CN104893213B - Carry the preparation method of silver-colored graphene oxide polyvinyl alcohol compound film - Google Patents
Carry the preparation method of silver-colored graphene oxide polyvinyl alcohol compound film Download PDFInfo
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- CN104893213B CN104893213B CN201510345694.7A CN201510345694A CN104893213B CN 104893213 B CN104893213 B CN 104893213B CN 201510345694 A CN201510345694 A CN 201510345694A CN 104893213 B CN104893213 B CN 104893213B
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Abstract
The invention discloses a kind of preparation method for carrying silver-colored graphene oxide polyvinyl alcohol compound film.Graphene oxide is disperseed to obtain finely dispersed mixed liquor in deionized water, add the silver ammino solution newly configured, under the conditions of 40 60 DEG C stirring mixing simultaneously be added dropwise polyethylene glycol, 115 125 DEG C of 3h of insulation reaction 2, washing, dry after obtain carrying silver-colored graphene oxide powder；PVA is dissolved in deionized water, the silver-colored graphene oxide of above-mentioned load is added, is thoroughly mixed, 85 95 DEG C of 1 2h of reaction, cooling, plastic film mulch obtain carrying silver-colored graphene oxide polyvinyl alcohol compound film.Obtained composite membrane is smooth, uniform and has larger pliability, can use pocket knife or scissors cut into preferable shape of all kinds；With preferably the excellent properties such as intensity, heat endurance are drawn high, also with certain anti-microbial property.
Description
Technical field
The invention belongs to field of compound material, and in particular to a kind of system of the silver-colored graphene oxide polyvinyl alcohol compound film of load
Preparation Method.
Background technology
In recent years, the increasing visual field for entering people of active food packaging, active food packaging is i.e. by antiseptic etc.
Additive is added in the packaging material of food, to reach the purpose of extension Food Shelf-life.Polyvinyl alcohol (PVA) is a kind of water-soluble
Property synthesising macromolecule copolymer, its is intermolecular to have great amount of hydroxy group, has preferable water imbibition, excellent barrier properties for gases is nontoxic
Property, the features such as degradation speed is fast, compared to the polyethylene largely used on market today, the packaging material for food such as polyvinyl chloride is one
Plant environmentally friendly material.However, relatively low mechanical property limits the application of PVA film.
The two-dimensional slice that the carbon atom that graphene oxide is connected by covalent bond is constituted is stacked and formed, and is carried in basal plane and edge
Various hydrophilic acidic oxygenated functional groups, such as hydroxyl, epoxy radicals, with the features such as specific surface area is big, ion-exchange capacity is strong,
These features impart its good compound ability.These oxygen-containing functional groups enable graphene oxide and polar micromolecules or poly-
Compound interacts to form graphene oxide intercalation composite material or graphene oxide stripping composite.
Nano Silver has very strong bactericidal effect, and the larger and superpower activity of surface area, can be antibacterial as preparing
The anti-biotic material of film.There are many scholars to propose the characteristic using two kinds of materials of Nano Silver and graphene oxide recently, oxidation is made
Graphene-nano silver composite material, is expected to develop the excellent novel antibacterial material of anti-microbial property.Such a method can both be prevented
The reunion of Nano Silver in aqueous, can improve antibacterial ability again.
The content of the invention
Present invention aims at offer one kind thin polymer film is applied to oxidation nanometer silver-graphene oxide composite material
On method, reach good anti-bacterial effect, cheap, and easily film forming, stability is good, solves after membrane modifying in application process
The purpose of problems.
The preparation method of silver-colored graphene oxide polyvinyl alcohol compound film is carried, is comprised the following steps：
Graphene oxide is disperseed to obtain finely dispersed mixed liquor in deionized water, the silver-colored ammonia newly configured is added molten
Liquid, stirring mixing is added dropwise polyethylene glycol simultaneously under the conditions of 40-60 DEG C, 115-125 DEG C of insulation reaction 2-3h, washing, dry after
To the silver-colored graphene oxide powder of load；
PVA is dissolved in deionized water, the silver-colored graphene oxide of above-mentioned load is added, is thoroughly mixed, 85-95 DEG C of reaction
1-2h, cooling, plastic film mulch obtain carrying silver-colored graphene oxide polyvinyl alcohol compound film.
By such scheme, the scattered concentration range for obtaining mixed liquor in deionized water of the graphene oxide is 1mg/mL
~3mg/mL.
