CN101381524A - Mono-layer graphite oxide and water-soluble high molecule reinforced compound material - Google Patents
Mono-layer graphite oxide and water-soluble high molecule reinforced compound material Download PDFInfo
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- CN101381524A CN101381524A CNA2008101524691A CN200810152469A CN101381524A CN 101381524 A CN101381524 A CN 101381524A CN A2008101524691 A CNA2008101524691 A CN A2008101524691A CN 200810152469 A CN200810152469 A CN 200810152469A CN 101381524 A CN101381524 A CN 101381524A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
- C08J3/215—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase at least one additive being also premixed with a liquid phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
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- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/02—Polyamines
Abstract
The invention relates to a monolayer graphite oxide and water-soluble polymer reinforced composite material and a preparation method thereof. The preparation method comprises a concrete step of filling a water-soluble polymer matrix with monolayer graphite oxide material, wherein the weight proportion is 0.1 to 20 percent of the monolayer graphite oxide and 99.9 to 80 percent of the water-soluble polymer matrix material. The preparation method is characterized by utilizing the excellent mechanical properties, large length-diameter ratio and good water dispersity of the monolayer graphite oxide to prepare the reinforced water-soluble polymer composite material. As a solvent used in the process of preparing the composite material is mainly water, the preparation method is friendly to environment, simple in process and easy to popularize and apply.
Description
Technical field
The present invention relates to the preparation of functional composite material, particularly a kind of mono-layer graphite oxide and water-soluble high molecule reinforced compound material and preparation method thereof.
Background technology
Compare with traditional packing material, nano material makes its needs addition seldom just can improve a lot to the performance of polymer composites because the many of himself are had a few.And this more than ten years recently, because the very outstanding performance of carbon nanotube utilizes it to obtain paying attention to very widely as the performance that the carbon-based nano strongthener improves polymer composites.Yet, because some shortcomings that are very difficult to overcome of carbon nanotube self, a lot of as impurity in the resulting product of method of mass preparation carbon nanotube (especially Single Walled Carbon Nanotube), easily assemble be difficult to disperse, preparation cost height or the like, make it but be subjected to very big restriction at practical application technical.
Recently, because its excellent performance, the appearance of mono-layer graphite has caused a lot of people's concern.Theoretical and experimental data shows the mechanical property of the mono-layer graphite that the complete unit molecule of a slice is thick even has surpassed single complete carbon nanotube.The mono-layer graphite oxide material is the mono-layer graphite that has connected some oxygen-containing functional groups (as hydroxyl, carboxyl, carbonyl and epoxy group(ing) etc.) on the graphite flake.Because it is well water-soluble that the existence of these oxygen-containing functional groups makes that the mono-layer graphite oxide material has.These advantages make mono-layer graphite oxide can strengthen matrix material in the water-soluble polymer.
Water-soluble high-molecular material is a kind of hydrophilic macromolecular material, can dissolving in water or swelling and form solution or dispersion liquid.It has advantages such as excellent performance, easy to use, enabling environment protection, is widely used in the every field of national economy.With the polyvinyl alcohol is example; because polyvinyl alcohol has unique powerful cementability, epithelium snappiness, smoothness, oil-proofness, solvent resistance, protective colloid, gas barrier performance, wear resistance and the water tolerance that has through special processing; therefore be used to produce products such as coating, tackiness agent, paper product machining agent, emulsifying agent, dispersion agent, film in a large number, range of application spreads all over a large amount of industries.Therefore, water-soluble high-molecular material is carried out the important subject that filling enhancing modified has become this field.
Summary of the invention
Purpose of the present invention provides a kind of mono-layer graphite oxide and water-soluble high molecule reinforced compound material and preparation method thereof.Because the mono-layer graphite oxide material has good water dispersible, excellent mechanical property, big length-to-diameter ratio and specific surface area, and also contain relatively large oxygen-containing functional group on this mono-layer graphite oxide material, therefore the mono-layer graphite oxide material is filled into the matrix material that can expect in the water-soluble polymer that the acquisition mechanical property is enhanced.This matrix material low price, environmental protection, complete processing is simple.
The invention provides a kind of mono-layer graphite oxide and water-soluble high molecule reinforced compound material and be with mono-layer graphite and body material water-soluble polymer is feedstock production, its weight proportion is: mono-layer graphite oxide 0.1-20%, water-soluble polymer body material 80-99.9%.
Concrete preparation method: the aqueous dispersions thorough mixing that obtains oxidation mono-layer graphite aqueous dispersions and water-soluble polymer through ultrasonication, stir 20-30min, ultrasonic again 0.5-2h, the mono-layer graphite oxide material obtains homodisperse in the water-soluble polymer matrix, aqueous solution volatilization back obtains mono-layer graphite oxide and water-soluble high molecule reinforced compound material.By typical thin films preparation methods such as spraying, spin coating and casting, make aqueous solution volatilization back obtain mono-layer graphite oxide and water-soluble polymer enhancing composite film material.
