 400 mesh
Ester, the addition of chlorine dioxide microscapsule powder are the 20% of PLA dry weights, and the addition of activator tartaric acid presses formula：5ClO2 -
+4H+=4ClO2+Cl-+2H2O is calculated, and the addition of plasticizer tributyl 2-acetylcitrate is the 5-30% of PLA dry weights, stirring
After uniformly, 60min is stood, bubble is eliminated, with flat board coating machine coating film forming.
2. the preparation technology of slow released ClO 2 microcapsule antibacterial film according to claim 1, it is characterised in that step
1) in, the volume ratio of aqueous phase solution and oil-phase solution is 1:The addition of 1~20,80 emulsifying agents is the 1- of oil-phase solution volume
20%；The addition of atoleine is the 2/3 of oil-phase solution volume.
3. the preparation technology of slow released ClO 2 microcapsule antibacterial film according to claim 1 or claim 2, it is characterised in that
The concentration of the stability chlorine dioxide water solution is 37000mg/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484027A (en) * | 2020-06-11 | 2020-08-04 | 漳州阳盛贸易有限公司 | Kaolin product for catalytic cracking catalyst and preparation method thereof |
| CN113367153A (en) * | 2021-06-04 | 2021-09-10 | 湖南天为环保科技有限公司 | Deodorant based on chlorine dioxide |
| CN116041763A (en) * | 2023-02-28 | 2023-05-02 | 广西大学 | Humidity response type chlorine dioxide slow-release fresh-keeping film and preparation method thereof |
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| CN106476380A (en) * | 2016-09-30 | 2017-03-08 | 广西大学 | A kind of preparation technology of slow released ClO 2 antibacterial film |
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| CN106476380A (en) * | 2016-09-30 | 2017-03-08 | 广西大学 | A kind of preparation technology of slow released ClO 2 antibacterial film |
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| 池致超等: ""稳定性二氧化氯胶囊的制备及其释放速率的研究"，池致超等，《食品工业科技》，第31卷第2期，2010年2月", 《食品工业科技》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484027A (en) * | 2020-06-11 | 2020-08-04 | 漳州阳盛贸易有限公司 | Kaolin product for catalytic cracking catalyst and preparation method thereof |
| CN113367153A (en) * | 2021-06-04 | 2021-09-10 | 湖南天为环保科技有限公司 | Deodorant based on chlorine dioxide |
| CN116041763A (en) * | 2023-02-28 | 2023-05-02 | 广西大学 | Humidity response type chlorine dioxide slow-release fresh-keeping film and preparation method thereof |
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