CN109280194A - A kind of preparation method of antibacterial polylactic acid film - Google Patents
A kind of preparation method of antibacterial polylactic acid film Download PDFInfo
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- CN109280194A CN109280194A CN201811099916.1A CN201811099916A CN109280194A CN 109280194 A CN109280194 A CN 109280194A CN 201811099916 A CN201811099916 A CN 201811099916A CN 109280194 A CN109280194 A CN 109280194A
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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
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- 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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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/08—Metals
- C08K2003/0806—Silver
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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Abstract
The present invention relates to a kind of preparation methods of antibacterial polylactic acid film, belong to technical field of film preparation.The present invention not only can effectively adsorb organic matter and part inorganic impurity in air, and the polylactic acid film that can also effectively inhibit the growth and breeding of bacterium to make preparation has good antibacterial effect;The present invention uses solution intercalation method by polylactic acid intercalation medical stone powder, it is prepared for that there is good flexibility, the polylactic acid film of hot property and mechanical property, polylactic acid has nontoxic, easy processing, heat stable property, also there is excellent biocompatibility and biodegradable properties, in polylactic acid molecule structure, the hydrolysis of ester bond is one of the major way of polylactic acid degradation, since ester bond is sensitive to alkali, therefore in alkaline solution, the hydrolysis of ester group of polylactic acid generates carboxylate, be conducive to hydrolysis to carry out to positive reaction direction, ester group cleavage caused by the polylactic acid film of preparation mainly hydrolyzes, the acid that degradation process generates may have catalytic action to degradation.
Description
Technical field
The present invention relates to a kind of preparation methods of antibacterial polylactic acid film, belong to technical field of film preparation.
Background technique
With the acceleration of people's life rhythm, improvement of living standard, more and more plastic refuses, especially plastics
Packaging material and foamed plastics finished product, so that white pollution is got worse.Be unable to the plastic garbage of natural degradation, to city,
The different degrees of pollution of the compositions such as rural area, ocean, lake becomes worldwide one big public hazards.Polylactic acid has well due to it
Biocompatibility and biological degradability are increasingly paid attention to by people.And the good mechanical performance of polylactic acid allows to lead to
It crosses various ways and is processed into film, so that polylactic acid film has many excellent properties, many necks can be widely used in
Domain.
Currently, polylactic acid film has its unique advantage as packaging material, it may be said that polylactic acid packaging material can replace
Conventional packaging material is better than for the packaging material of parts of traditional, and at many aspects.Poly-lactic acid material is due to its nontoxicity
With good mechanical performance, it is suitble to the housing material for being processed into various beverages, food, cosmetics of super quality etc. and is pressed into
Transparent fiber, container, eyeglass etc..Also, polylactic acid can be natural fibre blended with other, fabric good permeability, resists
Wrinkle property is strong.There is good toughness in industrial and agricultural production field poly-lactic acid material, be suitble to be processed into the agricultural mulching of high added value;
Also it can be applied in agriculture and forestry make sowing fabric, film, anti-straw bag, the anti-beast evil drop cloth of insect prevention etc.;Also act as soil, desert
Afforest water-keeping material, agriculture chemical slow-release material etc..
Macromolecule flexible packing material brings serious problem of environmental pollution while greatly facilitating people's life,
And widely used packaging material all relies on greatly the non-renewable resources such as petroleum.Therefore, novel biomass source is prepared
Biodegradable films material becomes the hot spot of packaging field research.
Summary of the invention
The technical problems to be solved by the invention: being directed to existing thin-film material non-degradable, burns burial processing and causes sternly
Again the problem of environmental pollution, a kind of preparation method of antibacterial polylactic acid film is provided.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) in mass ratio 1: 10 medical stone powder and tannic acid being mixed, sonic oscillation obtains mixed liquor A, and it is filtered by vacuum, obtains filter residue,
In mass ratio 1: 5 mixes filter residue and mass fraction for 10% silver nitrate solution, after 6~8h of persistent oscillation, obtains mixed liquid B, filters
Precipitating, is washed with deionized 3~5 times, is placed in 100~120 DEG C of baking oven and dries to constant weight, is cooled to room temperature, and grinds
Up to modified medical stone powder;
(2) according to parts by weight, weigh respectively 20~33 parts of polylactic acid, 1~10 part of polycaprolactone, 40~56 parts of chloroforms,
20~26 parts of modified medical stone powders, polylactic acid, polycaprolactone, chloroform are uniformly mixed, and stirring in water bath processing obtains mixed liquor
C is added modified medical stone powder, continues 6~7h of stirring, standing and defoaming is to get polydactyl acid;
(3) according to parts by weight, 30~60 parts of polydactyl acids, 4~10 parts of polyethylene glycol, 10~16 parts of Nanowires are weighed respectively
Dimension element, 20~40 parts of chloroforms, polydactyl acid and polyethylene glycol are mixed, and after 5~10min of ultrasound and are stirred 1~3h, are obtained
Precursor solution mixes nano-cellulose and chloroform, stirs 2~3h, obtains blended liquid, blended liquid is added to presoma
In solution, stir process obtains matrix, and matrix is scraped film process, takes off film after natural drying, and dries extremely in 40~50 DEG C of baking ovens
Constant weight is to get polylactic acid film.