Described mono-layer graphite oxide material is meant that its molecular skeleton is made up of the mono-layer graphite atom of sexangle lattice arrangement, contains the two dimensional surface material that a large amount of organic oxygen-containing functional group comprises carboxyl, hydroxyl, epoxy group(ing), carbonyl etc., and monolithic area size is at 100nm
2To 400 μ m
2Between, single-sheet thickness is between 0.3 to 2nm, and this material can adopt method preparations such as mechanically peel method, crystal epitaxy method and chemical oxidation.This mono-layer graphite oxide material can well be distributed in the aqueous solution of water and water-soluble polymer.
Described water-soluble polymer matrix is meant in water can dissolving or swelling and form the polymer of solution or dispersion liquid, polyvinyl alcohol is preferably arranged, polymine, polyacrylic acid, sodium polystyrene sulfonate, polyacrylamide, polyoxyethylene; Molecular weight is 2-12 ten thousand.
The preparation method of mono-layer graphite oxide provided by the invention and water-soluble high molecule reinforced compound material may further comprise the steps:
1). the mono-layer graphite oxide material is added in the water,, makes the mono-layer graphite oxide dispersion of materials in water, get the mono-layer graphite oxide dispersion soln, water-soluble polymer is distributed to gets the water-soluble polymer dispersion soln in the water simultaneously through supersound process 20-100min.
2) two kinds of solution of step 1) are mixed, stir 20-30min, use ultrasonication 0.5-2h again, make the mono-layer graphite oxide material in the water-soluble polymer matrix, obtain homodisperse.Aqueous solution volatilization back obtains mono-layer graphite oxide and water-soluble high molecule reinforced compound material; By typical thin films preparation methods such as spraying, spin coating and casting, make aqueous solution volatilization back obtain mono-layer graphite oxide and water-soluble polymer enhanced film material.
The mechanical property of this mono-layer graphite oxide and water-soluble polymer matrix material has the raising of 10-100%.With mono-layer graphite oxide/polyvinyl alcohol composite material is example, and when the content of mono-layer graphite oxide material was 0.7wt (weight) %, its Young's modulus improved above 60%, and tensile strength increases above 70%.And, the experimental value of the Young's modulus of mono-layer graphite oxide/polyvinyl alcohol high performance composite with mate very much with Halpin-Tsai formula mimic calculated value, having illustrated between mono-layer graphite oxide and the polyvinyl alcohol matrix has very strong interaction.
The distinguishing feature of mono-layer graphite oxide of the present invention and water-soluble high molecule reinforced compound material is:
1, the mono-layer graphite oxide material has excellent mechanical property, big length-to-diameter ratio and specific surface area are big, the characteristics of good dispersity etc. are implemented in the homodisperse in the water-soluble polymer body material easily in the aqueous solution, can obtain the mechanical property of bigger raising under the low situation of content.
2,, thereby greatly reduce the cost of material because the addition of an a spot of mono-layer graphite oxide material of needs just can make the mechanical property of matrix material be greatly improved.
3, because the solvent that uses in the preparation process of mono-layer graphite oxide and water-soluble polymer matrix material mainly all is a water, both environmental protection, technology has fairly simple, is easy to apply.
Description of drawings
The stress-strain curve of the mono-layer graphite oxide/polyvinyl alcohol composite material of Fig. 1, different mono-layer graphite oxide material contents.
The Young's modulus curve of the mono-layer graphite oxide/polyvinyl alcohol composite material of Fig. 2, different mono-layer graphite oxide material contents and with the curve of Halpin-Tsai formula mimic calculated value.
Embodiment
Below by embodiment the present invention is specifically described; present embodiment only is used for the present invention is further detailed; can not be interpreted as limiting the scope of the invention; those skilled in the art makes some nonessential improvement and adjustment according to above-mentioned content, all belongs to protection domain of the present invention.
Embodiment 1:
The preparation of mono-layer graphite oxide material
The reference literature reported method prepare the mono-layer graphite oxide material (Carbon, 2204,42,2929-2937).The a large amount of organic oxygen-containing functional group contained of the mono-layer graphite oxide material of Shi Yonging comprises carboxyl, hydroxyl, epoxy group(ing), carbonyl etc., monolithic area size average out to 6 μ m in this example
2, single-sheet thickness average out to 0.8nm (following examples are identical).
