CN105218996A - A kind of preparation method of modified graphene-polyvinyl alcohol compound film - Google Patents
A kind of preparation method of modified graphene-polyvinyl alcohol compound film Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of modified graphene-polyvinyl alcohol compound film, Hymecromone selected by properties-correcting agent of the present invention, and the present invention selects the chemical reducing agents such as hydrazine hydrate, vitamins C or glucose; First prepare modified graphene, then prepare the dispersion liquid of modified graphene, then the dispersion liquid of modified graphene is joined in polyvinyl alcohol water solution, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution; Finally above-mentioned mixing solutions is poured in vessel, under air or vacuum environment, be dried to constant weight in 40-70 degree Celsius, obtain modified graphene/polyvinyl alcohol compound film.Wherein, the massfraction of modified graphene is 0.1%-10%.The present invention has that preparation is simple, reaction conditions is gentle, be easy to the advantages such as manipulation system.
Description
Technical field
The invention belongs to polymer composites preparing technical field, be specifically related to a kind of preparation method of modified graphene-polyvinyl alcohol compound film.
Background technology
Polyvinyl alcohol (PVA) is by a kind of water-soluble polymers of Vinyl Acetate Copolymer Ester hydrolysis, has excellent wetting ability and film-forming properties, also has good chemical stability and biocompatibility, safety non-toxic, of many uses.But the poor performance such as the intensity of polyvinyl alcohol own is low, heat-resisting, this makes polyvinyl alcohol and matrix material thereof all be restricted in the application of numerous areas.
Graphene is a kind of novel two-dimensional nano carbon material, has excellent electrical property, mechanical property and thermal characteristics etc., therefore, it can be used as nanofiller component to add in polymkeric substance, effectively can improve the electricity of polymkeric substance, machinery and the performance such as hot.Therefore, this method will become study hotspot and the emphasis in polymer based nanocomposites field.But, the surface of Graphene is inert condition, and the interaction between other media is weak, and there is between graphene sheet layer stronger Van der Waals force, cause that it is hydrophilic, lipophilicity is all very poor, this makes its bad dispersibility in polyvinyl alcohol matrix and easily reunites, thus can not well with polymer-based carbon volume recombination, which greatly limits the further investigation and application scope of Graphene-polyvinyl alcohol composite material.
The dispersion state of Graphene can produce obvious impact to the performance of matrix material, and therefore, the dispersion problem of Graphene is the key issue in Graphene/polyvinyl alcohol composite material preparation.
Summary of the invention
For prior art above shortcomings, the present invention utilizes properties-correcting agent to modify Graphene, thus improve and improve its dispersiveness in water and organic solvent, and then provide a kind of prepare simple, reaction conditions is gentle, be easy to manipulation system and the preparation method of finely dispersed modified graphene-polyvinyl alcohol compound film.
To achieve these goals, the technical solution used in the present invention is as follows:
A preparation method for modified graphene-polyvinyl alcohol compound film, is characterized in that, comprises the steps:
1) preparation of modified graphene: first by graphene oxide dispersion in deionized water, ultrasonic vibration stirs 0.5-12h at normal temperatures, obtains graphene oxide-aqueous dispersions that concentration is 0.01-2.0mg/mL; Hymecromone is joined in this graphene oxide-aqueous dispersions again, at 20-60 DEG C, stir 0.1-6h; Then add basic solution, stir 0.1-6h, and adjust ph is to 9-10; Add chemical reducing agent again, at 60-95 DEG C, react 12-96h obtain modification mixed solution; This modification mixed solution suction filtration is obtained solid matter, then uses the solid matter described in ethanol and deionized water wash to neutral successively; Under being placed on air or vacuum environment, being dried to constant weight in 40-70 DEG C, namely obtaining modified graphene.
2) prepare the dispersion liquid of modified graphene: modified graphene step 1) obtained joins in solvent as solute, stir 0.5-6h, then ultrasonic vibration 0.5-10h, obtain the dispersion liquid that concentration is the modified graphene of 0.01-2.0mg/mL.
3) prepare film: be dissolved in deionized water by polyvinyl alcohol at 20-95 DEG C, obtain the polyvinyl alcohol water solution that mass concentration is 1%-10%; By step 2) dispersion liquid of modified graphene that obtains joins in above-mentioned polyvinyl alcohol water solution, and stir 0.1-5h, then use ultrasonic vibration 0.5-12h, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution.By above-mentioned modified graphene-polyvinyl alcohol mixing solution is poured in vessel, under air or vacuum environment, at 40-70 DEG C, be dried to constant weight, obtain modified graphene-polyvinyl alcohol compound film; Wherein, the massfraction of modified graphene is 0.1%-10%.
