CN104830001A - 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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- CN104830001A CN104830001A CN201510260049.5A CN201510260049A CN104830001A CN 104830001 A CN104830001 A CN 104830001A CN 201510260049 A CN201510260049 A CN 201510260049A CN 104830001 A CN104830001 A CN 104830001A
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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, be specifically related to a kind of preparation method utilizing nano-titanium dioxide modified transparent polyethylene alcohol compound water congealing glued membrane.
Background technology
Macromolecule hydrogel is that a class can be water-swellable but the water-fast polymkeric substance with three-dimensional net structure.It by the swelling of volume or can shrink the sensitivity response realizing stimulating to external world.Polyvinyl alcohol (PVA) hydrogel is one of hydrogel be most widely used at present.PVA not only possesses the performances such as the water suction of general hydrogel, water conservation, slowly-releasing and the sensitivity response that stimulates to external world, also there is due to its special property low toxicity, physiologically acceptable and the advantageous property such as transparent, in biological medicine, the fields such as foodstuffs industry have a wide range of applications.
Along with the fast development of modern society and improving constantly of people's living standard, the defect of hydrogel in mechanical strength, water-retentivity, snappiness etc. day by day restricts it and applies widely.The preparation of high-performance novel macromolecule hydrogel more and more receives publicity.Nanoparticle has biologically inert and chemical stability, by inorganic nano-particle and hydrogel compound, carries out blending and modifying, can improve the over-all properties of hydrogel.Current Nanometer composite hydrogel is of greatest concern in modified water gel, because the structure of this hydrogel and biological tissue is very similar, preparation process is comparatively simple, and method has ubiquity, has good application prospect.
Nano titanium oxide (TiO
2) as conventional inorganic nano-particle, inorganic UV tamper, it has higher specific refractory power, plays refraction and reflex action to ultraviolet luminous energy; Work as nano-TiO
2when running into bacterium, the cell of energy attack bacterium, makes its intracellular organic substance decomposing, goes out except bacterium with this, and makes it to decompose.Nano-TiO is added in PVA hydrogel
2powder, can make PVA hydrogel not only had hydrogel water conservation, slowly-releasing performance but also there is function that is antibacterial, antiultraviolet, inorganic nano-particle adds organic basis material simultaneously, can also improve its mechanical property.Thus, this problem studies nano-TiO emphatically
2modified PVA high molecular aquagel membrane preparation method, to obtaining the good novel high-performance aquagel membrane material of a kind of over-all properties.
Summary of the invention
The object of the present invention is to provide and a kind of there is water conservation, antibacterial, many performances such as uvioresistant, medicament slow release and the preparation method of mechanical property good high-performance transparent polyethylene alcohol compound water congealing glued membrane.
The object of the invention is to realize by the following technical solutions: the preparation method of this transparent polyethylene alcohol compound water congealing glued membrane, comprises the steps:
(1) prepare polyvinyl alcohol solution 30 ~ 50ml that mass percentage is 5 ~ 20%, its polymerization degree is 1600 ~ 2400, and at 75 ~ 95 DEG C of temperature, more than stirring and dissolving 4h is to dissolving completely;
(2) polyvinyl alcohol solution prepared by 10ml step (1) is measured and PVA solution joins in another reaction flask, add Sodium dodecylbenzene sulfonate and SDBS that relative PVA mass content is 0.5%, relative PVA mass content is silane coupling agent and the KH550 of 10% ~ 12%, stirring and dissolving; Adding relative PVA mass content is the nano-TiO of 0.5% ~ 30%
2to in this reaction flask, ultrasonic disperse process 30min; By the nano-TiO of described ultrasonic wave dispersion treatment
2mixing solutions slowly joins in step (1) reaction flask in remaining consoluet polyvinyl alcohol solution, accelerates to stir, and makes its Homogeneous phase mixing; 75 ~ 95 DEG C of temperature leave standstill 10min, then remove bubble by ultrasonication;
(3) step (2) is removed product spreader film or the additive method masking of bubble, film phonograph seal will be coated with freezing, take out after freezing 12h at-18 DEG C ~-22 DEG C temperature, thawed at room temperature 4h, repeat above-mentioned freezing, operation more than 3 times of thawing; Get film, by PVA composite membrane distilled water cleaning and dipping, to remove uncrosslinked monomer or polymkeric substance; Vacuum-drying PVA compound water congealing glued membrane, drying temperature is 25 ~ 55 DEG C, obtained film is put into sealing bag and preserves.
The inventive method is simple, and obtained composite membrane is not only cheap, is easy to get, convenient, practical, and has many performances such as water conservation, antibacterial, uvioresistant, medicament slow release, physiologically acceptable, printing opacity, can be used as the various fields such as biology, medical science and material protection.
