CN107488339A - A kind of preparation method of the transparent self-supporting film of antibacterial degradable based on PLA - Google Patents
A kind of preparation method of the transparent self-supporting film of antibacterial degradable based on PLA Download PDFInfo
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- CN107488339A CN107488339A CN201710800734.1A CN201710800734A CN107488339A CN 107488339 A CN107488339 A CN 107488339A CN 201710800734 A CN201710800734 A CN 201710800734A CN 107488339 A CN107488339 A CN 107488339A
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- 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
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- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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
- 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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- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
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Abstract
The invention discloses a kind of preparation method of the transparent self-supporting film of the antibacterial degradable based on PLA, this method is using polylactic acid PLA as material of main part, and chitosan CS is auxiliary material, and step is as follows：By N, N dimethylformamides drop in water after making PLA solution and chitosan solution blending as chloroform and the intermediate flux of formic acid, by phase separation method, obtain the self-supporting film with loose structure.Film prepared by the present invention has good anti-microbial property, and excellent transparency, regulatable degradation speed, method is simple, is easy to industrialization production and commercial applications.
Description
Technical field
The present invention is on a kind of preparation method of the transparent self-supporting film of the antibacterial degradable based on PLA, belongs to food
Product are fresh-keeping to wait the field of biomedical materials such as agricultural product field and tissue engineering bracket material.
Background technology
In the field of biomedical materials such as the agricultural product such as food fresh keeping field and tissue engineering bracket material, to suppressing micro- life
The amount reproduction and transparency of thing have higher requirement, while the existing antimicrobial film material applied to these fields is led at present
Often because non-degradable causes substantial amounts of environmental pollution and problem of energy crisis.In face of these problems, prepare and substitute petroleum base
Degradable antibacterial plastic product necessity and emergency arise at the historic moment.
PLA (PLA) is also equipped with other uniquenesses in addition to the degradable advantage for possessing general Biodegradable material
Advantage, such as：Good glossiness and transparency, good gas permeability, antibacterial and anti-mildew characteristic, outstanding physical property, quite
Good biocompatibility and the accreditation of United States food and drag administration (FDA), therefore PLA is selected as degradable films
Main component, it is faster and better applied to food and medicine field.
Chitosan (CS), it is widely present in nature, it may have outstanding biodegradability, biocompatibility and antibacterial
Performance, using chitosan as auxiliary element, it is primarily due to chitosan and is provided simultaneously with 2 unique properties：Hydrophily, improve
The hydrophilic and hydrophobic of polylactic acid membrane, promote PLA degraded；Cation type polymer, alkaline small thing can be discharged during degraded
Matter, neutralize lactic acid caused by PLA degraded, Delayed onset foreign matter inflammatory reaction caused by suppression PLA.
By PLA and chitosan blend, preparing the PLA/CS with anti-microbial property by phase separation method can drop
Solve transparent membrane.This method does not both need large scale equipment, does not need high-temperature and high-pressure conditions and shuttering supporting again, can control life
Cost is produced, improves processing safety.The film that profit is prepared in this way simultaneously has loose structure, can regulate and control degraded speed
Rate.
The content of the invention
Technical problem：The present invention is intended to provide one kind is provided simultaneously with antibacterial, degradable, transparency is high and four kinds of self-supporting is excellent
The preparation of the transparent self-supporting film of the antibacterial degradable based on PLA suitable for industrialization production and commercial applications of point
Method, explain the mechanism between surface modification and membrane structure performance.Being prepared by phase separation method has anti-microbial property
The degradable transparent self-supporting film of PLA/chitosan.
Technical scheme：A kind of preparation method of the transparent self-supporting film of antibacterial degradable based on PLA of the present invention
For：PLA solution and chitosan solution are blended to obtain using N,N-dimethylformamide as the intermediate flux of chloroform and formic acid
PLA and chitosan solution blend solution, then the blend solution is dropped in water, form one by phase separation method
Strata lactic acid-chitosan blend self-supporting film；The film is provided simultaneously with antibacterial, degradable, the high spy with self-supporting of transparency
Property.
Wherein：
It is described using DMF as chloroform and the intermediate flux of formic acid, make PLA solution and chitosan molten
Liquid blending detailed process be：It is PLA solution I of the solvent configuration quality volume ratio as 20mg/ml-50mg/ml using chloroform,
It is 5mg/ml-12.5mg/ml chitosan solutions II that mass volume ratio is prepared by solvent of formic acid；According to volume ratio 2:1-1:1,
Quantitative DMF is added dropwise under condition of heating and stirring into solution I, is configured to 2:1-1:The chloroform of 1 ratio:N,
Dinethylformamide is the PLA solution III of cosolvent；The solution II prepared is added dropwise to the speed of 3-5 drops per second
In PLA solution III, heating stirring mixing 5-10min, PLA and chitosan solution blend solution are obtained.