By such scheme, the graphene oxide：AgNO in silver ammino solution3：The mass ratio of polyethylene glycol is 100：
100：1.
By such scheme, the concentration range that the PVA is dissolved in deionized water is 5g/mL~15g/mL.
By such scheme, the PVA：It is 10 to carry silver-colored graphene oxide mass ratio:1~10:0.5.
The present invention possesses effective as follows relative to prior art：
Obtained composite membrane is smooth, uniform and has larger pliability, can be with pocket knife or scissors cut into various each
The preferable shape of sample.
Obtained composite membrane, which has, preferably draws high the excellent properties such as intensity, heat endurance.
Obtained composite membrane has certain anti-microbial property.
Brief description of the drawings
Fig. 1：Carry silver-colored graphene oxide polyvinyl alcohol compound film tensile strength.
Embodiment
Following examples further explain technical scheme, but not as limiting the scope of the invention.
Embodiment 1
100mg graphite oxide powder is taken to be dispersed in 50mL deionized waters, ultrasonic 1h, which is fully peeled off, obtains graphene oxide
(GO) dispersion liquid；Simultaneously by 100mgAgNO3It is dissolved in 10mL deionized waters, and the ammoniacal liquor of mass fraction 3% is instilled into AgNO3
Until AgOH/Ag in the aqueous solution2O precipitations just disappear, and are prepared into silver ammino solution；At 60 DEG C by freshly prepd silver ammino solution with
Above obtained 50mL graphene oxide water solutions are mixed, while adding 1g polyethylene glycol (PEG-400), are sufficiently stirred for
1.5h.In the hydrothermal reaction kettle of polytetrafluoroethyllining lining after 120 DEG C of insulation 2h, question response liquid natural cooling, deionized water is used
Product is repeatedly washed with ethanol, the silver-colored graphene oxide of load is dried to obtain.
10g PVA is dissolved in deionized water, 2h is stirred under the conditions of 90 DEG C, PVA all dissolves.Take the above-mentioned load silver of 0.1g
Graphene oxide is added in the PVA aqueous solution, is stirred 1h under the conditions of 90 DEG C of oil bath heatings, is cooled to after room temperature, the tape casting plastic film mulch.
Embodiment 2
100mg graphite oxide powder is taken to be dispersed in 50mL deionized waters, ultrasonic 1h, which is fully peeled off, obtains graphene oxide
(GO) dispersion liquid；Simultaneously by 100mgAgNO3It is dissolved in 10mL deionized waters, and the ammoniacal liquor of mass fraction 3% is instilled into AgNO3
Until AgOH/Ag in the aqueous solution2O precipitations just disappear, and are prepared into silver ammino solution；At 60 DEG C by freshly prepd silver ammino solution with
Above obtained 50mL graphene oxide water solutions are mixed, while adding 1g polyethylene glycol (PEG-400), are sufficiently stirred for
1.5h.In the hydrothermal reaction kettle of polytetrafluoroethyllining lining after 120 DEG C of insulation 2h, question response liquid natural cooling, deionized water is used
Product is repeatedly washed with ethanol, the silver-colored graphene oxide of load is dried to obtain.
10g PVA is dissolved in deionized water, 2h is stirred under the conditions of 90 DEG C, PVA all dissolves.Take the above-mentioned load silver of 0.2g
Graphene oxide is added in the PVA aqueous solution, is stirred 1.2h under the conditions of 90 DEG C of oil bath heatings, is cooled to after room temperature, the tape casting plastic film mulch.
Embodiment 3
100mg graphite oxide powder is taken to be dispersed in 50mL deionized waters, ultrasonic 1h, which is fully peeled off, obtains graphene oxide
(GO) dispersion liquid；Simultaneously by 100mgAgNO3It is dissolved in 10mL deionized waters, and the ammoniacal liquor of mass fraction 3% is instilled into AgNO3
Until AgOH/Ag in the aqueous solution2O precipitations just disappear, and are prepared into silver ammino solution；At 60 DEG C by freshly prepd silver ammino solution with
Above obtained 50mL graphene oxide water solutions are mixed, while adding 1g polyethylene glycol (PEG-400), are sufficiently stirred for
1.5h.In the hydrothermal reaction kettle of polytetrafluoroethyllining lining after 120 DEG C of insulation 2h, question response liquid natural cooling, deionized water is used
Product is repeatedly washed with ethanol, the silver-colored graphene oxide of load is dried to obtain.
