CN102391738A - Silver ion-containing polyvinyl alcohol-based nano composite antibacterial film material and preparation method thereof - Google Patents
Silver ion-containing polyvinyl alcohol-based nano composite antibacterial film material and preparation method thereof Download PDFInfo
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- CN102391738A CN102391738A CN2011102792001A CN201110279200A CN102391738A CN 102391738 A CN102391738 A CN 102391738A CN 2011102792001 A CN2011102792001 A CN 2011102792001A CN 201110279200 A CN201110279200 A CN 201110279200A CN 102391738 A CN102391738 A CN 102391738A
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Abstract
The invention relates to a method for preparing a silver ion-containing polyvinyl alcohol-based nano composite antibacterial film material. The method is characterized by comprising the following steps of: soaking 1 to 10 weight parts of polyvinyl alcohol in water for more than 2-4 hours to make the polyvinyl alcohol fully absorb water and swell, thoroughly dissolving a polyvinyl alcohol solution at the temperature of between 85 and 95DEG C, adding stearic acid dissolved by a solvent, magnetically stirring at constant temperature of between 85 and 95DEG C for 5 minutes, adding a nanomaterial silicon dioxide, magnetically stirring at the constant temperature of between 85 and 95DEG C for 15 minutes, and performing ultrasonic treatment; coating the solution on a smooth glass plate, putting into a fume cupboard, evaporating the solution at room temperature for 48 to 72 hours, allowing a film to be naturally peeled, soaking the film in 1 to 3 weight percent sodium hydroxide for 1 to 2 hours, removing the residual solvent, repeatedly washing with distilled water until neutrality, and naturally drying to obtain a polyvinyl alcohol-based nano composite film material; and immersing the film in 30 to 70ml of 0.1 to 0.7 mol/L silver nitrate solution, stirring for 2 to 6 hours, cleaning with deionized water to remove residual silver ions, and drying at room temperature to obtain the silver ion-containing polyvinyl alcohol-based nano composite antibacterial film material.
Description
Technical field
The invention belongs to the preparation field of polymer composite, be specifically related to a kind of PVA-based nanocomposite coating preparation methods, PVA-based nano composite antibacterial class coating material of particularly a kind of argentiferous ionic and preparation method thereof.
Background technology
Along with people's when utilizing the mikrobe helpfulness, is also very watched out for its hazardness as pathogenic bacteria to the research of environmental microorganism and improving constantly of the level of understanding.It is reported that the whole world dead 5,200 ten thousand people of nineteen ninety-five wherein because of the death toll that bacterial infection causes is 1,700 ten thousand, account for 1/3.These transmissible diseases comprise cholera, pneumonia, dysentery, tuberculosis etc.The food poisoning of the nationwide that the pathogenicity bo intestinal bacteria O-157 of Japan's generation in 1996 causes was once once causing global fear.In addition, mikrobe also can cause the decomposition, rotten and corrupt of various Industrial materials, makeup, pharmaceuticals etc., thereby makes the lost of life of product.Therefore, the growth and the breeding of control and elimination unwanted bacteria in today of development in Hi-Tech, remain a research topic closely bound up with human health.
One of approach of human infection bacterium is exactly the food through inlet, and packaging material for food generally directly contacts with food, and the nutritive ingredient of food in abundance just becomes the nutrition source of microbial growth breeding under pyritous package interior environment.Therefore, the development that has a packaging material for food of anti-bacterial refreshing function just seems extremely important.
Nano anti-biotic material is one type of type material with bacteriostasis property; Because the endowing antibacterial of material own; Can make mikrobe comprise that the growth of bacterium, fungi, yeast, algae and virus etc. and breeding keep lower level; And silver ions is the strongest bacterinertness metal of bacterinertness of generally acknowledging, therefore develops a kind of nano composite antibacterial class coating material that contains silver ions, has great importance for the life and the health level that improve people.