It is described to be dropped to after PLA solution and chitosan solution blending in water, form one by phase separation method
The detailed process of strata lactic acid-chitosan blend self-supporting film is：By the PLA and chitosan solution blend solution with
The speed of 3-5 drops per second is instilled in water, after standing 5-10min, the adrift self-supporting film of layer of transparent on the water surface；By the water surface
Upper afloat film picks up, and puts into 50 DEG C of -65 DEG C of baking ovens and dries 1h-5h, that is, obtains the PLA-shell with anti-microbial property
The degradable transparent self-supporting film of glycan.
The PLA solution III, when preparing, heating-up temperature is 55 to 65 DEG C, mixing speed 750-850rpm, stirring
Incorporation time is 5-10min.
PLA and the chitosan solution blend solution, its volume ratio are：PLA solution III：Chitosan solution II=
(3-8):1, heating-up temperature is 55-65 DEG C, mixing speed 750-850rpm.
For this film using PLA as material of main part, chitosan is auxiliary material, by phase separation method, is obtained
Self-supporting film with loose structure, there is good anti-microbial property, excellent transparency, regulatable degradation speed, side
Method is simple, is easy to industrialization production and commercial applications.
Beneficial effect：The present invention compared with prior art, has advantages below：
1st, the innovation in terms of preparation method, rarely have prepare the base with anti-microbial property using phase separation method at present
In the research of polylactic acid degradable self-supporting film, this method is easy and effective, and device is simple, and cost is low, can be quick without substrate
Efficiently it is prepared on a large scale.
2nd, in terms of product, transparency height (transmitance>95%), degradation rate can regulate and control, and antibiotic property is good.
3rd, have a wide range of application:The degradable transparent membrane of PLA/chitosan anti-bacteria of acquisition, can apply to food fresh keeping
Deng field of biomedical materials such as agricultural product field and tissue engineering bracket materials, reduce environmental pollution simultaneously.
Brief description of the drawings
Fig. 1 is that the antibacterial effect of polylactic acid-chitose blend film contrasts, (a) blank control group, (b) 7/1 PLA-shell
Glycan blend film, (c) pure polylactic acid membrane.
Fig. 2 is the degradation effect comparison diagram of polylactic acid-chitose blend film.
Fig. 3 is the transparency interaction comparison diagram of polylactic acid-chitose blend film.
Embodiment
The present invention is done with reference to embodiment and further explained, the following example is merely to illustrate the present invention, but
It is not used to limit the practical range of the present invention.
A kind of preparation method of the transparent self-supporting film of antibacterial degradable based on PLA comprises the following steps：
Step 1: the PLA solution I for being 20mg/ml to 50mg/ml as solvent configuration quality volume ratio using chloroform, with first
Acid is that to prepare mass volume ratio be 5mg/ml to 12.5mg/ml chitosan solutions II to solvent；
Step 2: according to volume ratio 1:1, quantitative N, N- dimethyl methyls is added dropwise into solution I under condition of heating and stirring
Acid amides, it is configured to 1:The chloroform of 1 ratio:N,N-dimethylformamide is the (heating-up temperature 55 of PLA solution III of cosolvent
To 65 DEG C, mixing speed is 750 to 850rpm, is stirred the time as 5 to 10min)；
Step 3: the solution II prepared is added dropwise to the 3 drops speed per second to 5 drops per second according to certain mixed proportion
In solution III, heating stirring mixing 5min to 10min, PLA and chitosan solution blend solution IV (the poly- breasts of volume ratio are obtained
Acid solution III：The mixed proportion of chitosan solution II is 3:1 to 8:1, heating-up temperature be 55 to 65 DEG C, mixing speed be 750 to
850rpm)。
Step 4: blend solution IV is instilled in water with the 3 drops speed per second to 5 drops per second, 5min to 10min is stood
Afterwards, the adrift self-supporting film of layer of transparent on the water surface；
Step 5: afloat film on the water surface is picked up, put into 50 DEG C to 65 DEG C baking ovens and dry 1h to 5h, that is, obtain
The degradable transparent self-supporting film of PLA/chitosan with anti-microbial property.
