CN104830001B - Preparation method of transparent polyvinyl alcohol (PVA) composite aquagel film - Google Patents
Preparation method of transparent polyvinyl alcohol (PVA) composite aquagel film Download PDFInfo
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- CN104830001B CN104830001B CN201510260049.5A CN201510260049A CN104830001B CN 104830001 B CN104830001 B CN 104830001B CN 201510260049 A CN201510260049 A CN 201510260049A CN 104830001 B CN104830001 B CN 104830001B
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Abstract
The invention discloses a preparation method of a transparent polyvinyl alcohol (PVA) composite aquagel film. The technical scheme is as follows: the method comprises the following steps: preparing a PVA solution, and stirring at 75-95 DEG C until the solid is completely dissolved; adding 10ml of PVA solution into another reaction bulb, adding certain amounts of SDBS (sodium dodecyl benzene sulfonate) and KH550, and dissolving by stirring; adding a certain amount of nano TiO2 into the reaction bulb, and carrying out ultrasonic dispersion treatment; adding the nano TiO2 mixed solution subjected to ultrasonic dispersion treatment into the residual PVA solution, and accelerating stirring uniformly; standing at 75-95 DEG C, and removing bubbles with ultrasonic treatment; coating a film with a coating applicator or preparing the film by other methods, sealing the coated film, and repeating freezing and defreezing; cleaning and immersing the PVA composite film with distilled water; and carrying out vacuum drying to obtain the product. The product prepared by the method has the advantages of favorable mechanical properties, water retention, bacterial resistance, ultraviolet resistance, slow drug release and the like.
Description
Technical field
The invention belongs to polymeric material field, and in particular to a kind of using nano-titanium dioxide modified transparent polyethylene
The preparation method of alcohol compound water congealing glued membrane.
Background technology
Macromolecule hydrogel is that a class can be water-swellable but the water-fast polymer with three-dimensional net structure.Its energy
The sensitivity response for stimulating to external world is realized enough by the swelling of volume or contraction.Polyvinyl alcohol (PVA) hydrogel is current
One of hydrogel being most widely used.PVA not only possesses the water suction of general hydrogel, water conservation, slow release and stimulates to external world
The performances such as sensitivity response, due also to its special nature and there is low toxicity, bio-compatible and the advantageous property such as transparent, in biological doctor
The fields such as medicine, food industry have a wide range of applications.
With the fast development and the continuous improvement of people's living standard of modern society, hydrogel is in mechanical strength, water conservation
The defect of the aspects such as property, pliability increasingly restricts which and is widely applied.High-performance novel macromolecule hydrogel is prepared and is increasingly received
To concern.Nanoparticle has biologically inert and chemical stability, and inorganic nano-particle is combined with hydrogel, carries out blending and changes
Property, the combination property of hydrogel can be improved.At present Nanometer composite hydrogel be it is of greatest concern in modified hydrogel because this
Kind hydrogel is very similar with the structure of biological tissue, and preparation process is relatively simple, and method has universality, answers with good
Use prospect.
Nano titanium oxide (TiO2) used as conventional inorganic nano-particle, inorganic UV reflective agent, it has higher
Refractive index, plays refraction and reflection to ultraviolet luminous energy；Work as nano-TiO2When running into antibacterial, the cell of energy attack antibacterial makes
Its intracellular Organic substance decomposes, and is gone out except antibacterial with this, and is allowed to decompose.Add nano-TiO in PVA hydrogels2Powder body, energy
PVA hydrogels are made not only to have there is hydrogel water conservation, the performance of slow release but also there is antibacterial, the function of anti-ultraviolet, while inorganic nano
Particle adds organic basis material, additionally it is possible to improve its mechanical property.Thus, this problem studies emphatically nano-TiO2Modified PVA
High molecular aquagel membrane preparation method, the novel high-performance aquagel membrane material good to obtaining a kind of combination property.
The content of the invention
It is an object of the invention to provide a kind of have many performances and the mechanics such as water conservation, antibacterial, uvioresistant, medicament slow release
The preparation method of the high-performance polyvinyl alcohol composite hydrogel film of better performances.
