CN101381511A - Mono-layer graphite and polymer compound material and preparation and application thereof - Google Patents
Mono-layer graphite and polymer compound material and preparation and application thereof Download PDFInfo
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- CN101381511A CN101381511A CNA2008101524668A CN200810152466A CN101381511A CN 101381511 A CN101381511 A CN 101381511A CN A2008101524668 A CNA2008101524668 A CN A2008101524668A CN 200810152466 A CN200810152466 A CN 200810152466A CN 101381511 A CN101381511 A CN 101381511A
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The invention relates to a composite material of monolayer graphite and polymers, as well as a preparation method thereof. The composite material takes the monolayer graphite and the polymers as raw materials which are well mixed, wherein the weight portions of the raw materials are: 0.1 to 100 portions of the monolayer graphite and 0.1 to 100 portions of the polymers or other matrix materials. The preparation method is characterized by utilizing the excellent conductivity and large length-diameter ratio of the monolayer graphite to prepare conducting composite materials. Micro analysis proves that the monolayer graphite evenly disperses in the matrix materials, and a conducting network can be formed only by adding a small amount of the monolayer graphite, so as to obtain the conducting composite material with a plurality of forms. The composite material simultaneously has high strength and modulus, and is used in building, mechanical, aerospace and other special environments. In addition, as the monolayer graphite has excellent heat-conducting property, the composite material has the advantages of heat dissipation convenience and the like, and is expected to be applied to the precision instrument, microelectronic and other fields.
Description
Technical field
The present invention relates to the manufacturing of functional composite material, particularly a kind of mono-layer graphite and polymer composites and preparation method thereof.
Background technology
First synthesizing polymeric material-phenoplast in the world appearred in 1907.Because polymer materials has advantages such as cheap, good combination property, light weight, forming process are good, obtains large-scale promotion application in numerous fields such as electronics, machinery, building, clothes and national defence, military projects.The output of whole world polymer materials is by volume calculated and is surpassed metallic substance, becomes one of description of materials that is most widely used in the world.
The resistance of most polymers material is all very high, and (volume specific resistance can reach 10
12-10
18Ω cm), easily because of friction produces static, bring out electromagnetic interference even set off an explosion.Therefore, people add the conductive filler material of metal and metal oxide in polymeric matrix, to obtain conduction and antistatic effect preferably.But metallic substance have density greatly, shortcoming such as not corrosion-resistant, forming process difference, and can reduce the mechanical property of polymer composites.In recent years, it is found that interpolation novel nano carbon material can improve the conductivity of polymkeric substance greatly.When Coleman etc. replace the carbon nanotube of adding 7～11% in the poly-phenylene vinylene (ppv) (PMPV) at a position methoxyl group (Physical Review B, 1998,58:7942), the specific conductivity of matrix material has increased about 8 orders of magnitude.Ounaies etc. are distributed to N with Single Walled Carbon Nanotube, in the dinethylformamide, add diamine then and the dicarboxylic anhydride monomer carries out in-situ polymerization, have made polyimide/carbon nano tube compound material.Only need to add carbon nanotube less than 1%, just can make the specific conductivity of matrix material increase about 10 orders of magnitude (Composites Scienceand Technology, 2003,63:1637), reach the requirement of antistatic material.But the preparation of carbon nanotube and purification ratio be difficulty, the cost height, and reunite easily, be difficult in homodisperse in the polymeric matrix.
Mono-layer graphite (graphene) is a kind of novel two-dimensional nano carbon material of being made up of one deck carbon atom.Discover (Science, 2004,306,666-669) mono-layer graphite has good conductive capability, and its room temperature electronic mobility can reach 10,000cm
2V
-1s
-1, its physical strength surpass at present best Single Walled Carbon Nanotube (Science, 2008,321,385-388), its good quantum hall effect (Quantum Hall Effect) has also obtained proof.Mono-layer graphite is a raw material with the natural graphite, is easy to realize preparation in enormous quantities, low price; And, in water and organic solvent, have good solvability through the later mono-layer graphite of chemistry functional, help its dispersion and forming process in various polymkeric substance.
Summary of the invention
The purpose of this invention is to provide a kind of mono-layer graphite and polymer composites and preparation method thereof, utilize the plurality of advantages of mono-layer graphite, preparation contains the conducing composite material of mono-layer graphite.This matrix material low price, light weight has the solution handlability, and forming process is good, is widely used.
Mono-layer graphite provided by the invention and polymer composites are to be raw material with mono-layer graphite and polymkeric substance, and thorough mixing is made, and its parts by weight are:
0.1～100 part of mono-layer graphite;
0.1～100 part of polymkeric substance or other body material.