Further, sodium hydroxide solution or the massfraction of to be concentration the be 0.1-2.0mol/L of the basic solution described in step 1) are the ammonia soln of 25%-28%.
Further, the mass ratio of the graphene oxide described in step 1), Hymecromone, chemical reducing agent is 1:1-20:1-50.
Further, the chemical reducing agent described in step 1) is hydrazine hydrate, vitamins C or glucose.
Further, step 2) described in solvent be deionized water or tetrahydrofuran (THF).
Compared with prior art, the present invention has following beneficial effect:
1, the polymeric matrix that the present invention chooses is polyvinyl alcohol (PVA), and can be prepared by purchase commercially available product or synthesis, material source is extensive, safety non-toxic, chemical stability and good biocompatibility.The common organic solvents such as solubility property is good, soluble in water and dimethyl sulfoxide (DMSO) (DMSO), film forming properties is good, is conducive to processing preparation.
2, the properties-correcting agent that the present invention chooses is Hymecromone, its molecule contains hydroxyl, ester group and conjugated structure etc., can with the interactions such as oxy radical generation hydrogen bond and e-e key such as the carbonyl in graphene oxide and carboxyl, also containing groups such as hydroxyls in the modified graphene obtained by being reduced, interaction of hydrogen bond can be produced with the hydroxyl in polyvinyl alcohol molecule, be conducive to improving and improving the dispersiveness of Graphene in polyvinyl alcohol, strengthen interface binding power.
3, the properties-correcting agent that the present invention chooses is Hymecromone, can be prepared by purchase commercially available product or synthesis, and material is easy to obtain, and solubility property is good, and chemical stability is good, and cost is low.
4, the chemical reducing agent chosen of the present invention, can by buying commercially available product or synthesis prepare, and material is easy to obtain, and solubility property is good, and chemical stability is good, cheap.
5, the preparation method of a kind of modified graphene/polyvinyl alcohol compound film of the present invention, can be regulated the quality of polyvinyl alcohol thermal characteristics etc. by the addition controlling modified graphene, the laminated film prepared is uniformly dispersed, stable performance.
6, this preparation method is simple, and mild condition, is easy to operate and control.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Polyvinyl alcohol used in the present invention (PVA) is by a kind of polymkeric substance of Vinyl Acetate Copolymer Ester hydrolysis, can be prepared by purchase commercially available product or synthesis.The organic solvents such as its solubility property is good, soluble in water and dimethyl sulfoxide (DMSO) (DMSO), film forming properties is good, is convenient to processing preparation.
Properties-correcting agent that the present invention utilizes, i.e. Hymecromone, come grapheme modified, thus improve the dispersiveness of Graphene in water and organic solvent.Wherein, properties-correcting agent, i.e. Hymecromone, Chinese another name is tonka bean camphor 4, and its molecular structural formula is as follows:
It can be prepared by purchase commercially available product or synthesis, and chemical stability is good, and solubility property is good.
Raw material of the present invention---graphene oxide can be prepared by purchase commercially available product or synthesis.
one, a kind of preparation method of modified graphene-polyvinyl alcohol compound film, comprise the steps:
1) preparation of modified graphene: first by graphene oxide dispersion in deionized water, ultrasonic vibration stirs 0.5-12h at normal temperatures, obtains graphene oxide-aqueous dispersions that concentration is 0.01-2.0mg/mL; Hymecromone is joined in this graphene oxide-aqueous dispersions again, at 20-60 DEG C, stir 0.1-6h; Then add basic solution, stir 0.1-6h, and adjust ph is to 9-10; Add chemical reducing agent again, at 60-95 DEG C, react 12-96h obtain modification mixed solution; This modification mixed solution suction filtration is obtained solid matter, then uses the solid matter described in ethanol and deionized water wash to neutral successively; Under being placed on air or vacuum environment, being dried to constant weight in 40-70 DEG C, namely obtaining modified graphene.
The operation of this step adopts the method for adding properties-correcting agent and chemical reduction graphene oxide to prepare modified graphene.In described graphene oxide, Hymecromone, chemical reducing agent, Hymecromone, chemical reducing agent answer excessive use, react and remove excessive properties-correcting agent and chemical reducing agent with by washing operation.
2) prepare the dispersion liquid of modified graphene: modified graphene step 1) obtained joins in solvent as solute, stir 0.5-6h, then ultrasonic vibration 0.5-10h, obtain the dispersion liquid that concentration is the modified graphene of 0.01-2.0mg/mL.