The purpose of the present invention is by the following technical solutions realizing：The transparent polyethylene alcohol compound water congealing glued membrane
Preparation method, comprises the steps：
(1) prepare weight/mass percentage composition be 5～20% 30～50ml of poly-vinyl alcohol solution, its degree of polymerization be 1600～
2400, to being completely dissolved more than stirring and dissolving 4h at a temperature of 75～95 DEG C；
(2) measure poly-vinyl alcohol solution i.e. PVA solution prepared by 10ml steps (1) to be added in another reaction bulb, add
With respect to the dodecylbenzene sodium sulfonate that PVA mass contents are 0.5% i.e. SDBS, it is 10%～12% with respect to PVA mass contents
Silane coupler is KH550, stirring and dissolving；Add the nano-TiO that relative PVA mass contents are 0.5%～30%2To the reaction
In bottle, ultrasonic disperse processes 30min；By the nano-TiO of the ultrasound wave decentralized processing2Mixed solution is slowly added into step
(1) in reaction bulb in the remaining poly-vinyl alcohol solution being completely dissolved, accelerate stirring so as to uniform to mix；75～95 DEG C of temperature
10min is stood, and then bubble removing is removed with ultrasonic Treatment；
(3) step (2) is gone product spreader film or the additive method masking of bubble removing, film phonograph seal freezing will be applied,
Take out after 12h is freezed at a temperature of -18 DEG C～-22 DEG C, thaw under room temperature 4h, the above-mentioned freezing of repetition, operation more than 3 times of thawing；
Film is taken, by PVA composite membranes distilled water cleaning and dipping, to remove uncrosslinked monomer or polymer；Vacuum drying PVA Compound Waters
Gel film, baking temperature are 25～55 DEG C, obtained film is put in hermetic bag and is preserved.
The inventive method is simple, and obtained composite membrane is not only cheap, is easy to get, convenient, practical, and have water conservation,
Many performances such as antibacterial, uvioresistant, medicament slow release, bio-compatible, printing opacity, can be used as biology, medical science and material protection etc. numerous
Field.
Description of the drawings
Fig. 1 is the SEM image of polyvinyl alcohol composite hydrogel film prepared by the embodiment of the present invention 1.
Fig. 2 is that the present invention prepares difference TiO2The polyvinyl alcohol composite hydrogel film of content is to escherichia coli antibacterial effect
Figure；In figure, A is to be not added with TiO2, B is TiO2It is TiO that content is 0.5%, C2It is TiO that content is 1.0%, D2Content
It is TiO for 2.0%, E2It is TiO that content is 5.0%, F2Content is 7.5%.
Fig. 3 is PVA aquagel membranes and PVA compound water congealing glued membrane ultraviolet permeability curve charts；In figure, A curves are PVA water-settings
Glue, B curves are 0.5%TiO2/ PVA hydrogels, C curve is 0.75%TiO2/ PVA hydrogels, D curves are 1.0%
TiO2/ PVA hydrogels, E curves are 3%TiO2/ PVA hydrogels, F curves are 7.5%TiO2/ PVA hydrogels, G curves
It is 30%TiO2/ PVA hydrogels.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment 1：
2g polyvinyl alcohol (degree of polymerization 2350 ± 50) is weighed, distilled water 30ml is measured, in adding there-necked flask, in 95 DEG C of temperature
Lower stirring simultaneously dissolves 4h.Measure 10ml PVA solutions from there-necked flask to be added in round-bottomed flask, add 0.01g SDBS, 0.25
Milliliter KH550, stirring and dissolving weigh 0.02g nano-TiOs with electronic balance2It is added in round-bottomed flask, ultrasonic disperse process
30min.By the nano-TiO of ultrasonic disperse process2Mixed solution is slowly added into remaining polyethylene in the there-necked flask of dissolving 4h
In alcoholic solution, accelerate stirring so as to uniform to mix.At a temperature of 90 DEG C, insulation stands 10min, then goes degasification with ultrasonic Treatment
Bubble.By the above-mentioned product for removing bubble removing with spreader film, the glass plate after film is put into into sealing freezing in box.At -18 DEG C
Take out to put from refrigerator after lower freezing 12h and thaw at room temperature 4h, the above-mentioned freeze-thaw of repetition is operated 5 times.Film is taken, by composite membrane
Distilled water cleaning and dipping is used, to remove uncrosslinked monomer or polymer.Vacuum drying PVA compound water congealing glued membranes, baking temperature
For 45 DEG C.Film is put in hermetic bag and is preserved.Obtained high-performance polyvinyl alcohol composite hydrogel film and pure PVA hydrogels
Film is compared, and tensile strength improves 35%, and uvioresistant performance improves 20%, and antibiotic property improves 38%, while compound water congealing glued membrane
Light transmittance is up to 85% and has good medicament slow release performance.The SEM image of polyvinyl alcohol composite hydrogel film manufactured in the present embodiment
As shown in Figure 1；Polyvinyl alcohol composite hydrogel film manufactured in the present embodiment is to shown in C in escherichia coli antibacterial effect figure such as Fig. 2；
In polyvinyl alcohol composite hydrogel film ultraviolet permeability curve chart such as Fig. 3 manufactured in the present embodiment shown in D curves.