Described mono-layer graphite 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 of organo-functional group through functionalization, and single graphite flake area is at 10nm
2To 400 μ m
2Between, single-sheet thickness is between 0.34 to 2nm, and this material can adopt method preparations such as mechanically peel method, crystal epitaxy method and chemical oxidation.Preferably, mono-layer graphite can prepare in enormous quantities by the chemical oxidation method that document (Carbon, 2004,42,2929) provide.
Described mono-layer graphite can contain carboxyl, hydroxyl, epoxy bond, sulfonic group, phenyl isocyanate, thiophene, pyrroles, aniline through functionalization and/or contain the functional groups such as chain alkyl of 6 to 18 carbon at least a.
Described polymkeric substance is selected from least a in urethane, polyacrylic ester, polyester, polymeric amide, ABS, polyethylene, polypropylene, polycarbonate, polyvinyl chloride, Resins, epoxy, polyimide, resol and/or the rubber.Polymericular weight is between 2000-200000.
The preparation method of mono-layer graphite provided by the invention and polymer composites may further comprise the steps:
1) mono-layer graphite is added in entry or the organic solvent,, mono-layer graphite is dispersed or dissolved through ultrasonication 0.5-2 hour; Described organic solvent comprises methyl alcohol, ethanol, Virahol, acetone, ethyl acetate, chloroform, tetracol phenixin, tetrahydrofuran (THF), N, dinethylformamide, dimethyl sulfoxide (DMSO), benzene, toluene, dimethylbenzene, chlorobenzene, dichlorobenzene, trichlorobenzene.
2) polymkeric substance fully is dissolved in the corresponding organic solvent;
3) with step 1) and 2) two kinds of solution mix, and stir 0.5-3 hour, use ultrasonication 0.5-3 hour again, obtain the mother liquor (dispersion soln or suspension) of the matrix material of even, stable mono-layer graphite and polymkeric substance;
The matrix material mother liquor of step 3) is by typical thin films preparation methods such as spraying, spin coating, brushing and casting, makes the thin-film material that obtains to have conducting function after the solvent evaporates;
The matrix material mother liquor of step 3) adds in the ball mill, and rotating speed is 50-300 rev/mins, and through 0.5-6 hour ball-milling processing, the moulding that is heating and curing under 60-160 ℃ then obtained having the mono-layer graphite matrix material of conducting function.
The matrix material mother liquor spontaneous curing at room temperature of step 3) obtains having the mono-layer graphite matrix material of conducting function.
The preparation method of mono-layer graphite provided by the invention and polymer composites may further comprise the steps:
1) gets mono-layer graphite and polymkeric substance by metering, it is joined in the high-speed mixer simultaneously rotating speed: 1000-5000 rev/mins.Mixing temperature is 60-100 ℃, mix mixture;
2) the gained mixture joins in twin screw extruder or the Banbury mixer by volume pump, and screw speed is 40-150 rev/mins, and temperature is 140-300 ℃, obtains the master batch of matrix material after extruding also pelletizing;
Step 2) composite master batch of gained adopts injection moulding or mould pressing method, makes the goods of sheet material, tubing and complicated shape;
Step 2) adopt conventional spinning technique to be prepared into the polymer composite fibrous material that contains mono-layer graphite after the composite master batch drying of gained.
Characteristics of the present invention are to utilize good electroconductibility of mono-layer graphite and high major diameter recently to prepare conducing composite material.Microanalysis proof mono-layer graphite homodisperse in body material, only need to add just can form conductive network on a small quantity, obtain the conducing composite material of variform, for example at first make the mother liquor of matrix material or the solid master batch of matrix material, make the material of different purposes then according to different needs.Conduct electricity preferably and antistatic effect because mono-layer graphite and polymer composites have, as electro-conductive material can be applied to build, the manufacturing of precision instrument and microelectronics, machinery and aerospace device.
Because the density of mono-layer graphite is lower, make the density of matrix material of the present invention be significantly less than traditional metal and metal oxide composite among the present invention, low price, light weight has the solution handlability, and forming process is good.Particularly mono-layer graphite has the best mechanical property of known nano material, makes matrix material of the present invention have higher intensity and modulus, might use under particular surroundingss such as building, machinery and aerospace.Simultaneously,, make matrix material of the present invention have advantages such as the heat radiation of being easy to, be expected in the acquisition widespread use of fields such as precision instrument and microelectronics because mono-layer graphite has good heat conductivility.
Description of drawings
The transmission electron microscope photo of Fig. 1 mono-layer graphite (embodiment 1).
The stereoscan photograph of Fig. 2 mono-layer graphite/compound polyurethane material (embodiment 1) section.
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 the content of the invention described above, all belongs to protection domain of the present invention.