Accompanying drawing explanation
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 different Ti O
2the polyvinyl alcohol composite hydrogel film of content is to intestinal bacteria antibacterial effect figure; In figure, A does not add TiO
2, B is TiO
2content is 0.5%, and C is TiO
2content is 1.0%, and D is TiO
2content is 2.0%, and E is TiO
2content is 5.0%, and F is TiO
2content is 7.5%.
Fig. 3 is PVA aquagel membrane and PVA compound water congealing glued membrane ultraviolet permeability graphic representation; In figure, A curve is PVA hydrogel, and B curve is 0.5%TiO
2/ PVA hydrogel, C curve is 0.75%TiO
2/ PVA hydrogel, D curve is 1.0%TiO
2/ PVA hydrogel, E curve is 3%TiO
2/ PVA hydrogel, F curve is 7.5%TiO
2/ PVA hydrogel, G curve is 30%TiO
2/ PVA hydrogel.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
Take 2g polyvinyl alcohol (polymerization degree 2350 ± 50), measure distilled water 30ml, add in there-necked flask, stir at 95 DEG C of temperature and dissolve 4h.From there-necked flask, measure 10ml PVA solution joins in round-bottomed flask, and add 0.01g SDBS, 0.25 milliliter KH550, stirring and dissolving, takes 0.02g nano-TiO with electronic balance
2join in round-bottomed flask, ultrasonic disperse process 30min.By the nano-TiO of ultrasonic disperse process
2mixing solutions slowly joins in the there-necked flask dissolving 4h in remaining polyvinyl alcohol solution, accelerates to stir, makes its Homogeneous phase mixing.At 90 DEG C of temperature, insulation leaves standstill 10min, then removes bubble by ultrasonication.By the product of above-mentioned removal bubble with spreader film, the sheet glass after film is put into box and seals freezing.Take out from refrigerator after freezing 12h at-18 DEG C and be placed in thawed at room temperature 4h, repeat above-mentioned freeze-thaw and operate 5 times.Get film, composite membrane is used distilled water cleaning and dipping, to remove uncrosslinked monomer or polymkeric substance.Vacuum-drying PVA compound water congealing glued membrane, drying temperature is 45 DEG C.Film is put into sealing bag preserve.Obtained high-performance transparent polyethylene alcohol compound water congealing glued membrane is compared with pure PVA aquagel membrane, tensile strength improves 35%, uvioresistant performance improves 20%, and germ resistance raising 38%, simultaneously compound water congealing glued membrane transmittance reach 85% and the good medicament slow release performance of tool.The SEM image of polyvinyl alcohol composite hydrogel film prepared by the present embodiment as shown in Figure 1; Polyvinyl alcohol composite hydrogel film prepared by the present embodiment to intestinal bacteria antibacterial effect figure as shown in C in Fig. 2; Polyvinyl alcohol composite hydrogel film ultraviolet permeability graphic representation prepared by the present embodiment is as shown in D curve in Fig. 3.
Embodiment 2:
Take 2g polyvinyl alcohol (polymerization degree 2350 ± 50), measure distilled water 30ml, add in there-necked flask, stir at 95 DEG C of temperature and dissolve 4h.From there-necked flask, measure 10ml PVA solution adds in round-bottomed flask, and add 0.01g SDBS, 0.25 milliliter KH550, stirring and dissolving, takes 0.03g nano-TiO with electronic balance
2join in round-bottomed flask, ultrasonic wave dispersion treatment 30min.By the nano-TiO of ultrasonic wave dispersion treatment
2mixing solutions slowly joins in the there-necked flask dissolving 4h in remaining polyvinyl alcohol solution, accelerates to stir, makes its Homogeneous phase mixing.At 90 DEG C of temperature, insulation leaves standstill 10min, then adds 0.01g Whitfield's ointment, ultrasonic disperse 30min, Whitfield's ointment is uniformly dispersed.By the product of above-mentioned removal bubble with spreader film, the sheet glass after film is put into box and seals, then put into refrigerator and cooled and freeze, take out from refrigerator after freezing 12h at-18 DEG C and be placed in thawed at room temperature 4h, repeat above-mentioned freezing solution-freeze operation 5 times.Get film, composite membrane is used distilled water cleaning and dipping, to remove uncrosslinked monomer or polymkeric substance.Vacuum-drying PVA compound water congealing glued membrane, drying temperature is 45 DEG C.Film is put into sealing bag preserve.Obtained high-performance transparent polyethylene alcohol compound water congealing glued membrane is compared with pure PVA aquagel membrane, tensile strength improves 24%, between 280nm ~ 320nm, uvioresistant performance improves 80%, between 340nm ~ 400nm, uvioresistant performance improves 20%, germ resistance improves 48%, compound water congealing glued membrane transmittance reaches 80% simultaneously, and the good medicament slow release performance of tool.