3) prepare film: be dissolved in deionized water by polyvinyl alcohol at 20-95 DEG C, obtain the polyvinyl alcohol water solution that mass concentration is 1%-10%; By step 2) dispersion liquid of modified graphene that obtains joins in above-mentioned polyvinyl alcohol water solution, and stir 0.1-5h, then use ultrasonic vibration 0.5-12h, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution; By above-mentioned modified graphene-polyvinyl alcohol mixing solution is poured in vessel, under air or vacuum environment, at 40-70 DEG C, be dried to constant weight, obtain modified graphene-polyvinyl alcohol compound film; Wherein, the massfraction of modified graphene is 0.1%-10%.
The operation of this step adopts solution blended process to prepare modified graphene-polyvinyl alcohol compound film.
Wherein, sodium hydroxide solution or the massfraction of to be concentration the be 0.1-2.0mol/L of the basic solution described in step 1) are the ammonia soln of 25%-28%; Described chemical reducing agent is hydrazine hydrate, vitamins C or glucose.
The mass ratio of the graphene oxide described in step 1), Hymecromone, chemical reducing agent is 1:1-20:1-50.This ratio is a kind of prioritization scheme, and the effect of preparation is best.
Step 2) described in solvent be deionized water or tetrahydrofuran (THF).
Hymecromone selected by properties-correcting agent of the present invention, and the present invention selects hydrazine hydrate, the chemical reducing agent such as vitamins C or glucose; First prepare modified graphene, then prepare the dispersion liquid of modified graphene, then the dispersion liquid of modified graphene is joined in polyvinyl alcohol water solution, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution; Finally above-mentioned mixing solutions is poured in vessel, under air or vacuum environment, be dried to constant weight in 40-70 degree Celsius, obtain modified graphene/polyvinyl alcohol compound film.Wherein, the massfraction of modified graphene is 0.1%-10%.
two, embodiment
embodiment 1
Adopt and prepare modified graphene-polyvinyl alcohol compound film with the following method:
1) preparation of modified graphene: first by graphene oxide dispersion in deionized water, ultrasonic vibration stirs 1h at normal temperatures, obtains graphene oxide-aqueous dispersions that concentration is 0.05mg/mL;
Hymecromone is joined in this graphene oxide-aqueous dispersions again, at 25 DEG C, stir 2h; Then add the aqueous sodium hydroxide solution that concentration is 1.0mol/L, stir 0.5h, and adjust ph is 9-10; Add chemical reducing agent hydrazine hydrate again, at 80 DEG C, react 48h obtain modification mixed solution;
This modification mixed solution suction filtration is obtained solid matter, then uses the solid matter described in ethanol and deionized water wash to neutral successively; Under being placed on atmospheric environment, being dried to constant weight in 50 DEG C, namely obtaining modified graphene;
The mass ratio of described graphene oxide, Hymecromone, hydrazine hydrate is 1:5:10;
2) prepare the dispersion liquid of modified graphene: modified graphene step 1) obtained joins in tetrahydrofuran (THF) as solute, stir 1h, then ultrasonic vibration 8h, obtain the dispersion liquid that concentration is the modified graphene of 0.05mg/mL;
3) prepare film: be dissolved in deionized water by polyvinyl alcohol at 80 DEG C, obtain the polyvinyl alcohol water solution that mass concentration is 5%; By step 2) dispersion liquid of modified graphene that obtains joins in above-mentioned polyvinyl alcohol water solution, and stir 1h, then use ultrasonic vibration 5h, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution;
By above-mentioned modified graphene-polyvinyl alcohol mixing solution is poured in vessel, under vacuum conditions, at 50 DEG C, be dried to constant weight, obtain modified graphene-polyvinyl alcohol compound film; Wherein, the massfraction of modified graphene is 0.3%.