Embodiment 1:
Method according to bibliographical information prepares mono-layer graphite (Carbon, 2004,42,2929.).(this mono-layer graphite is the mono-layer graphite that contains carboxyl, hydroxyl and epoxy bond functionalization).(mean diameter 1-2 μ m, thickness is about 0.8nm) add in the entry with the 1g mono-layer graphite, handle 30 minutes through ultrasonic wave (500W), and it is dissolved fully; (Zhejiang Nicca Chemical Co., Ltd 9009-54-5) stirred 1 hour in the adding 400ml water, fully dissolving with 9g urethane.With above-mentioned two kinds of aqueous solution, stirred 0.5 hour, used ultrasonication again 1 hour, mono-layer graphite is disperseed in polymkeric substance, obtain even, stable mono-layer graphite/urethane mixing solutions.This mixing solutions is added in the ball mill (Nanjing Univ. Instrument Factory, the comprehensive planetary ball mill of QM-QX),, obtain containing the polyurethane water-based paint of mono-layer graphite through the processing of 6 hours ball millings (100 rev/mins).This coating is filmed, at room temperature or at 60 ℃ of following curing moldings, obtain mono-layer graphite/urethane composite film material, the specific conductivity of this film is 5 * 10
-2S/cm has conduction and antistatic effect preferably.
Embodiment 2:
Method according to bibliographical information prepares mono-layer graphite (Carbon, 2004,42,2929.).The 100mg mono-layer graphite is added in the 500mL round-bottomed bottle, add the DMF that 200mL dewaters through distillation, nitrogen protection, ultrasonic (500W) handled after 1 hour, formed homodisperse suspension.Add the 100mg phenyl isocyanate, nitrogen protection, stirring at room 10 hours is passed through high speed centrifugation (10000 rev/mins) again, and vacuum-drying.Obtain the mono-layer graphite of homodisperse phenyl isocyanate functionalization.The mono-layer graphite of 100mg isocyanate functionization is added in the acetone,, it is dissolved fully through ultrasonication 0.5 hour; 9.9 gram Resins, epoxy (Tianjin resin processing plant, 618 types) fully are dissolved in the 100mL acetone.Then two kinds of solution are mixed, stirred 2 hours, used ultrasonication again 1 hour, mono-layer graphite is disperseed in polymkeric substance, obtain even, stable mono-layer graphite/urethane mixing solutions.This mixing solutions is added in the ball mill,, obtain containing the polyurethane water-based paint of mono-layer graphite through the processing of 6 hours ball millings (100 rev/mins).This coating is filmed, at room temperature or at 120 ℃ of following curing moldings, obtain mono-layer graphite/urethane Fu He Bao Mo material, the specific conductivity of Gai Bao Mo is 0.5S/cm, has conduction and antistatic effect preferably.
Embodiment 3:
Method according to bibliographical information prepares mono-layer graphite (Carbon, 2004,42,2929.).At 400 ℃, roast is 2 hours under the nitrogen atmosphere with mono-layer graphite, the mono-layer graphite after obtaining reducing.With the polyethylene terephthalate after the vacuum-drying (PET) 900g, polybutylene terephthalate (PBT) 90g and mono-layer graphite 10g join in the high-speed mixer, mix 30 minutes.By volume pump mixture is added in the twin screw extruder, screw speed is controlled at 60 rev/mins again, and extrusion temperature is controlled at 230-250 ℃, through extrude, drawing-off, use the dicing machine pelletizing then, obtain composite master batch.Master batch is dry in vacuum drying oven, and, obtain to contain the composite product of mono-layer graphite through injection moulding machine injection molding.The thickness of this product is 1mm, and the specific conductivity of Gai Bao Mo is 3 * 10
-1S/cm has conduction and antistatic effect preferably.
Embodiment 4:
Method according to bibliographical information prepares mono-layer graphite (Carbon, 2004,42,2929.).With 99.9 parts of the nylon after the vacuum-drying 66 (Jiangsu Hua Yang nylon company limited, nilon66), 0.1 part of mono-layer graphite joins in the high-speed mixer and mixed 30 minutes.By volume pump mixture is joined in the twin screw extruder (blue safe plastics machinery company limited, SHJ type), screw speed is controlled at 60 rev/mins again, and extrusion temperature is controlled at 260-280 ℃, through extrude, pelletizing obtains composite master batch.With master batch in vacuum drying oven in 80 ℃ dry 4 hours down, obtain to contain the conjugated fibre of mono-layer graphite then through melt-spinning and drawing-off, the specific conductivity of this fiber is 8 * 10
-5S/cm can be used for antistatic clothes.