Embodiment 1
1) it is PLA solution I of the solvent configuration quality volume ratio as 20mg/ml using chloroform, matter is prepared by solvent of formic acid
Amount volume ratio is 5mg/ml chitosan solutions II；
2) according to volume ratio 1:1, quantitative DMF is added dropwise into solution I under condition of heating and stirring,
It is configured to 1:The chloroform of 1 ratio:DMF be cosolvent PLA solution III (heating-up temperature be 55 DEG C, stir
It is 750rpm to mix speed, and it is 10min to be stirred the time)；
3) according to volume ratio PLA solution III：Chitosan solution II=7:1 ratio, by the solution II prepared with 3
Drip speed per second to be added dropwise in solution III, heating stirring mixing 10min, obtain PLA and chitosan solution blend solution IV
(heating-up temperature is 55 to 65 DEG C, mixing speed 750rpm).
4) blend solution IV is instilled in water with 3 drop speed per second, after standing 10min, adrift one layer thoroughly on the water surface
Bright self-supporting film；
5) afloat film on the water surface is picked up, puts into 50 DEG C of baking ovens and dry 5h, that is, obtain that there is anti-microbial property
The degradable transparent self-supporting film of PLA/chitosan.
Embodiment 2
1) 1) using chloroform it is PLA solution I of the solvent configuration quality volume ratio as 30mg/ml, is prepared by solvent of formic acid
Mass volume ratio is 7.5mg/ml chitosan solutions II；
2) according to volume ratio 1:1, quantitative DMF is added dropwise into solution I under condition of heating and stirring,
It is configured to 1:The chloroform of 1 ratio:DMF be cosolvent PLA solution III (heating-up temperature be 55 DEG C, stir
It is 750rpm to mix speed, and it is 10min to be stirred the time)；
3) according to volume ratio PLA solution III：Chitosan solution II=6:1 ratio, by the solution II prepared with 3
Drip speed per second to be added dropwise in solution III, heating stirring mixing 10min, obtain PLA and chitosan solution blend solution IV
(heating-up temperature is 55 to 65 DEG C, mixing speed 750rpm).
4) blend solution IV is instilled in water with 3 drop speed per second, after standing 10min, adrift one layer thoroughly on the water surface
Bright self-supporting film；
5) afloat film on the water surface is picked up, puts into 50 DEG C of baking ovens and dry 5h, that is, obtain that there is anti-microbial property
The degradable transparent self-supporting film of PLA/chitosan.
Embodiment 3
1) 1) PLA solution I using chloroform as solvent configuration quality volume ratio 40mg/ml, matter is prepared by solvent of formic acid
Amount volume ratio is 10mg/ml chitosan solutions II；
2) according to volume ratio 1:1, quantitative DMF is added dropwise into solution I under condition of heating and stirring,
It is configured to 1:The chloroform of 1 ratio:DMF be cosolvent PLA solution III (heating-up temperature be 55 DEG C, stir
It is 750rpm to mix speed, and it is 10min to be stirred the time)；
3) according to volume ratio PLA solution III：Chitosan solution II=8:1 ratio, by the solution II prepared with 3
Drip speed per second to be added dropwise in solution III, heating stirring mixing 10min, obtain PLA and chitosan solution blend solution IV
(heating-up temperature is 55 to 65 DEG C, mixing speed 750rpm).
4) blend solution IV is instilled in water with 3 drop speed per second, after standing 10min, adrift one layer thoroughly on the water surface
Bright self-supporting film；
5) afloat film on the water surface is picked up, puts into 50 DEG C of baking ovens and dry 5h, that is, obtain that there is anti-microbial property
The degradable transparent self-supporting film of PLA/chitosan.
Embodiment 4
1) it is PLA solution I of the solvent configuration quality volume ratio as 50mg/ml using chloroform, matter is prepared by solvent of formic acid
Amount volume ratio is 12.5mg/ml chitosan solutions II；
2) according to volume ratio 1:1, quantitative DMF is added dropwise into solution I under condition of heating and stirring,
It is configured to 1:The chloroform of 1 ratio:DMF be cosolvent PLA solution III (heating-up temperature be 55 DEG C, stir
It is 750rpm to mix speed, and it is 10min to be stirred the time)；
3) according to volume ratio PLA solution III：Chitosan solution II=5:1 ratio, by the solution II prepared with 3
Drip speed per second to be added dropwise in solution III, heating stirring mixing 10min, obtain PLA and chitosan solution blend solution IV
(heating-up temperature is 55 to 65 DEG C, mixing speed 750rpm).