10g PVA is dissolved in deionized water, 2.5h is stirred under the conditions of 90 DEG C, PVA all dissolves.Take the above-mentioned loads of 0.3g
Silver-colored graphene oxide is added in the PVA aqueous solution, is stirred 1.5h under the conditions of 90 DEG C of oil bath heatings, is cooled to after room temperature, the tape casting paving
Film.
Embodiment 4
100mg graphite oxide powder is taken to be dispersed in 50mL deionized waters, ultrasonic 1h, which is fully peeled off, obtains graphene oxide
(GO) dispersion liquid；Simultaneously by 100mgAgNO3It is dissolved in 10mL deionized waters, and the ammoniacal liquor of mass fraction 3% is instilled into AgNO3
Until AgOH/Ag in the aqueous solution2O precipitations just disappear, and are prepared into silver ammino solution；It is at 40-60 DEG C that freshly prepd silver-colored ammonia is molten
Liquid is mixed with above obtained 50mL graphene oxide water solutions, while adding 1g polyethylene glycol (PEG-400), is fully stirred
Mix 1.52h.In the hydrothermal reaction kettle of polytetrafluoroethyllining lining after 120 DEG C of insulation 2h, question response liquid natural cooling, deionization is used
Water and ethanol are repeatedly washed to product, are dried to obtain the silver-colored graphene oxide of load.
10g PVA is dissolved in deionized water, 2.5h is stirred under the conditions of 90 DEG C, PVA all dissolves.Take the above-mentioned loads of 0.4g
Silver-colored graphene oxide is added in the PVA aqueous solution, is stirred 1.8h under the conditions of 90 DEG C of oil bath heatings, is cooled to after room temperature, the tape casting paving
Film.
Embodiment 5
100mg graphite oxide powder is taken to be dispersed in 50mL deionized waters, ultrasonic 1h, which is fully peeled off, obtains graphene oxide
(GO) dispersion liquid；Simultaneously by 100mgAgNO3It is dissolved in 10mL deionized waters, and the ammoniacal liquor of mass fraction 3% is instilled into AgNO3
Until AgOH/Ag in the aqueous solution2O precipitations just disappear, and are prepared into silver ammino solution；It is at 40-60 DEG C that freshly prepd silver-colored ammonia is molten
Liquid is mixed with above obtained 50mL graphene oxide water solutions, while adding 1g polyethylene glycol (PEG-400), is fully stirred
Mix 1.52h.In the hydrothermal reaction kettle of polytetrafluoroethyllining lining after 120 DEG C of insulation 2h, question response liquid natural cooling, deionization is used
Water and ethanol are repeatedly washed to product, are dried to obtain the silver-colored graphene oxide of load.
10g PVA is dissolved in deionized water, 3h is stirred under the conditions of 90 DEG C, PVA all dissolves.Take the above-mentioned load silver of 0.5g
Graphene oxide is added in the PVA aqueous solution, is stirred 2h under the conditions of 90 DEG C of oil bath heatings, is cooled to after room temperature, the tape casting plastic film mulch.
The present invention carries the performance of silver-colored graphene oxide polyvinyl alcohol compound film as shown in Figure 1.Add the load of different content
Silver-colored graphene oxide and the test that tensile strength is carried out to it, the tensile strength of PVA blank is 34MPa, with filler quality
The trend of first increases and then decreases is presented in the increase of fractional content, PVA tensile strength.The silver-colored graphene oxide of a small amount of load is to PVA
There is good strengthening action, one is due to that functional graphene oxide monolithic/multi-slice nanoscale is dispersed, specific surface area
Greatly, there is good compatibility with PVA matrixes, add the mechanical property of composite.On the other hand due to carrying silver-colored graphite oxide
The active function groups of alkene sheet surfaces can make it improve composite wood within the specific limits with-OH formation hydrogen bond in PVA molecules
The tensile strength of material.But with the increase for carrying silver-colored graphene oxide content, the formation of excessive additional chemical crosslinking points so that high score
Subchain is further fettered, and this inevitably results in the decline of tensile strength.