The preparation of mono-layer graphite oxide/polyvinyl alcohol composite material of 0.3wt%
In 6ml distilled water and ultrasonic half an hour, the mono-layer graphite oxide material is dispersed in the aqueous solution uniformly and stably in this process with 3mg mono-layer graphite oxide material dissolves.Under 90 ℃, 1g polyvinyl alcohol (molecular weight: 3-5 ten thousand, alcoholysis degree: 86-89% purchase in Alpha Co., Ltd, and following examples are identical) is dissolved in the 14ml distilled water, after treating to dissolve fully polyvinyl alcohol solution is cooled to 40 ℃.Then the scattered mono-layer graphite oxide aqueous solution is added drop-wise in the polyvinyl alcohol solution.After mixing solutions continued ultrasonic half an hour, cast in film forming on the poly-tetrafluoro substrate, and do not change basically to quality at 60 ℃ of following vacuum bakeouts and to get final product.
Mono-layer graphite oxide/PVA (PVOH) FILM of 0.3wt% has improved 36% than the tensile strength of pure PVA (PVOH) FILM, and Young's modulus has improved 18%.
Embodiment 2:
The preparation of mono-layer graphite oxide/polyvinyl alcohol composite material of 0.5wt%
In 6ml distilled water and ultrasonic half an hour, the mono-layer graphite oxide material is dispersed in the aqueous solution uniformly and stably in this process with 5mg mono-layer graphite oxide material dissolves.Under 90 ℃, the 1g polyvinyl alcohol is dissolved in the 14ml distilled water, after treating to dissolve fully polyvinyl alcohol solution is cooled to 40 ℃.Then the scattered mono-layer graphite oxide aqueous solution is added drop-wise in the polyvinyl alcohol solution.After mixing solutions continued ultrasonic half an hour, cast in film forming on the poly-tetrafluoro substrate, and do not change basically to quality at 60 ℃ of following vacuum bakeouts and to get final product.
Mono-layer graphite oxide/PVA (PVOH) FILM of 0.5wt% has improved 47% than the tensile strength of pure PVA (PVOH) FILM, and Young's modulus has improved 35%.
Embodiment 3:
The preparation of mono-layer graphite oxide/polyvinyl alcohol composite material of 0.7wt%
In 6ml distilled water and ultrasonic half an hour, the mono-layer graphite oxide material is dispersed in the aqueous solution uniformly and stably in this process with 7mg mono-layer graphite oxide material dissolves.Under 90 ℃, the 1g polyvinyl alcohol is dissolved in the 14ml distilled water, after treating to dissolve fully polyvinyl alcohol solution is cooled to 40 ℃.Then the scattered mono-layer graphite oxide aqueous solution is added drop-wise in the polyvinyl alcohol solution.After mixing solutions continued ultrasonic half an hour, cast in film forming on the poly-tetrafluoro substrate, and do not change basically to quality at 60 ℃ of following vacuum bakeouts and to get final product.
Mono-layer graphite oxide/PVA (PVOH) FILM of 0.7wt% has improved 76% than the tensile strength of pure PVA (PVOH) FILM, and Young's modulus has improved 62%.
As can be seen from Figure 1, increase along with mono-layer graphite oxide content, the physical strength of mono-layer graphite oxide/polyvinyl alcohol composite material constantly increase and reach maximum value during for 0.7wt% at content, illustrate that mono-layer graphite oxide has played good enhancement to the mechanical property of polyvinyl alcohol matrix, is highly suitable for strengthening this water-soluble polymer body material.
Claims (8)
1, a kind of mono-layer graphite oxide and water-soluble high molecule reinforced compound material, it is characterized in that it is is feedstock production with mono-layer graphite and body material water-soluble polymer, its weight proportion is: mono-layer graphite oxide 0.1-20%, water-soluble polymer body material 80-99.9%;
Concrete preparation method: the aqueous dispersions thorough mixing that obtains oxidation mono-layer graphite aqueous dispersions and water-soluble polymer through ultrasonication, stir 20-30min, ultrasonic again 0.5-2h, the mono-layer graphite oxide material obtains homodisperse liquid in the water-soluble polymer matrix, aqueous solution volatilization back obtains mono-layer graphite oxide and water-soluble high molecule reinforced compound material.
2, matrix material according to claim 1, it is characterized in that described mono-layer graphite oxide material is meant that its molecular skeleton is made up of the mono-layer graphite atom of sexangle lattice arrangement, contain the two dimensional surface material that a large amount of organic oxygen-containing functional group comprises carboxyl, hydroxyl, epoxy group(ing), carbonyl etc., monolithic area size is at 100nm
2To 400 μ m
2Between, single-sheet thickness is between 0.3 to 2nm.
3, matrix material according to claim 1, it is characterized in that described matrix water-soluble polymer matrix is meant in water can dissolving or swelling and form the polymer of solution or dispersion liquid.
4, matrix material according to claim 3 is characterized in that described matrix water-soluble polymer matrix is polyvinyl alcohol, polymine, polyacrylic acid, sodium polystyrene sulfonate, polyacrylamide or polyoxyethylene.