It is 300~350W that sonic oscillation described in step (1), which is in power, 4~5h of sonic oscillation under room temperature.
Medical stone powder described in step (1) crosses 400~500 meshes.
The processing of stirring in water bath described in step (2) is that low whipping speed is 60~100r/min, and temperature is at 40~50 DEG C
30~50min of stirring in water bath.
Stir process described in step (3) is that low whipping speed is 20~30min of stirring under 1000~2000r/min.
It with speed is 10mm/s knifing on a glass that film process is scraped described in step (3), which is by matrix, with a thickness of 50~
60um。
The present invention is compared with other methods, and advantageous effects are:
(1) present invention restores silver using organic reducing method and is attached on medical stone powder, is made and carries silver-colored medical stone powder, carries silver-colored wheat
Meal mountain flour has stronger absorption property and antibacterial action, not only can effectively adsorb organic matter in air and part is inorganic miscellaneous
Matter, can also effectively inhibit the growth and breeding of bacterium, and silver can be in conjunction with phosphide and sulfide on bacterial cell membrane, thus broken
Bad cell permeability of the membrane;Into cell membrane nano silver can in intracellular protein and DNA sulfide or phosphide it is anti-
It answers, the function of desmoenzyme and the duplication transcription of DNA is blocked, so that the polylactic acid film of preparation has good antibacterial effect;
(2) present invention carries out polylactic acid by the way that polyethylene glycol is added using solution intercalation method by polylactic acid intercalation medical stone powder
Plasticization and modification, is prepared for the polylactic acid film with good flexibility, hot property and mechanical property, polylactic acid have it is nontoxic,
Easy processing, heat stable property also have excellent biocompatibility and biodegradable properties, in polylactic acid molecule structure,
The hydrolysis of ester bond is one of the major way of polylactic acid degradation, since ester bond is sensitive to alkali, in alkaline solution, and polylactic acid
Hydrolysis of ester group generate carboxylate, be conducive to hydrolysis to positive reaction direction carry out, the polylactic acid film of preparation is mainly water
Ester group cleavage caused by solving, the acid that degradation process generates may have catalytic action to degradation.
Specific embodiment
In mass ratio 1: 10 mixes medical stone powder and tannic acid, is 300~350W, sonic oscillation 4 under room temperature in power
~5h obtains mixed liquor A, vacuum filtration, obtains filter residue, and in mass ratio 1: 5 mixes filter residue and mass fraction for 10% silver nitrate solution
It closes, after 6~8h of persistent oscillation, obtains mixed liquid B, filter to obtain precipitating, be washed with deionized 3~5 times, be placed in 100~120 DEG C
It dries in baking oven to constant weight, is cooled to room temperature, grind up to modified medical stone powder;According to parts by weight, 20~33 are weighed respectively
Part polylactic acid, 1~10 part of polycaprolactone, 40~56 parts of chloroforms, 20~26 parts of modified medical stone powders, by polylactic acid, gather oneself
Lactone, chloroform be uniformly mixed, low whipping speed be 60~100r/min, temperature be 40~50 DEG C at stirring in water bath 30~
50min obtains mixed liquor C, and modified medical stone powder is added, continues 6~7h of stirring, standing and defoaming is to get polydactyl acid;By weight
Number meter weighs 30~60 parts of polydactyl acids, 4~10 parts of polyethylene glycol, 10~16 parts of nano-celluloses, 20~40 parts respectively
Chloroform mixes polydactyl acid and polyethylene glycol, after 5~10min of ultrasound and stirs 1~3h, obtains precursor solution, will
Nano-cellulose and chloroform mixing, stir 2~3h, obtain blended liquid, blended liquid is added in precursor solution, stirring
Speed is that 20~30min is stirred under 1000~2000r/min, obtains matrix, and matrix is scraped with speed for 10mm/s on a glass
Film takes off film after natural drying, and dries to constant weight in 40~50 DEG C of baking ovens to get polylactic acid film.