Summary of the invention
The purpose of this invention is to provide PVA-based nano composite antibacterial class coating material of a kind of argentiferous ionic and preparation method thereof; Be characterized in utilizing the special construction of nano silicon and performance that macromolecular material is carried out modification; And the bacterinertness of combination silver ions; It is continuous to obtain a kind of anti-microbial property, and the nano composite antibacterial class coating material that the persistent over-all properties of anti-microbial effect is better can be expanded its application at aspects such as wrapping material, coating greatly.
The PVA-based nano composite antibacterial class coating material of a kind of argentiferous ionic that the present invention proposes, said class coating material comprises: Z 150PH, Triple Pressed Stearic Acid, nano silicon, silver ions and water, the weight percent of its raw material and volumetric molar concentration are:
Z 150PH 1wt% ~ 10wt%,
Triple Pressed Stearic Acid 0.1wt% ~ 5wt%,
Nano silicon 0.5wt% ~ 8wt%,
Silver ions volumetric molar concentration 0.1mmol/L ~ 0.7mmol/L,
All the other are water, and its gross weight satisfies 100%.
Among the present invention, described Z 150PH is 4 wt % ~ 8 wt %, and Triple Pressed Stearic Acid is 0.5 wt % ~ 3 wt %, and nano silicon is 0.5wt% ~ 4wt%.The silver ions volumetric molar concentration is 0.1mmol/L ~ 0.7mmol/L, and all the other are water, and its gross weight satisfies 100%.
The preparation method of the PVA-based nano composite antibacterial class coating material of a kind of argentiferous ionic that the present invention proposes, concrete steps are following:
(1) preparation of PVA-based nanocomposite coating material
Z 150PH is immersed in makes its abundant water absorption and swelling in the water more than 2 ~ 4 hours, polyvinyl alcohol solution 85 ℃ ~ 95 ℃ thoroughly dissolvings, is added the Triple Pressed Stearic Acid through dissolution with solvents simultaneously; 80 ℃ ~ 95 ℃ magnetic agitation of constant temperature 5 minutes add nano material silicon-dioxide again, 80 ℃ ~ 95 ℃ magnetic agitation of constant temperature 15 minutes; Through after the supersound process, above-mentioned solution is coated on the slick sheet glass, place stink cupboard; Solution evaporation is 48 ~ 72 hours under the room temperature, treats that film takes off naturally, film is immersed in the sodium hydroxide of 1wt% ~ 3wt% to soak 1 ~ 2 hour; Remove residual dissolving; Wash repeatedly to neutrality with zero(ppm) water, seasoning obtains PVA-based nanocomposite coating material.
(2) preparation of the PVA-based nano composite antibacterial class coating material of argentiferous ionic
It is in the silver nitrate solution of 0.1 ~ 0.7mmol/L that above-mentioned PVA-based nanocomposite coating material is immersed 30 ~ 70ml concentration; Stirred 2 ~ 6 hours; Remove residual silver ions through washed with de-ionized water, drying at room temperature obtains the PVA-based nano composite antibacterial class coating material of argentiferous ionic.
Among the present invention, solvent described in the step (1) is one or more compositions in methyl alcohol, ethanol, propyl alcohol, propyl carbinol or the terepthaloyl moietie.
Among the present invention, the temperature of described constant temperature magnetic agitation is 85 ~ 95 ℃.
Among the present invention, during supersound process, control power is 80 ~ 270W; The supersound process time is 5 ~ 20 minutes.
With respect to scheme of the prior art, advantage of the present invention is:
Utilize the special construction and the performance of nano silicon that macromolecular material is carried out modification, and combine the bacterinertness of silver ions, it is continuous to obtain a kind of anti-microbial property, the nano composite antibacterial class coating material that the persistent over-all properties of anti-microbial effect is better.Utilize the class coating material of the present invention's technology preparation to have the following advantages:
1, has tangible water preventing ability, can delay the migration and the diffusion of food Zhong Shui and oil and other compositions;
2, have selectable ventilation property and impermeabilisation ability;
3, can stop the volatilization of flavour substances in the food;
4, can be used as the food color, the carrier of nutritional fortification and antioxidant etc.;
5, anti-microbial property has continuity and persistence.