Embodiment 3:
Take 2g polyvinyl alcohol (polymerization degree 1750 ± 50), measure distilled water 30mL, add in there-necked flask, heating in water bath stirs and dissolves 4h at 90 DEG C of temperature.From there-necked flask, measure 10ml deionized water adds in round-bottomed flask, adds 0.01g SDBS, 0.25 milliliter KH550 stirring and dissolving, takes 0.02g nano-TiO with electronic balance
2join in round-bottomed flask, ultrasonic wave dispersion treatment 30min.By the nano-TiO of ultrasonic wave dispersion treatment
2mixing solutions slowly joins in the there-necked flask dissolving 4h in remaining polyvinyl alcohol solution, accelerates to stir, makes its Homogeneous phase mixing.At 90 DEG C of temperature, insulation leaves standstill 10min, then removes bubble by ultrasonication.By the product of above-mentioned removal bubble with spreader film, the sheet glass after film is put into box and seals, then put into refrigerator and cooled and freeze, take out from refrigerator after freezing 12h at-18 DEG C and be placed in thawed at room temperature 4h, repeat above-mentioned freeze-thaw and operate 4 times.Get film, composite membrane is used distilled water cleaning and dipping, to remove uncrosslinked monomer or polymkeric substance.Vacuum-drying PVA compound water congealing glued membrane, drying temperature is 45 DEG C.Film is put into sealing bag preserve.Obtained compound water congealing glued membrane is compared with pure PVA aquagel membrane, and tensile strength improves 52.4%, and uvioresistant performance improves 65%, and germ resistance improves 35%, and compound water congealing glued membrane transmittance reaches 87% simultaneously, and the good medicament slow release performance of tool.
Composite aquogel thickness used 0.024 ~ 0.045mm in above-described embodiment; Nano-TiO
2self-control, particle diameter about 100nm; Germ resistance experimental strain is intestinal bacteria, streptococcus aureus or aspergillus niger.
Claims (1)
1. a preparation method for transparent polyethylene alcohol compound water congealing glued membrane, is characterized in that comprising the steps:
(1) prepare polyvinyl alcohol solution 30 ~ 50ml that mass percentage is 5 ~ 20%, its polymerization degree is 1600 ~ 2400, and at 75 ~ 95 DEG C of temperature, more than stirring and dissolving 4h is to dissolving completely;
(2) polyvinyl alcohol solution prepared by 10ml step (1) is measured and PVA solution joins in another reaction flask, add Sodium dodecylbenzene sulfonate and SDBS that relative PVA mass content is 0.5%, relative PVA mass content is silane coupling agent and the KH550 of 10% ~ 12%, stirring and dissolving; Adding relative PVA mass content is the nano-TiO of 0.5% ~ 30%
2to in this reaction flask, ultrasonic disperse process 30min; By the nano-TiO of described ultrasonic wave dispersion treatment
2mixing solutions slowly joins in step (1) reaction flask in remaining consoluet polyvinyl alcohol solution, accelerates to stir, and makes its Homogeneous phase mixing; 75 ~ 95 DEG C of temperature leave standstill 10min, then remove bubble by ultrasonication;
(3) step (2) is removed product spreader film or the additive method masking of bubble, film phonograph seal will be coated with freezing, take out after freezing 12h at-18 DEG C ~-22 DEG C temperature, thawed at room temperature 4h, repeat above-mentioned freezing, operation more than 3 times of thawing; Get film, by PVA composite membrane distilled water cleaning and dipping, to remove uncrosslinked monomer or polymkeric substance; Vacuum-drying PVA compound water congealing glued membrane, drying temperature is 25 ~ 55 DEG C, obtained film is put into sealing bag and preserves.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110359292A (en) * | 2019-07-12 | 2019-10-22 | 陕西科技大学 | A kind of flexible, ventilative and wearable leather coating and preparation method thereof |
| CN112113498A (en) * | 2020-09-14 | 2020-12-22 | 山西大学 | Preparation method of high-sensitivity piezoresistive strain sensor |
| CN113457218A (en) * | 2021-07-13 | 2021-10-01 | 扬州大学 | Oil-water separation material based on electrostatic spinning/PVA composite hydrogel and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110359292A (en) * | 2019-07-12 | 2019-10-22 | 陕西科技大学 | A kind of flexible, ventilative and wearable leather coating and preparation method thereof |
| CN112113498A (en) * | 2020-09-14 | 2020-12-22 | 山西大学 | Preparation method of high-sensitivity piezoresistive strain sensor |
| CN112113498B (en) * | 2020-09-14 | 2021-09-28 | 山西大学 | Preparation method of high-sensitivity piezoresistive strain sensor |
| CN113457218A (en) * | 2021-07-13 | 2021-10-01 | 扬州大学 | Oil-water separation material based on electrostatic spinning/PVA composite hydrogel and preparation method thereof |
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| CN104830001B (en) | 2017-03-22 |
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