embodiment 2
Adopt and prepare modified graphene-polyvinyl alcohol compound film with the following method:
1) preparation of modified graphene: first by graphene oxide dispersion in deionized water, ultrasonic vibration stirs 3h at normal temperatures, obtains graphene oxide-aqueous dispersions that concentration is 0.1mg/mL;
Hymecromone is joined in this graphene oxide-aqueous dispersions again, at 30 DEG C, stir 1h; Then add the aqueous sodium hydroxide solution that concentration is 2.0mol/L, stir 1h, and adjust ph is 9-10; Add chemical reducing agent vitamins C again, at 90 DEG C, react 32h obtain modification mixed solution;
This modification mixed solution suction filtration is obtained solid matter, then uses the solid matter described in ethanol and deionized water wash to neutral successively; Under being placed on atmospheric environment, being dried to constant weight in 60 DEG C, namely obtaining modified graphene;
Described graphene oxide, Hymecromone, ascorbic mass ratio are 1:10:20;
2) prepare the dispersion liquid of modified graphene: modified graphene step 1) obtained joins in tetrahydrofuran (THF) as solute, stir 3h, then ultrasonic vibration 6h, obtain the dispersion liquid that concentration is the modified graphene of 0.1mg/mL;
3) prepare film: be dissolved in deionized water by polyvinyl alcohol at 85 DEG C, obtain the polyvinyl alcohol water solution that mass concentration is 3%; By step 2) dispersion liquid of modified graphene that obtains joins in above-mentioned polyvinyl alcohol water solution, and stir 2h, then use ultrasonic vibration 8h, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution;
By above-mentioned modified graphene-polyvinyl alcohol mixing solution is poured in vessel, under atmospheric environment, at 55 DEG C, be dried to constant weight, obtain modified graphene-polyvinyl alcohol compound film; Wherein, the massfraction of modified graphene is 0.7%.
embodiment 3
Adopt and prepare modified graphene-polyvinyl alcohol compound film with the following method:
1) preparation of modified graphene: first by graphene oxide dispersion in deionized water, ultrasonic vibration stirs 5h at normal temperatures, obtains graphene oxide-aqueous dispersions that concentration is 0.5mg/mL;
Hymecromone is joined in this graphene oxide-aqueous dispersions again, at 40 DEG C, stir 0.5h; Then add the ammonia soln that massfraction is 25%-28%, stir 2h, and adjust ph is 9-10; Add chemical reducing agent glucose again, at 95 DEG C, react 18h obtain modification mixed solution;
This modification mixed solution suction filtration is obtained solid matter, then uses the solid matter described in ethanol and deionized water wash to neutral successively; Place under vacuum conditions, be dried to constant weight in 65 DEG C, namely obtain modified graphene;
The mass ratio of described graphene oxide, Hymecromone, glucose is 1:20:50;
2) prepare the dispersion liquid of modified graphene: modified graphene step 1) obtained joins in deionized water as solute, stir 5h, then ultrasonic vibration 10h, obtain the dispersion liquid that concentration is the modified graphene of 0.5mg/mL;
3) prepare film: be dissolved in deionized water by polyvinyl alcohol at 90 DEG C, obtain the polyvinyl alcohol water solution that mass concentration is 6%; By step 2) dispersion liquid of modified graphene that obtains joins in above-mentioned polyvinyl alcohol water solution, and stir 3h, then use ultrasonic vibration 10h, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution;
By above-mentioned modified graphene-polyvinyl alcohol mixing solution is poured in vessel, under vacuum conditions, at 60 DEG C, be dried to constant weight, obtain modified graphene-polyvinyl alcohol compound film; Wherein, the massfraction of modified graphene is 1.5%.
Postmenstruation, test proved, the thermal weight loss temperature of the modified graphene-polyvinyl alcohol compound film of different mass mark is different, refers to table 1:
the thermal weight loss temperature of the modified graphene-polyvinyl alcohol compound film of table 1 different mass mark
The above embodiment of the present invention is only for example of the present invention is described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (5)
1. a preparation method for modified graphene-polyvinyl alcohol compound film, is characterized in that, comprises the steps:
1) preparation of modified graphene: first by graphene oxide dispersion in deionized water, ultrasonic vibration stirs 0.5-12h at normal temperatures, obtains graphene oxide-aqueous dispersions that concentration is 0.01-2.0mg/mL;
Hymecromone is joined in this graphene oxide-aqueous dispersions again, at 20-60 DEG C, stir 0.1-6h; Then add basic solution, stir 0.1-6h, and adjust ph is to 9-10; Add chemical reducing agent again, at 60-95 DEG C, react 12-96h obtain modification mixed solution;
This modification mixed solution suction filtration is obtained solid matter, then uses the solid matter described in ethanol and deionized water wash to neutral successively; Under being placed on air or vacuum environment, being dried to constant weight in 40-70 DEG C, namely obtaining modified graphene;
2) prepare the dispersion liquid of modified graphene: modified graphene step 1) obtained joins in solvent as solute, stir 0.5-6h, then ultrasonic vibration 0.5-10h, obtain the dispersion liquid that concentration is the modified graphene of 0.01-2.0mg/mL;
3) prepare film: be dissolved in deionized water by polyvinyl alcohol at 20-95 DEG C, obtain the polyvinyl alcohol water solution that mass concentration is 1%-10%; By step 2) dispersion liquid of modified graphene that obtains joins in above-mentioned polyvinyl alcohol water solution, and stir 0.1-5h, then use ultrasonic vibration 0.5-12h, obtain finely dispersed modified graphene-polyvinyl alcohol mixing solution;
By above-mentioned modified graphene-polyvinyl alcohol mixing solution is poured in vessel, under air or vacuum environment, at 40-70 DEG C, be dried to constant weight, obtain modified graphene-polyvinyl alcohol compound film; Wherein, the massfraction of modified graphene is 0.1%-10%.