Description of drawings
Fig. 1 is the influence figure of silica concentration to permeability rate and transmittance.
Fig. 2 is the influence figure of ultrasonication power to the film forming permeability rate.
Fig. 3 is the influence figure of ultrasonic treatment time to permeability rate.
Embodiment
Below in conjunction with specific embodiment such scheme is further specified.Should be understood that these embodiment are used to the present invention is described and are not limited to limit scope of the present invention.
Embodiment 1
(1) preparation of PVA-based nanocomposite coating material
Z 150PH 2g part is immersed in makes its abundant water absorption and swelling in the water more than 2 hours, polyvinyl alcohol solution 85 ℃ of thoroughly dissolvings, is added the Triple Pressed Stearic Acid through dissolve with methanol simultaneously; 85 ℃ of magnetic agitation of constant temperature 5 minutes add nano material silicon-dioxide again, 85 ℃ of magnetic agitation of constant temperature 15 minutes; Under the UW of 80W ultrasonic 5 minutes, with above-mentioned solution apply with slick sheet glass on, place stink cupboard; Solution evaporation is 48 hours under the room temperature, treats that film takes off naturally, film is immersed in the sodium hydroxide of 1wt% to soak 1 hour; Remove residual dissolving, wash repeatedly to neutrality with zero(ppm) water, seasoning obtains PVA-based nanocomposite coating material.
(2) preparation of the PVA-based nano composite antibacterial class coating material of argentiferous ionic
It is in the silver nitrate solution of 0.1mmol/L that above-mentioned PVA-based nanocomposite coating material is immersed 30ml concentration; Stirred 2 hours; Remove residual silver ions through washed with de-ionized water, drying at room temperature obtains the PVA-based nano composite antibacterial class coating material of argentiferous ionic.
Embodiment 2:
(1) preparation of PVA-based nanocomposite coating material
Z 150PH 4g is immersed in makes its abundant water absorption and swelling in the water more than 2.5 hours, polyvinyl alcohol solution 88 ℃ of thoroughly dissolvings, is added the Triple Pressed Stearic Acid through dissolve with ethanol simultaneously; 88 ℃ of magnetic agitation of constant temperature 5 minutes add nano material silicon-dioxide again, 88 ℃ of magnetic agitation of constant temperature 15 minutes; Under the UW of 100W ultrasonic 10 minutes, with above-mentioned solution apply with slick sheet glass on, place stink cupboard; Solution evaporation is 55 hours under the room temperature, treats that film takes off naturally, film is immersed in the sodium hydroxide of 1.5wt% to soak 1.5 hours; Remove residual dissolving, wash repeatedly to neutrality with zero(ppm) water, seasoning obtains PVA-based nanocomposite coating material.
(2) preparation of the PVA-based nano composite antibacterial class coating material of argentiferous ionic
It is in the silver nitrate solution of 0.2mmol/L that above-mentioned PVA-based nanocomposite coating material is immersed 40ml concentration; Stirred 3 hours; Remove residual silver ions through washed with de-ionized water, drying at room temperature obtains the PVA-based nano composite antibacterial class coating material of argentiferous ionic.
Embodiment 3:
(1) preparation of PVA-based nanocomposite coating material
Z 150PH 6g is immersed in makes its abundant water absorption and swelling in the water more than 3 hours, polyvinyl alcohol solution 90 ℃ of thoroughly dissolvings, is added through propyl alcohol dissolved Triple Pressed Stearic Acid simultaneously; 90 ℃ of magnetic agitation of constant temperature 5 minutes add nano material silicon-dioxide again, 90 ℃ of magnetic agitation of constant temperature 15 minutes; Under the UW of 150W ultrasonic 18 minutes, with above-mentioned solution apply with slick sheet glass on, place stink cupboard; Solution evaporation is 60 hours under the room temperature, treats that film takes off naturally, film is immersed in the sodium hydroxide of 2wt% to soak 1.8 hours; Remove residual dissolving, wash repeatedly to neutrality with zero(ppm) water, seasoning obtains PVA-based nanocomposite coating material.