Example 1
In mass ratio 1: 10 mixes medical stone powder and tannic acid, is 300W in power, sonic oscillation 4h under room temperature obtains mixed liquor
A, vacuum filtration, obtains filter residue, and filter residue and mass fraction are the mixing of 10% silver nitrate solution by mass ratio 1: 5, after persistent oscillation 6h,
Mixed liquid B is obtained, filters to obtain precipitating, be washed with deionized 3 times, is placed in 100 DEG C of baking oven and dries to constant weight, be cooled to room
Temperature is ground up to modified medical stone powder;According to parts by weight, 20 parts of polylactic acid, 1 part of polycaprolactone, 40 parts of trichlorines are weighed respectively
Methane, 20 parts of modified medical stone powders, polylactic acid, polycaprolactone, chloroform are uniformly mixed, low whipping speed 60r/min,
Temperature is stirring in water bath 30min at 40 DEG C, obtains mixed liquor C, and modified medical stone powder is added, and continues to stir 6h, standing and defoaming to get
Polydactyl acid;According to parts by weight, 30 parts of polydactyl acids, 4 parts of polyethylene glycol, 10 parts of nano-celluloses, 20 are weighed respectively
Part chloroform, polydactyl acid and polyethylene glycol are mixed, and after ultrasonic 5min and are stirred 1h, precursor solution are obtained, by nanometer
Cellulose and chloroform mixing, stir 2h, obtain blended liquid, blended liquid is added in precursor solution, low whipping speed is
20min is stirred under 1000r/min, obtains matrix, with speed is 10mm/s knifing on a glass by matrix, takes off after natural drying
Film, and dry to constant weight in 40 DEG C of baking ovens to get polylactic acid film.
Example 2
In mass ratio 1: 10 mixes medical stone powder and tannic acid, is 325W in power, sonic oscillation 4h under room temperature obtains mixed liquor
A, vacuum filtration, obtains filter residue, and filter residue and mass fraction are the mixing of 10% silver nitrate solution by mass ratio 1: 5, after persistent oscillation 7h,
Mixed liquid B is obtained, filters to obtain precipitating, be washed with deionized 4 times, is placed in 110 DEG C of baking oven and dries to constant weight, be cooled to room
Temperature is ground up to modified medical stone powder;According to parts by weight, 28 parts of polylactic acid, 5 parts of polycaprolactones, 48 parts of trichlorines are weighed respectively
Methane, 23 parts of modified medical stone powders, polylactic acid, polycaprolactone, chloroform are uniformly mixed, low whipping speed 80r/min,
Temperature is stirring in water bath 40min at 45 DEG C, obtains mixed liquor C, and modified medical stone powder is added, and continues to stir 6h, standing and defoaming to get
Polydactyl acid;According to parts by weight, 45 parts of polydactyl acids, 7 parts of polyethylene glycol, 13 parts of nano-celluloses, 30 are weighed respectively
Part chloroform, polydactyl acid and polyethylene glycol are mixed, and after ultrasonic 8min and are stirred 2h, precursor solution are obtained, by nanometer
Cellulose and chloroform mixing, stir 2h, obtain blended liquid, blended liquid is added in precursor solution, low whipping speed is
25min is stirred under 1500r/min, obtains matrix, with speed is 10mm/s knifing on a glass by matrix, takes off after natural drying
Film, and dry to constant weight in 45 DEG C of baking ovens to get polylactic acid film.
Example 3
In mass ratio 1: 10 mixes medical stone powder and tannic acid, is 350W in power, sonic oscillation 5h under room temperature obtains mixed liquor
A, vacuum filtration, obtains filter residue, and filter residue and mass fraction are the mixing of 10% silver nitrate solution by mass ratio 1: 5, after persistent oscillation 8h,
Mixed liquid B is obtained, filters to obtain precipitating, be washed with deionized 5 times, is placed in 120 DEG C of baking oven and dries to constant weight, be cooled to room
Temperature is ground up to modified medical stone powder;According to parts by weight, 33 parts of polylactic acid, 10 parts of polycaprolactones, 56 parts of trichlorines are weighed respectively
Methane, 26 parts of modified medical stone powders, polylactic acid, polycaprolactone, chloroform are uniformly mixed, low whipping speed 100r/
Min, temperature are stirring in water bath 50min at 50 DEG C, obtain mixed liquor C, and modified medical stone powder is added, and continue to stir 7h, standing and defoaming,
Up to polydactyl acid;According to parts by weight, 60 parts of polydactyl acids, 10 parts of polyethylene glycol, 16 parts of nanofibers are weighed respectively
Element, 40 parts of chloroforms mix polydactyl acid and polyethylene glycol, after ultrasonic 10min and stir 3h, obtain precursor solution,
Nano-cellulose and chloroform are mixed, 3h is stirred, obtains blended liquid, blended liquid is added in precursor solution, stirring
Speed is to stir 30min under 2000r/min, obtains matrix, with speed is 10mm/s knifing on a glass, naturally dry by matrix
After take off film, and in 50 DEG C of baking ovens dry to constant weight to get polylactic acid film.