5, according to claim 1 or 4 described matrix materials, it is characterized in that described water-soluble polymer matrix is a polyvinyl alcohol, molecular weight is 2-12 ten thousand, alcoholysis degree is 70-90%.
6, the preparation method of the described matrix material of claim 1 is characterized in that may further comprise the steps:
1). the mono-layer graphite oxide material is added in the water,, makes the mono-layer graphite oxide dispersion of materials in water, get the mono-layer graphite oxide dispersion soln, water-soluble polymer is distributed to gets the water-soluble polymer dispersion soln in the water simultaneously through supersound process 20-100min;
2) two kinds of solution of step 1) are mixed, stir 20-30min, use ultrasonication 0.5-2h again, make the mono-layer graphite oxide material obtain homodisperse solution in the water-soluble polymer matrix, aqueous solution volatilization back obtains mono-layer graphite oxide and water-soluble polymer strengthens.
7, the preparation method of matrix material according to claim 6 is characterized in that described water-soluble polymer matrix is a polyvinyl alcohol.
8, the preparation method of matrix material according to claim 6, it is characterized in that step 2) preparation method of described dispersion soln by spraying, spin coating and casting film, make aqueous solution volatilization back obtain mono-layer graphite oxide and water-soluble polymer enhanced film matrix material.
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| CNA2008101524691A CN101381524A (en) | 2008-10-24 | 2008-10-24 | Mono-layer graphite oxide and water-soluble high molecule reinforced compound material |
| PCT/CN2009/074622 WO2010045889A1 (en) | 2008-10-24 | 2009-10-26 | Polymer reinforced composite |
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Cited By (7)
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| WO2010045889A1 (en) * | 2008-10-24 | 2010-04-29 | 南开大学 | Polymer reinforced composite |
| CN102115566A (en) * | 2011-01-06 | 2011-07-06 | 西安理工大学 | Preparation method for graphene oxide with high barrier property and polymer nanocomposite film |
| CN102357356A (en) * | 2011-09-13 | 2012-02-22 | 中山大学 | Preparation method and application of azo dye adsorbent |
| CN102492296A (en) * | 2011-11-25 | 2012-06-13 | 江南大学 | Synthesis method of water dispersible polyaniline/graphene composite material |
| CN103194055A (en) * | 2013-04-18 | 2013-07-10 | 中国科学技术大学 | Material for regulating humidity and preparation method and application thereof |
| CN109238522A (en) * | 2018-09-21 | 2019-01-18 | 南开大学 | A kind of wearable flexibility stress sensor and its preparation method and application |
| CN109778591A (en) * | 2019-01-11 | 2019-05-21 | 浙江理工大学 | A kind of hydrophilic flexibility graphite composite seal preparation method |
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| US7745528B2 (en) * | 2006-10-06 | 2010-06-29 | The Trustees Of Princeton University | Functional graphene-rubber nanocomposites |
| CN101381524A (en) * | 2008-10-24 | 2009-03-11 | 南开大学 | Mono-layer graphite oxide and water-soluble high molecule reinforced compound material |
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2008
- 2008-10-24 CN CNA2008101524691A patent/CN101381524A/en active Pending
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| WO2010045889A1 (en) * | 2008-10-24 | 2010-04-29 | 南开大学 | Polymer reinforced composite |
| CN102115566A (en) * | 2011-01-06 | 2011-07-06 | 西安理工大学 | Preparation method for graphene oxide with high barrier property and polymer nanocomposite film |
| CN102357356A (en) * | 2011-09-13 | 2012-02-22 | 中山大学 | Preparation method and application of azo dye adsorbent |
| CN102357356B (en) * | 2011-09-13 | 2013-02-06 | 中山大学 | Preparation method of azo dye adsorbent |
| CN102492296A (en) * | 2011-11-25 | 2012-06-13 | 江南大学 | Synthesis method of water dispersible polyaniline/graphene composite material |
| CN102492296B (en) * | 2011-11-25 | 2014-02-12 | 江南大学 | Synthesis method of water dispersible polyaniline/graphene composite material |
| CN103194055A (en) * | 2013-04-18 | 2013-07-10 | 中国科学技术大学 | Material for regulating humidity and preparation method and application thereof |
| CN103194055B (en) * | 2013-04-18 | 2015-06-17 | 中国科学技术大学 | Material for regulating humidity and preparation method and application thereof |
| CN109238522A (en) * | 2018-09-21 | 2019-01-18 | 南开大学 | A kind of wearable flexibility stress sensor and its preparation method and application |
| CN109778591A (en) * | 2019-01-11 | 2019-05-21 | 浙江理工大学 | A kind of hydrophilic flexibility graphite composite seal preparation method |
| CN109778591B (en) * | 2019-01-11 | 2021-07-09 | 浙江理工大学 | Preparation method of hydrophilic flexible graphite composite sealing material |
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