(2) preparation of the PVA-based nano composite antibacterial class coating material of argentiferous ionic
It is in the silver nitrate solution of 0.3mmol/L that above-mentioned PVA-based nanocomposite coating material is immersed 50ml concentration; Stirred 4 hours; Remove residual silver ions through washed with de-ionized water, drying at room temperature obtains the PVA-based nano composite antibacterial class coating material of argentiferous ionic.
Embodiment 4:
(1) preparation of PVA-based nanocomposite coating material
Z 150PH 8g is immersed in makes its abundant water absorption and swelling in the water more than 3.5 hours, polyvinyl alcohol solution 92 ℃ of thoroughly dissolvings, is added through propyl carbinol dissolved Triple Pressed Stearic Acid simultaneously; 92 ℃ of magnetic agitation of constant temperature 5 minutes add nano material silicon-dioxide again, 92 ℃ of magnetic agitation of constant temperature 15 minutes; Under the UW of 200W ultrasonic 19 minutes, with above-mentioned solution apply with slick sheet glass on, place stink cupboard; Solution evaporation is 65 hours under the room temperature, treats that film takes off naturally, film is immersed in the sodium hydroxide of 2.5wt% to soak 2 hours; Remove residual dissolving, wash repeatedly to neutrality with zero(ppm) water, seasoning obtains PVA-based nanocomposite coating material.
(2) preparation of the PVA-based nano composite antibacterial class coating material of argentiferous ionic
It is in the silver nitrate solution of 0.4mmol/L that above-mentioned PVA-based nanocomposite coating material is immersed 60ml concentration; Stirred 5 hours; Remove residual silver ions through washed with de-ionized water, drying at room temperature obtains the PVA-based nano composite antibacterial class coating material of argentiferous ionic.
Embodiment 5:
(1) preparation of PVA-based nanocomposite coating material
Z 150PH 10g is immersed in makes its abundant water absorption and swelling in the water more than 4 hours, polyvinyl alcohol solution 95 ℃ of thoroughly dissolvings, is added through terepthaloyl moietie dissolved Triple Pressed Stearic Acid simultaneously; 95 ℃ of magnetic agitation of constant temperature 5 minutes add nano material silicon-dioxide again, 95 ℃ of magnetic agitation of constant temperature 15 minutes; Under the UW of 220W ultrasonic 20 minutes, with above-mentioned solution apply with slick sheet glass on, place stink cupboard; Solution evaporation is 72 hours under the room temperature, treats that film takes off naturally, film is immersed in the sodium hydroxide of 3wt% to soak 2 hours; Remove residual dissolving, wash repeatedly to neutrality with zero(ppm) water, seasoning obtains PVA-based nanocomposite coating material.
(2) preparation of the PVA-based nano composite antibacterial class coating material of argentiferous ionic
It is in the silver nitrate solution of 0.7mmol/L that above-mentioned PVA-based nanocomposite coating material is immersed 70ml concentration; Stirred 6 hours; Remove residual silver ions through washed with de-ionized water, drying at room temperature obtains the PVA-based nano composite antibacterial class coating material of argentiferous ionic.
Fig. 1 is the influence figure of silica concentration to permeability rate and transmittance.Fig. 1 result shows that silica concentration was less than 2% o'clock, and nano composite antibacterial class coating material film forming permeability rate is along with the increase of silica concentration sharply reduces, and 2% later film forming permeability rate slowly reduces.This shows that use nano composite antibacterial class coating material can significantly reduce permeability rate.Silica concentration is when 0%-1%, and transmittance is along with the increase of silica concentration sharply reduces, and is little greater than 1% transmittance variation later on, maintains lower level.This shows that the use nano silicon can significantly reduce composite antibiosis class coating material film forming transmittance.Comprehensive permeability rate and transmittance are considered from the materials economic benefit with the variation tendency of silica concentration, silica concentration are fixed on 2% be advisable.