Reference examples: the polylactic acid film of Dongguan company production.
The polylactic acid film that example and reference examples are prepared is detected, specific detection is as follows:
Mass loss rate: the palliating degradation degree of polylactic acid film is investigated using polylactic acid film mass loss rate (%).Polylactic acid film
Mass loss rate is calculated according to formula.
Tensile property: standard tensile specimen prepared by establishing criteria GB/T1040.2, in Shanghai, skill instrument science and technology of inclining has
The tensile property of test polylactic acid film degradation front and back, rate of extension on the QJ210A-1000N universal testing machine of limit company production
For 2mm/min.5 samples of every group of test, acquire average value.
Specific test result such as table 1.
1 performance characterization contrast table of table
As shown in Table 1, polylactic acid film prepared by the present invention has good tensile property and degradability.
Claims (6)
1. a kind of preparation method of antibacterial polylactic acid film, it is characterised in that specific steps are as follows:
(1) in mass ratio 1: 10 medical stone powder and tannic acid being mixed, sonic oscillation obtains mixed liquor A, and it is filtered by vacuum, obtains filter residue,
In mass ratio 1: 5 mixes filter residue and mass fraction for 10% silver nitrate solution, after 6~8h of persistent oscillation, obtains mixed liquid B, filters
Precipitating, is washed with deionized 3~5 times, is placed in 100~120 DEG C of baking oven and dries to constant weight, is cooled to room temperature, and grinds
Up to modified medical stone powder;
(2) according to parts by weight, weigh respectively 20~33 parts of polylactic acid, 1~10 part of polycaprolactone, 40~56 parts of chloroforms,
20~26 parts of modified medical stone powders, polylactic acid, polycaprolactone, chloroform are uniformly mixed, and stirring in water bath processing obtains mixed liquor
C is added modified medical stone powder, continues 6~7h of stirring, standing and defoaming is to get polydactyl acid;
(3) according to parts by weight, 30~60 parts of polydactyl acids, 4~10 parts of polyethylene glycol, 10~16 parts of Nanowires are weighed respectively
Dimension element, 20~40 parts of chloroforms, polydactyl acid and polyethylene glycol are mixed, and after 5~10min of ultrasound and are stirred 1~3h, are obtained
Precursor solution mixes nano-cellulose and chloroform, stirs 2~3h, obtains blended liquid, blended liquid is added to presoma
In solution, stir process obtains matrix, and matrix is scraped film process, takes off film after natural drying, and dries extremely in 40~50 DEG C of baking ovens
Constant weight is to get polylactic acid film.
2. a kind of preparation method of antibacterial polylactic acid film according to claim 1, it is characterised in that: step (1) is described
Sonic oscillation be in power be 300~350W, 4~5h of sonic oscillation under room temperature.
3. a kind of preparation method of antibacterial polylactic acid film according to claim 1, it is characterised in that: step (1) is described
Medical stone powder cross 400~500 meshes.
4. a kind of preparation method of antibacterial polylactic acid film according to claim 1, it is characterised in that: step (2) is described
Stirring in water bath processing be low whipping speed be 60~100r/min, temperature is 30~50min of stirring in water bath at 40~50 DEG C.
5. a kind of preparation method of antibacterial polylactic acid film according to claim 1, it is characterised in that: step (3) is described
Stir process be low whipping speed be under 1000~2000r/min stirring 20~30min.
6. a kind of preparation method of antibacterial polylactic acid film according to claim 1, it is characterised in that: step (3) is described
Film process of scraping be by matrix with speed be 10mm/s knifing on a glass, with a thickness of 50~60 μm.
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CN113045216A (en) * | 2021-03-02 | 2021-06-29 | 胡敏文 | Self-cleaning coated glass for curtain wall and preparation method thereof |
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CN111058150A (en) * | 2019-12-26 | 2020-04-24 | 刘学谷 | Preparation method of copper ammonia fiber antibacterial blended fabric |
CN113045216A (en) * | 2021-03-02 | 2021-06-29 | 胡敏文 | Self-cleaning coated glass for curtain wall and preparation method thereof |
CN114835407A (en) * | 2021-03-02 | 2022-08-02 | 胡敏文 | Self-cleaning coated glass for curtain wall |
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Application publication date: 20190129 |