2. the preparation method of modified graphene-polyvinyl alcohol compound film according to claim 1, is characterized in that, sodium hydroxide solution or the massfraction of to be concentration the be 0.1-2.0mol/L of the basic solution described in step 1) are the ammonia soln of 25%-28%.
3. the preparation method of modified graphene-polyvinyl alcohol compound film according to claim 1, is characterized in that, the mass ratio of the graphene oxide described in step 1), Hymecromone, chemical reducing agent is 1:1-20:1-50.
4. the preparation method of the modified graphene-polyvinyl alcohol compound film according to claim 1 or 2 or 3, is characterized in that, the chemical reducing agent described in step 1) is hydrazine hydrate, vitamins C or glucose.
5. the preparation method of modified graphene-polyvinyl alcohol compound film according to claim 1, is characterized in that, step 2) described in solvent be deionized water or tetrahydrofuran (THF).
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| CN106046523A (en) * | 2016-07-21 | 2016-10-26 | 合肥市智源包装科技有限公司 | Modified graphene-polyethylene film material for toothpaste sheeting and preparation method thereof |
| CN106000319B (en) * | 2016-08-03 | 2018-06-08 | 四川理工学院 | Remove the sorbing material of trace arsenic and its minimizing technology to trace arsenic in water body in water body |
| CN106000319A (en) * | 2016-08-03 | 2016-10-12 | 四川理工学院 | Adsorption material for removal of trace arsenic from water and method for removal of trace arsenic from water therewith |
| CN106936065A (en) * | 2017-04-27 | 2017-07-07 | 西安石油大学 | Carboxylated graphene oxide saturable absorber device and preparation method thereof and its application in optical fiber laser |
| CN107586426A (en) * | 2017-10-21 | 2018-01-16 | 马小良 | A kind of preparation method of stable dispersion type molybdenum disulfide polyvinyl alcohol composite material |
| CN108610591A (en) * | 2018-04-26 | 2018-10-02 | 武汉工程大学 | A kind of graphene/polyvinyl alcohol coextruded elastic film and preparation method thereof |
| CN108610591B (en) * | 2018-04-26 | 2021-06-01 | 武汉工程大学 | Graphene/polyvinyl alcohol composite elastic film and preparation method thereof |
| CN108641107A (en) * | 2018-08-08 | 2018-10-12 | 苏州傅里烨新材料科技有限公司 | A kind of graphene composite material film and preparation method thereof |
| CN113921814A (en) * | 2021-09-30 | 2022-01-11 | 云南中晟新材料有限责任公司 | Production process of brightener modified lithium ion battery graphite negative electrode material |
| CN113921814B (en) * | 2021-09-30 | 2023-09-05 | 云南中晟新材料有限责任公司 | Production process of brightening agent modified lithium ion battery graphite anode material |
| CN114540812A (en) * | 2022-01-26 | 2022-05-27 | 山东大学 | Method for preparing reduced graphene film on metal surface |
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Effective date of registration: 20210611 Address after: Room 801, 85 Kefeng Road, Huangpu District, Guangzhou City, Guangdong Province Patentee after: Yami Technology (Guangzhou) Co.,Ltd. Address before: No. 69 lijiatuo Chongqing District of Banan City Road 400054 red Patentee before: Chongqing University of Technology |
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Effective date of registration: 20220805 Address after: 528000 No. 05 (F1) 2, North District, "National Torch Program Foshan Electronic and Electrical Industry Base", Baini Town, Sanshui District, Foshan City, Guangdong Province (Residence declaration) Patentee after: Foshan Yueyuancheng Packaging Products Co., Ltd. Address before: Room 801, 85 Kefeng Road, Huangpu District, Guangzhou City, Guangdong Province Patentee before: Yami Technology (Guangzhou) Co.,Ltd. |