Claims (4)
1. carry the preparation method of silver-colored graphene oxide polyvinyl alcohol compound film, it is characterised in that comprise the following steps：
Graphene oxide is disperseed to obtain finely dispersed mixed liquor in deionized water, the silver ammino solution newly configured, 40- is added
Under the conditions of 60 DEG C stirring mixing simultaneously be added dropwise polyethylene glycol, 115-125 DEG C of insulation reaction 2-3h, washing, dry after obtain carry silver
Graphene oxide powder；The graphene oxide：AgNO in silver ammino solution3：The mass ratio of polyethylene glycol is 100：100：1；
PVA is dissolved in deionized water, the silver-colored graphene oxide of above-mentioned load is added, is thoroughly mixed, 85-95 DEG C of reaction 1-
2h, cooling, plastic film mulch obtain carrying silver-colored graphene oxide polyvinyl alcohol compound film.
2. the preparation method of silver-colored graphene oxide polyvinyl alcohol compound film is carried as claimed in claim 1, it is characterised in that described
The scattered concentration range for obtaining mixed liquor in deionized water of graphene oxide is 1mg/mL~3mg/mL.
3. the preparation method of silver-colored graphene oxide polyvinyl alcohol compound film is carried as claimed in claim 1, it is characterised in that described
The concentration range that PVA is dissolved in deionized water is 5g/mL~15g/mL.
4. the preparation method of silver-colored graphene oxide polyvinyl alcohol compound film is carried as claimed in claim 1, it is characterised in that described
PVA：It is 10 to carry silver-colored graphene oxide mass ratio:1~10:0.5.
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| CN105778373A (en) * | 2016-05-10 | 2016-07-20 | 四川大学 | Method for preparing melt-processable modified polyvinyl alcohol-graphene composite material |
| KR102219506B1 (en) * | 2016-09-08 | 2021-02-25 | 닛토덴코 가부시키가이샤 | No antimicrobial graphene oxide |
| CN112210177B (en) * | 2020-10-12 | 2022-10-25 | 广安长明高端产业技术研究院 | 3D printing antibacterial conductive composite material and preparation method thereof |
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|---|---|---|---|---|
| GB1478411A (en) * | 1973-10-10 | 1977-06-29 | Hoechst Ag | Electrolytic polymerization process |
| CN101687584A (en) * | 2007-05-11 | 2010-03-31 | J-化学株式会社 | Plastic sheet for packaging container |
| CN103214772A (en) * | 2012-01-18 | 2013-07-24 | 广西格润科技有限公司 | Novel heat-dissipation material and preparation method thereof |
| CN103613773A (en) * | 2013-11-07 | 2014-03-05 | 常州大学 | Preparation method of flexible transparent conducting polymer thin film with antibacterial properties |
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2015
- 2015-06-19 CN CN201510345694.7A patent/CN104893213B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1478411A (en) * | 1973-10-10 | 1977-06-29 | Hoechst Ag | Electrolytic polymerization process |
| CN101687584A (en) * | 2007-05-11 | 2010-03-31 | J-化学株式会社 | Plastic sheet for packaging container |
| CN103214772A (en) * | 2012-01-18 | 2013-07-24 | 广西格润科技有限公司 | Novel heat-dissipation material and preparation method thereof |
| CN103613773A (en) * | 2013-11-07 | 2014-03-05 | 常州大学 | Preparation method of flexible transparent conducting polymer thin film with antibacterial properties |
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Effective date of registration: 20201021 Address after: No.9, merchants Avenue, Jiangling County, Jingzhou City, Hubei Province, 434100 Patentee after: Hubei Polymeric Polymer Material Co.,Ltd. Address before: 430074, No. 693 Xiong Chu street, Hongshan District, Hubei, Wuhan Patentee before: WUHAN INSTITUTE OF TECHNOLOGY |
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Effective date of registration: 20210810 Address after: 430074 No. 602, building 1-05, optical valley core center, 303 Guanggu Avenue, Donghu New Technology Development Zone, Wuhan City, Hubei Province Patentee after: WUHAN HEJU PLASTICIZING NEW MATERIAL Co.,Ltd. Address before: 434100 No.9, merchants Avenue, Jiangling County, Jingzhou City, Hubei Province Patentee before: Hubei Polymeric Polymer Material Co.,Ltd. |
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Effective date of registration: 20230119 Address after: 434100 No.9, merchants Avenue, Jiangling County, Jingzhou City, Hubei Province Patentee after: Hubei Polymeric Polymer Material Co.,Ltd. Address before: 430074 No. 602, building 1-05, optical valley core center, 303 Guanggu Avenue, Donghu New Technology Development Zone, Wuhan City, Hubei Province Patentee before: WUHAN HEJU PLASTICIZING NEW MATERIAL CO.,LTD. |