Fig. 2 is the influence figure of ultrasonication power to the film forming permeability rate.Fig. 2 result shows that in ultrasonication power 88W-264W scope, nano composite antibacterial class coating material film forming permeability rate reduces along with the increase of ultrasonic power.Ultrasonication power film forming permeability rate when the 88W-220W scope obviously reduces along with the increase of ultrasonic power, and descends no longer obvious when ultrasonication power film forming permeability rate when 220W brings up to 264W.Test shows that ultrasonication can effectively reduce the permeability rate of nanocomposite coating material.Consider from the power benefit, ultrasonication power is fixed on 220W be advisable.With ultra wave power is variable, and the film forming permeability rate is that objective function carries out index return, obtains indicial equation: Y=3.037e-0.4577X.R
2=0.9594, the very high (p of degree of fitting of indicial equation is described<0.01).
Fig. 3 is the influence figure of ultrasonic treatment time to permeability rate.Fig. 3 result shows that when 3-9min, nano composite antibacterial class coating material film forming permeability rate is along with the prolongation of UW time is the trend that sharply reduces, and permeability rate slowly reduces after the 9min.Consider from the time benefit, ultrasonic treatment time is fixed on 9min be advisable.With ultra wave power is variable, and the film forming permeability rate is that objective function carries out index return, obtains logarithmic equation: Y=-0.917Ln (X)+1.566. (R
2=0.8973).
Synthesizing map 2, Fig. 3 presentation of results ultrasonication can obviously reduce the permeability rate of nanocomposite coating material filming, significantly improve the performance of film.
Claims (6)
1. PVA-based nano composite antibacterial class coating material of argentiferous ionic is characterized in that said class coating material comprises: Z 150PH, Triple Pressed Stearic Acid, nano silicon, silver ions and water, and the weight percent and the volumetric molar concentration of its raw material are respectively:
Z 150PH 1wt% ~ 10wt%,
Triple Pressed Stearic Acid 0.1wt% ~ 5wt%,
Nano silicon 0.5wt% ~ 8wt%,
Silver ions volumetric molar concentration 0.1mmol/L ~ 0.7mmol/L,
All the other are water, and its gross weight satisfies 100%.
2. according to claim
1Described a kind of PVA-based nano composite antibacterial class coating material; It is characterized in that described Z 150PH is 4 wt % ~ 8 wt %; Triple Pressed Stearic Acid is 0.5 wt % ~ 3 wt %, and nano silicon is 0.5wt% ~ 4wt%, and the silver ions volumetric molar concentration is 0.1mmol/L ~ 0.7mmol/L; All the other are water, and its gross weight satisfies 100%.
3. one kind like claim
1The preparation method of described PVA-based nano composite antibacterial class coating material is characterized in that concrete steps are following:
(1) preparation of PVA-based nanocomposite coating material
Z 150PH 1 ~ 10 weight part is immersed in makes its abundant water absorption and swelling in the water more than 2 ~ 4 hours, polyvinyl alcohol solution 85 ℃ ~ 95 ℃ thoroughly dissolvings, is added the Triple Pressed Stearic Acid through dissolution with solvents simultaneously; 80 ~ 95 ℃ of magnetic agitation of constant temperature 5 minutes add nano material silicon-dioxide again, 80 ~ 95 ℃ of magnetic agitation of constant temperature 15 minutes; Through after the supersound process, on above-mentioned solution coating and slick sheet glass, place stink cupboard; Solution evaporation is 48 ~ 72 hours under the room temperature; Treat that film takes off naturally, film is immersed in the sodium hydroxide of 1wt% ~ 3wt% and soaked 1 ~ 2 hour, remove residual solvent; Wash repeatedly to neutrality with zero(ppm) water, seasoning obtains PVA-based nanocomposite coating material;
(2) preparation of the PVA-based nano composite antibacterial class coating material of argentiferous ionic
It is in the silver nitrate solution of 0.1 ~ 0.7mmol/L that above-mentioned PVA-based nanocomposite coating material is immersed 30 ~ 70ml concentration; Stirred 2 ~ 6 hours; Remove residual silver ions through washed with de-ionized water, drying at room temperature obtains the PVA-based nano composite antibacterial class coating material of argentiferous ionic.