Embodiment 2：
2g polyvinyl alcohol (degree of polymerization 2350 ± 50) is weighed, distilled water 30ml is measured, in adding there-necked flask, in 95 DEG C of temperature
Lower stirring simultaneously dissolves 4h.Measure from there-necked flask in 10ml PVA solutions addition round-bottomed flask, add 0.01g SDBS, 0.25 Bo
KH550 is risen, stirring and dissolving weighs 0.03g nano-TiOs with electronic balance2It is added in round-bottomed flask, ultrasound wave decentralized processing
30min.By the nano-TiO of ultrasound wave decentralized processing2Mixed solution is slowly added into remaining poly- second in the there-necked flask of dissolving 4h
In enolate solution, accelerate stirring so as to uniform to mix.At a temperature of 90 DEG C, insulation stands 10min, is subsequently adding 0.01g salicylic acid,
Ultrasonic disperse 30min, makes salicylic acid be uniformly dispersed.By the above-mentioned product for removing bubble removing with spreader film, by the glass after film
Glass plate is sealed in being put into box, is freezed in being then placed in refrigerator, puts from refrigerator taking-up solve at -18 DEG C after freezing 12h at room temperature
Freeze 4h, the above-mentioned freezing solution of repetition-jelly is operated 5 times.Film is taken, by composite membrane distilled water cleaning and dipping, to remove uncrosslinked list
Body or polymer.Vacuum drying PVA compound water congealing glued membranes, baking temperature are 45 DEG C.Film is put in hermetic bag and is preserved.It is obtained
Compared with pure PVA aquagel membranes, tensile strength improves 24% to high-performance polyvinyl alcohol composite hydrogel film, in 280nm
Between～320nm, uvioresistant performance improves 80%, and between 340nm～400nm, uvioresistant performance improves 20%, and antibiotic property is improved
48%, while compound water congealing glued membrane light transmittance is up to 80%, and have good medicament slow release performance.
Embodiment 3：
2g polyvinyl alcohol (degree of polymerization 1750 ± 50) is weighed, distilled water 30mL is measured, in adding there-necked flask, heating in water bath exists
Stir at a temperature of 90 DEG C and dissolve 4h.Measure from there-necked flask in 10ml deionized waters addition round-bottomed flask, add 0.01g
SDBS, 0.25 milliliter KH550 stirring and dissolving, weigh 0.02g nano-TiOs with electronic balance2It is added in round-bottomed flask, ultrasound wave
Decentralized processing 30min.By the nano-TiO of ultrasound wave decentralized processing2Mixed solution is remained in being slowly added into the there-necked flask of dissolving 4h
In remaining poly-vinyl alcohol solution, accelerate stirring so as to uniform to mix.At a temperature of 90 DEG C, insulation stands 10min, then uses ultrasound wave
Bubble removing is removed in process.By the above-mentioned product for removing bubble removing with spreader film, the glass plate after film is put in box and is sealed, so
After be put in refrigerator and freeze, take out to put from refrigerator after freezing 12h at -18 DEG C and thaw at room temperature 4h, the above-mentioned freezing-solution of repetition
Freeze operation 4 times.Film is taken, by composite membrane distilled water cleaning and dipping, to remove uncrosslinked monomer or polymer.Vacuum drying
PVA compound water congealing glued membranes, baking temperature are 45 DEG C.Film is put in hermetic bag and is preserved.Obtained compound water congealing glued membrane and pure PVA
Aquagel membrane is compared, and tensile strength improves 52.4%, and uvioresistant performance improves 65%, and antibiotic property improves 35%, while compound
Aquagel membrane light transmittance is up to 87%, and has good medicament slow release performance.