4) blend solution IV is instilled in water with 3 drop speed per second, after standing 10min, adrift one layer thoroughly on the water surface
Bright self-supporting film；
5) afloat film on the water surface is picked up, puts into 50 DEG C of baking ovens and dry 5h, that is, obtain that there is anti-microbial property
The degradable transparent self-supporting film of PLA/chitosan.
Claims (5)
- A kind of 1. preparation method of the transparent self-supporting film of antibacterial degradable based on PLA, it is characterised in that：By N, N- bis- PLA solution and chitosan solution are blended to obtain PLA and shell by NMF as the intermediate flux of chloroform and formic acid Glycan solution blending solution, then the blend solution is dropped in water, a strata lactic acid-shell is formed by phase separation method Self-supporting film is blended in glycan；The film is provided simultaneously with antibacterial, degradable, the high characteristic with self-supporting of transparency.
- 2. the preparation method of the transparent self-supporting film of antibacterial degradable as claimed in claim 1 based on PLA, its feature It is：It is described using DMF as chloroform and the intermediate flux of formic acid, make PLA solution and chitosan solution The detailed process of blending is：It is PLA solution I of the solvent configuration quality volume ratio as 20mg/ml-50mg/ml using chloroform, with Formic acid is that solvent preparation mass volume ratio is 5mg/ml-12.5mg/ml chitosan solutions II；According to volume ratio 2:1-1:1, adding Quantitative DMF is added dropwise under the conditions of thermal agitation into solution I, is configured to 2:1-1:The chloroform of 1 ratio:N,N- Dimethylformamide is the PLA solution III of cosolvent；The solution II prepared is added dropwise to the speed of 3-5 drops per second poly- In lactic acid solution III, heating stirring mixing 5-10min, PLA and chitosan solution blend solution are obtained.
- 3. the preparation method of the transparent self-supporting film of the antibacterial degradable according to claim 1 based on PLA, it is special Sign is：It is described to be dropped to after PLA solution and chitosan solution blending in water, form one by phase separation method The detailed process of strata lactic acid-chitosan blend self-supporting film is：By the PLA and chitosan solution blend solution with The speed of 3-5 drops per second is instilled in water, after standing 5-10min, the adrift self-supporting film of layer of transparent on the water surface；By the water surface Upper afloat film picks up, and puts into 50 DEG C of -65 DEG C of baking ovens and dries 1h-5h, that is, obtains the PLA-shell with anti-microbial property The degradable transparent self-supporting film of glycan.
- 4. the preparation method of the transparent self-supporting film of the antibacterial degradable according to claim 1 based on PLA, it is special Sign is：The PLA solution III, when preparing, heating-up temperature is 55 to 65 DEG C, mixing speed 750-850rpm, stirring Incorporation time is 5-10min.
- 5. the preparation method of the transparent self-supporting film of the antibacterial degradable according to claim 1 based on PLA, it is special Sign is：PLA and the chitosan solution blend solution, its volume ratio are：PLA solution III：Chitosan solution II= (3-8):1, heating-up temperature is 55-65 DEG C, mixing speed 750-850rpm.
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| CN201710800734.1A CN107488339A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation method of the transparent self-supporting film of antibacterial degradable based on PLA |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610502A (en) * | 2018-04-25 | 2018-10-02 | 东南大学 | The preparation method of transparent self-supporting packing film based on polylactic acid Visible Light Induced Photocatalytic |
| CN110655766A (en) * | 2019-10-14 | 2020-01-07 | 成都大学 | Preparation method of polylactic acid porous membrane for food preservation |
-
2017
- 2017-09-07 CN CN201710800734.1A patent/CN107488339A/en active Pending
Non-Patent Citations (2)
| Title |
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| 刘欢: ""聚L乳酸/壳聚糖抗菌膜的制备及性能研究"", 《中国优秀硕士学位论文全文数据库 工程科技II辑》 * |
| 陈光岩等: ""超临界二氧化碳在膜制备过程中的应用进展"", 《化工科技》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610502A (en) * | 2018-04-25 | 2018-10-02 | 东南大学 | The preparation method of transparent self-supporting packing film based on polylactic acid Visible Light Induced Photocatalytic |
| CN108610502B (en) * | 2018-04-25 | 2020-05-05 | 东南大学 | Preparation method of transparent self-supporting packaging film based on polylactic acid visible light degradation |
| CN110655766A (en) * | 2019-10-14 | 2020-01-07 | 成都大学 | Preparation method of polylactic acid porous membrane for food preservation |
| CN110655766B (en) * | 2019-10-14 | 2021-06-22 | 成都大学 | Preparation method of polylactic acid porous membrane for food preservation |
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Application publication date: 20171219 |