4. according to claim
3The preparation method of the PVA-based nano composite antibacterial class coating material of described a kind of argentiferous ionic is characterized in that said solvent is one or more compositions in methyl alcohol, ethanol, propyl alcohol, propyl carbinol or the terepthaloyl moietie.
5. according to claim
3The preparation method of the PVA-based nano composite antibacterial class coating material of described a kind of argentiferous ionic, the temperature that it is characterized in that said constant temperature magnetic agitation is 85 ~ 95 ℃.
6. according to claim
3The preparation method of the PVA-based nano composite antibacterial class coating material of described a kind of argentiferous ionic is characterized in that in the said supersound process that the control watt level is 80 ~ 270W, and the time is 5 ~ 20 minutes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104788777A (en) * | 2015-03-30 | 2015-07-22 | 安徽松泰包装材料有限公司 | Production process for nano packaging material |
| CN107641377A (en) * | 2017-11-02 | 2018-01-30 | 苏州甫众塑胶有限公司 | A kind of preparation method of food packaging antibiotic paint |
| CN109135142A (en) * | 2018-08-30 | 2019-01-04 | 盛世瑶兰（深圳）科技有限公司 | A kind of antibacterial food packaging material and preparation method thereof |
| CN110959610A (en) * | 2019-12-27 | 2020-04-07 | 浙江隆泰医疗科技股份有限公司 | Medical silver ion antibacterial film and preparation method thereof |
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| CN101125934A (en) * | 2007-09-30 | 2008-02-20 | 四川大学 | Method for preparing chitosan/nylon composite antibacterial film containing silver ion |
| CN101481565A (en) * | 2008-01-07 | 2009-07-15 | 刘建林 | Aqueous high isolation coating solution and boiling resistant high isolation coating obtained thereby |
| US20100150980A1 (en) * | 2007-04-04 | 2010-06-17 | Perlen Converting Ag | Antimicrobial material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100150980A1 (en) * | 2007-04-04 | 2010-06-17 | Perlen Converting Ag | Antimicrobial material |
| CN101125934A (en) * | 2007-09-30 | 2008-02-20 | 四川大学 | Method for preparing chitosan/nylon composite antibacterial film containing silver ion |
| CN101481565A (en) * | 2008-01-07 | 2009-07-15 | 刘建林 | Aqueous high isolation coating solution and boiling resistant high isolation coating obtained thereby |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788777A (en) * | 2015-03-30 | 2015-07-22 | 安徽松泰包装材料有限公司 | Production process for nano packaging material |
| CN107641377A (en) * | 2017-11-02 | 2018-01-30 | 苏州甫众塑胶有限公司 | A kind of preparation method of food packaging antibiotic paint |
| CN107641377B (en) * | 2017-11-02 | 2020-03-03 | 广东威雅包装印刷有限公司 | Preparation method of antibacterial coating for food packaging |
| CN109135142A (en) * | 2018-08-30 | 2019-01-04 | 盛世瑶兰（深圳）科技有限公司 | A kind of antibacterial food packaging material and preparation method thereof |
| CN110959610A (en) * | 2019-12-27 | 2020-04-07 | 浙江隆泰医疗科技股份有限公司 | Medical silver ion antibacterial film and preparation method thereof |
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Application publication date: 20120328 |