Embodiment 5:
Method according to bibliographical information prepares mono-layer graphite (Carbon, 2004,42,2929.).(Jilin Petrochemical company, 9715A) 80 parts, 20 parts of mono-layer graphites join in the high-speed mixer, mix 30 minutes with the ABS resin after the vacuum-drying.Again this mixture is put into Banbury mixer, screw speed is controlled at 40 rev/mins, and melting temperature is controlled at 220 ℃, and the time is 20 minutes.Use vulcanizing press hot-forming then, obtain the matrix material that thickness is 1mm, the specific conductivity of this matrix material is 2S/cm, has conduction and antistatic effect preferably.
Claims (10)
1, a kind of mono-layer graphite and polymer composites is characterized in that it is is raw material with mono-layer graphite and polymkeric substance, and thorough mixing is made, and its parts by weight are:
0.1～100 part of mono-layer graphite;
0.1～100 part of polymkeric substance or other body material;
Described mono-layer graphite 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 of organo-functional group through functionalization, and single graphite flake area is at 10nm
2To 400 μ m
2Between, single-sheet thickness adopts mechanically peel method, crystal epitaxy method and chemical oxidation method preparation between 0.34 to 2nm;
Described organo-functional group is that carboxyl, hydroxyl, epoxy bond, sulfonic group, phenyl isocyanate, thiophene, pyrroles, aniline and/or the chain alkyl functional group that contains 6 to 18 carbon are at least a;
Described polymkeric substance is selected from least a in urethane, polyacrylic ester, polyester, polymeric amide, ABS, polyethylene, polypropylene, polycarbonate, polyvinyl chloride, Resins, epoxy, polyimide, resol and/or the rubber, and polymericular weight is between 2000-200000.
2,, it is characterized in that described polymkeric substance is selected from urethane, polyacrylic ester, polyester, ABS or Resins, epoxy according to the described matrix material of claim 1.
3, the preparation method of a kind of mono-layer graphite and polymer composites is characterized in that may further comprise the steps:
1) mono-layer graphite is added in entry or the organic solvent,, mono-layer graphite is dispersed or dissolved through ultrasonication 0.5-2 hour;
2) polymkeric substance fully is dissolved in the corresponding organic solvent;
3) with step 1) and 2) two kinds of solution mix, and stir 0.5-3 hour, use ultrasonication 0.5-3 hour again, obtain the mother liquor of the matrix material of even, stable mono-layer graphite and polymkeric substance.
4,, it is characterized in that described organic solvent comprises methyl alcohol, ethanol according to the preparation method of the described matrix material of claim 3, Virahol, acetone, ethyl acetate, chloroform, tetracol phenixin, tetrahydrofuran (THF), N, dinethylformamide, dimethyl sulfoxide (DMSO), benzene, toluene, dimethylbenzene, chlorobenzene, dichlorobenzene, trichlorobenzene.
5, according to the preparation method of the described matrix material of claim 3, the matrix material mother liquor that it is characterized in that step 3) is by the method for spraying, spin coating, brushing and casting film preparation, makes the thin-film material that obtains to have conducting function after the solvent evaporates.
6, according to the preparation method of the described matrix material of claim 3, the matrix material mother liquor that it is characterized in that step 3) adds in the ball mill, rotating speed is 50-300 rev/mins, through 0.5-6 hour ball-milling processing, the moulding that is heating and curing under 60-160 ℃ then obtains having the mono-layer graphite matrix material of conducting function.
7, according to the preparation method of the described matrix material of claim 3, it is characterized in that the matrix material mother liquor spontaneous curing at room temperature of step 3), obtain having the mono-layer graphite matrix material of conducting function.
8, the preparation method of a kind of mono-layer graphite and polymer composites may further comprise the steps:
1) by 0.1～100 part of metering mono-layer graphite, 0.1～100 part of polymkeric substance or other body material are got mono-layer graphite and polymkeric substance, join it in high-speed mixer simultaneously, rotating speed: 1000-5000 rev/mins, mixing temperature is 60-100 ℃, mix mixture;
2) the gained mixture joins in twin screw extruder or the Banbury mixer by volume pump, and screw speed is 40-150 rev/mins, and temperature is 140-300 ℃, obtains the master batch of matrix material after extruding also pelletizing.
9, according to the preparation method of the described matrix material of claim 8, it is characterized in that step 2) composite master batch of gained adopts injection moulding or mould pressing method, makes the goods of sheet material, tubing and complicated shape.
10, according to the preparation method of the described matrix material of claim 8, it is characterized in that step 2) adopt conventional spinning technique to be prepared into the polymer composite fibrous material that contains mono-layer graphite after the composite master batch drying of gained.
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| CNA2008101524668A CN101381511A (en) | 2008-10-24 | 2008-10-24 | Mono-layer graphite and polymer compound material and preparation and application thereof |
| PCT/CN2009/074617 WO2010045887A1 (en) | 2008-10-24 | 2009-10-26 | Polymer composite and its preparation method |
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