Composite aquogel 0.024～0.045mm of thickness used in above-described embodiment；Nano-TiO2Self-control, particle diameter 100nm are left
It is right；Antibiotic property experimental strain is escherichia coli, staphylococcus aureuses or aspergillus niger.
Claims (1)
1. a kind of preparation method of transparent polyethylene alcohol compound water congealing glued membrane, it is characterised in that comprise the steps：
(1) 30～50ml of poly-vinyl alcohol solution that weight/mass percentage composition is 5～20% is prepared, its degree of polymerization is 1600～2400,
To being completely dissolved more than stirring and dissolving 4h at a temperature of 75～95 DEG C；
(2) measure poly-vinyl alcohol solution i.e. PVA solution prepared by 10ml steps (1) to be added in another reaction bulb, add relative
PVA mass contents are 0.5% dodecylbenzene sodium sulfonate i.e. SDBS, with respect to the silane that PVA mass contents are 10%～12%
Coupling agent is KH550, stirring and dissolving；Add the nano-TiO that relative PVA mass contents are 0.5%～30%2To the reaction bulb
In, ultrasonic disperse processes 30min；By the nano-TiO of the ultrasound wave decentralized processing2Mixed solution is slowly added into step (1)
In reaction bulb in the remaining poly-vinyl alcohol solution being completely dissolved, accelerate stirring so as to uniform to mix；75～95 DEG C of temperature stand
10min, then removes bubble removing with ultrasonic Treatment；
(3) step (2) is gone product spreader film or the additive method masking of bubble removing, film phonograph seal freezing will be applied, -18
DEG C～-22 DEG C at a temperature of freeze 12h after take out, thaw under room temperature 4h, the above-mentioned freezing of repetition, operation more than 3 times of thawing；Take film,
By PVA composite membranes distilled water cleaning and dipping, to remove uncrosslinked monomer or polymer；Vacuum drying PVA composite aquogels
Film, baking temperature are 25～55 DEG C, obtained film is put in hermetic bag and is preserved.
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| CN107082895A (en) * | 2017-04-27 | 2017-08-22 | 上海交通大学 | The preparation method of degradable nano antibacterial film |
| CN109824916A (en) * | 2019-02-19 | 2019-05-31 | 湖南工程学院 | A kind of composite hydrogel, compound water congealing glue film and its preparation method and application |
| CN109876741A (en) * | 2019-03-19 | 2019-06-14 | 北京中船经济技术开发有限公司 | A kind of tourmaline and photocatalytic semiconductor composite hydrogel and its preparation method and application |
| CN110359292B (en) * | 2019-07-12 | 2021-11-30 | 陕西科技大学 | Flexible, breathable and wear-resistant leather and preparation method thereof |
| CN112113498B (en) * | 2020-09-14 | 2021-09-28 | 山西大学 | Preparation method of high-sensitivity piezoresistive strain sensor |
| CN113457218B (en) * | 2021-07-13 | 2022-12-27 | 扬州大学 | Oil-water separation material based on electrostatic spinning/PVA composite hydrogel and preparation method thereof |
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| CN102504454A (en) * | 2011-11-04 | 2012-06-20 | 郝喜海 | Ultraviolet resistant polyvinyl alcohol fruit bag film preparation formula and technology thereof |
| CN103570065A (en) * | 2013-10-29 | 2014-02-12 | 台州学院 | Dual-template preparation method of mesoporous TiO2 sphere |
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| US3445275A (en) * | 1965-05-25 | 1969-05-20 | Anchor Hocking Glass Corp | Glass container coated with a lubricating film comprising carnauba wax and polyvinyl alcohol |
| JPS61197663A (en) * | 1985-02-26 | 1986-09-01 | Nippon Synthetic Chem Ind Co Ltd:The | Adhesive for building material |
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| CN102504454A (en) * | 2011-11-04 | 2012-06-20 | 郝喜海 | Ultraviolet resistant polyvinyl alcohol fruit bag film preparation formula and technology thereof |
| CN103570065A (en) * | 2013-10-29 | 2014-02-12 | 台州学院 | Dual-template preparation method of mesoporous TiO2 sphere |
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